Acicular hematite particles and magnetic recording medium

Information

  • Patent Grant
  • 6207253
  • Patent Number
    6,207,253
  • Date Filed
    Thursday, December 24, 1998
    26 years ago
  • Date Issued
    Tuesday, March 27, 2001
    23 years ago
Abstract
Acicular hematite particles of the present invention comprise an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35 and a pH value of not less than 8, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO4.Such acicular hematite particles are suitable as non-magnetic particles for a non-magnetic undercoat layer of a magnetic recording medium which exhibits a low light transmittance, an excellent smooth surface and a high strength, and can be prevented from being deteriorated in magnetic properties due to the corrosion of magnetic acicular metal particles containing iron as a main component which are dispersed in a magnetic recording layer thereof.
Description




BACKGROUND OF THE INVENTION:




The present invention relates to acicular hematite particles and a magnetic recording medium, and more particularly, to acicular hematite particles suitable as non-magnetic particles for a non-magnetic undercoat layer of a magnetic recording medium which exhibits a low light transmittance, an excellent smooth surface and a high strength, and can be prevented from being deteriorated in magnetic properties due to the corrosion of magnetic acicular metal particles containing iron as a main component which are dispersed in a magnetic recording layer thereof; a non-magnetic substrate for a magnetic recording medium provided with a non-magnetic undercoat layer containing the acicular hematite particles; and a magnetic recording medium comprising the non-magnetic substrate and a magnetic recording layer containing magnetic acicular metal particles containing iron as a main component.




With a development of miniaturized, lightweight video or audio magnetic recording and reproducing apparatuses for long-time recording, magnetic recording media such as a magnetic tape and magnetic disk have been increasingly and strongly required to have a higher performance, namely, a higher recording density, higher output characteristic, in particular, an improved frequency characteristic and a lower noise level.




Various attempts have been made at both enhancing the properties of magnetic particles and reducing the thickness of a magnetic recording layer in order to improve these properties of a magnetic recording medium.




The enhancement of the properties of magnetic particles is firstly described.




The required properties of magnetic particles in order to satisfy the above-described demands on a magnetic recording medium are a high coercive force and a large saturation magnetization.




As magnetic particles suitable for high-output and high-density recording, magnetic acicular metal particles containing iron as a main component, which are obtained by heat-treating acicular goethite particles or acicular hematite particles in a reducing gas, are widely known.




Although magnetic acicular metal particles containing iron as a main component have a high coercive force and a large saturation magnetization, since the magnetic acicular metal particles containing iron as a main component used for a magnetic recording medium are very fine particles having a particle size of not more than 1 μm, particularly, 0.01 to 0.3 μm, they easily corrode and the magnetic characteristics thereof are deteriorated, especially, the saturation magnetization and the coercive force are decreased.




Therefore, in order to maintain the characteristics of a magnetic recording medium which uses magnetic acicular metal particles containing iron as a main component as magnetic particles, over a long period, it is strongly demanded to suppress the corrosion of magnetic acicular metal particles containing iron as a main component as much as possible.




A reduction in the thickness of a magnetic recording layer is described. Video tapes have recently been required more and more to have a higher picture quality, and the frequencies of carrier signals recorded in recent video tapes are higher than those recorded in conventional video tapes. In other words, the signals in the short-wave region have come to be used, and as a result, the magnetization depth from the surface of a magnetic tape has come to be remarkably small.




With respect to short wavelength signals, a reduction in the thickness of a magnetic recording layer is also strongly demanded in order to improve the high output characteristics, especially, the S/N ratio of a magnetic recording medium. This fact is described, for example, on page 312 of


Development of Magnetic Materials and Technique for High Dispersion of Magnetic Powder,


published by Sogo Gijutsu Center Co., Ltd. (1982), “. . . the conditions for high-density recording in a coated-layer type tape are that the noise level is low with respect to signals having a short wavelength and that the high output characteristics are maintained. To satisfy these conditions, it is necessary that the tape has large coercive force Hc and residual magnetization Br, . . . and the coating film has a smaller thickness. . . . ”.




Development of a thinner film for a magnetic recording layer has caused some problems.




Firstly, it is necessary to make a magnetic recording layer smooth and to eliminate the non-uniformity of thickness. As well known, in order to obtain a smooth magnetic recording layer having a uniform thickness, the surface of the base film must also be smooth. This fact is described on pages 180 and 181 of


Materials for Synthetic Technology


-


Causes of Friction and Abrasion of Magnetic Tape and Head Running System and Measures for Solving the Problem


(hereinunder referred to as “


Materials for Synthetic Technology”


(1987), published by the Publishing Department of Technology Information Center,“. . . the surface roughness of a hardened magnetic coating film depends on the surface roughness of the base film (back surface roughness) so largely as to be approximately proportional, . . . , since the magnetic coating film is formed on the base film, the more smooth the surface of the base film is, the more uniform and larger head output is obtained and the more the S/N ratio is improved.”




Secondly, there has been caused a problem in the strength of a base film with a tendency of the reduction in the thickness of the base film in response to the demand for a thinner magnetic coating film. This fact is described, for example, on page 77 of the above-described


Development of Magnetic Materials and Technique for High Dispersion of Magnetic Powder,


“. . . Higher recording density is a large problem assigned t the present magnetic tape. This is important in order to shorten the length of the tape so as to miniaturize the size of a cassette and to enable long-time recording. For this purpose, it is necessary to reduce the thickness of a base film . . . With the tendency of reduction in the film thickness, the stiffness of the tape also reduces to such an extent as to make smooth travel in a recorder difficult. Therefore, improvement of the stiffness of a video tape both in the machine direction and in the transverse direction is now strongly demanded. . . . ”




There is no end to a demand for a higher performance in recent magnetic recording media. Since the above-described reduction in the thickness of a magnetic recording layer and a base film lowers the durability of the magnetic recording medium, an improvement of the durability of the magnetic recording medium is in strong demand.




This fact is described in Japanese Patent Application Laid-Open (KOKAI) No. 5-298679, “. . . With the recent development in magnetic recording, a high picture quality and a high sound quality have been required more and more in recording. The signal recording property is, therefore, improved. Especially, finer and higher-density ferromagnetic particles have come to be used. It is further required to make the surface of a magnetic tape smooth so as to reduce noise and raise the C/N . . . However, the coefficient of friction between the magnetic recording layer and an apparatus during the travel of the magnetic recording tape increases, so that there is a tendency of the magnetic recording layer of the magnetic recording medium being damaged or exfoliated even in a short time. Especially, in a videotape, since the magnetic recording medium travels at a high speed in contact with the video head, the ferromagnetic particles are apt to be dropped from the magnetic recording layer, thereby causing clogging on the magnetic head. Therefore, an improvement in the running durability of the magnetic recording layer of a magnetic recording medium is expected . . .”




The end portion of a magnetic recording medium such as a magnetic tape, especially, a video tape is judged by detecting a portion of the magnetic recording medium at which the light transmittance is large by a video deck. If the light transmittance of the whole part of a magnetic recording layer is made large by the production of a thinner magnetic recording medium or the ultrafine magnetic particles dispersed in the magnetic recording layer, it is difficult to detect the portion having a large light transmittance by a video deck. For reducing the light transmittance of the whole part of a magnetic recording layer, carbon black or the like is added to the magnetic recording layer. It is, therefore, essential to add carbon black or the like to a magnetic recording layer in the present video tapes.




However, addition of a large amount of non-magnetic particles such as carbon black impairs not only the enhancement of the magnetic recording density but also the development of a thinner magnetic recording layer. In order to reduce the magnetization depth from the surface of the magnetic tape and to produce a thinner magnetic recording layer, it is strongly demanded to reduce, as much as possible, the quantity of non-magnetic particles such as carbon black which are added to a magnetic recording layer.




It is, therefore, strongly demanded that the light transmittance of a magnetic recording layer should be small even if the carbon black or the like which is added to the magnetic recording layer is reduced to a small amount. From this point of view, improvements in the magnetic recording medium are now in strong demand.




There has, also, been pointed out such a problem that the magnetic acicular metal particles containing iron as a main component dispersed in the magnetic recording layer are corroded in a passage of time after the production thereof, so that magnetic properties of the magnetic recording medium are considerably deteriorated.




Various efforts have been made to improve the substrate for a magnetic recording layer with a demand for a thinner magnetic recording layer and a thinner base film. A magnetic recording medium having at least one undercoat layer (hereinunder referred to “non-magnetic undercoat layer”) comprising a binder resin and non-magnetic particles such as hematite particles which are dispersed therein, on a base film has been proposed and put to practical use (Japanese Patent Publication (KOKOKU) No. 6-93297 (1994), Japanese Patent Application Laid-Open (KOKAI) Nos. 62-159338 (1987), 63-187418 (1988), 4-167225 (1992), 4-325915 (1992), 5-73882 (1993), 5-182177 (1993), 5-347017 (1993), 6-60362 (1994), etc.)




The above-described magnetic recording media composed of a base film and a non-magnetic undercoat layer composed of a binder resin and non-magnetic particles dispersed therein and formed on the base film, have a small light transmittance and a high strength, but the durability and the surface smoothness thereof are inconveniently poor.




This fact is described in Japanese Patent Application Laid-Open (KOKAI) No. 5-182177 (1993), “. . . Although the problem of surface roughness is solved by providing a magnetic recording layer as an upper layer after forming a thick non-magnetic undercoat layer on the base film, the problem of the abrasion of a head and the problem of durability are not solved and still remain. This is considered to be caused because a thermoset resin is usually used as a binder of the non-magnetic undercoat layer, so that the magnetic recording layer is brought into contact with a head or other members without any cushioning owing to the hardened non-magnetic undercoat layer, and a magnetic recording medium having such a non-magnetic undercoat layer has a considerably poor flexibility.”




Therefore, it has been strongly required to improve surface smoothness of the non-magnetic undercoat layer. Hitherto, it has been attempted to enhance a dispersibility of acicular hematite particles as non-magnetic particles by directing attention to the particle size distribution of major axis diameters of the particles (Japanese Patent Application Laid-open (KOKAI) No. 9-170003(1997), and the like).




That is, in the above Japanese Patent Application Laid-open (KOKAI) No. 9-170003(1997), there has been described a method of heat-treating acicular goethite particles or acicular hematite particles produced by heat-dehydrating the acicular goethite particles, at a temperature of not less than 550° C., thereby obtaining high-density acicular hematite particles having a good geometrical standard deviation of a major axis diameter. However, as shown in Comparative Examples hereinafter, the obtained acicular hematite particles are deteriorated in a geometrical standard deviation of the minor axis diameter, so that the dispersibility of the particles is still unsatisfactory.




Accordingly, with a recent tendency of reducing the thickness of the magnetic recording layer and non-magnetic base film, there have been most demanded acicular hematite particles having a uniform particle size, which are suitable as non-magnetic particles for a non-magnetic undercoat layer having a smooth surface and a high mechanical; and a magnetic recording medium provided with a non-magnetic undercoat layer containing the acicular hematite particles, which exhibits a low light transmittance, an excellent smooth surface, a high mechanical strength and an excellent durability, and which can be prevented from being deteriorated in magnetic properties due to the corrosion of magnetic acicular metal particles containing iron as a main component contained in a magnetic recording layer. However, such acicular hematite particles and magnetic recording medium capable of satisfying these requirements have not been obtained yet.




Further, in recent years, for purposes of short-wavelength recording and high-density recording, it has been inevitably necessary to use magnetic acicular metal particles containing iron as a main component, having a high coercive force and a large saturation magnetization. However, since the magnetic acicular metal particles containing iron as a main component are fine particles, the magnetic acicular metal particles containing iron as a main component tend to be corroded, resulting in deterioration in magnetic properties thereof. Therefore, it has been demanded to provide a magnetic recording medium in which magnetic properties thereof are not deteriorated and can be maintained for a long period of time.




As a result of the present inventors' earnest studies, it has been found that (a) by heat-treating specific acicular goethite particles at a specific temperature and then heat-dehydrating the thus-treated acicular goethite particles to obtain specific acicular hematite particles, or (b) by subjecting specific acicular hematite particles to a acid-dissolving treatment under specific conditions to obtain specific acicular hematite particles, and then heating the acicular hematite particles obtained by the method (a) or (b) in an alkaline suspension, there can be obtained high-purity acicular hematite particles which exhibit a uniform particle size, especially wherein the geometrical standard deviation nears 1.0, and which are useful as non-magnetic particles for a non-magnetic undercoat layer of a magnetic recording medium which can be prevented from being deteriorated in magnetic properties due to the corrosion of magnetic acicular metal particles containing iron as a main component contained in a magnetic recording layer. The present invention has been attained on the basis of the finding.




SUMMARY OF THE INVENTION




It is an object of the present invention to provide acicular hematite particles which are useful as non-magnetic particles for a non-magnetic undercoat layer of a magnetic recording medium exhibiting an excellent surface smoothness, and have a uniform particle size, especially are excellent geometrical standard deviation of a minor axis diameter thereof.




It is another object of the present invention to provide acicular hematite particles suitable as non-magnetic particles for a non-magnetic undercoat layer of a magnetic recording medium which can exhibit a low light transmittance, a smooth surface and a high strength, and can be prevented from being deteriorated in magnetic properties due to the corrosion of magnetic acicular metal particles containing iron as a main component contained in a magnetic recording layer thereof, and a magnetic recording medium provided with a non-magnetic undercoat layer containing the acicular hematite particles.




It is an other object of the present invention to provide acicular hematite particles suitable as non-magnetic particles for a non-magnetic undercoat layer having a low light transmittance, a smooth surface and a high, and a magnetic recording medium which can exhibit a low light transmittance, a smooth surface, a high strength and an excellent durability, and can be prevented from being deteriorated in magnetic properties due to the corrosion of magnetic acicular metal particles containing iron as a main component contained in a magnetic recording layer thereof.




To accomplish the aims, in a first aspect of the present invention, there are provided acicular hematite particles comprising an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35 and a pH value of not less than 8, and




containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


.




In a second aspect of the present invention, there are provided acicular hematite particles comprising an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35 and a pH value of not less than 8, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


, and




having a coat formed on at least a part of the surface of said acicular hematite particle, comprising at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon in amount of 0.05 to 50% by weight, calculated as Al or SiO


2


, based on the weight of said acicular hematite particles.




In a third aspect of the present invention, there are provided acicular hematite particles comprising an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35 and a pH value of not less than 8,




containing aluminum existing within the particle in an amount of 0.05 to 50% by weight, calculated as Al, based on the weight of said acicular hematite particles, and




containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


.




In a fourth aspect of the present invention, there are provided acicular hematite particles comprising an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35 and a pH value of not less than 8, containing aluminum existing within the particle in an amount of 0.05 to 50% by weight, calculated as Al, based on the weight of said acicular hematite particles, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


, and




having a coat formed on at least a part of the surface of said acicular hematite particle, comprising at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon in amount of 0.05 to 50% by weight, calculated as Al or SiO


2


, based on the weight of said acicular hematite particles.




In a fifth aspect of the present invention, there are provided acicular hematite particles comprising an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35, a geometrical standard deviation of major axis diameter of not more than 1.50, a BET specific surface area of 35.9 to 180 m


2


/g and a pH value of not less than 8, and




containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


.




In a sixth aspect of the present invention, there are provided acicular hematite particles comprising an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35, a geometrical standard deviation of major axis diameter of not more than 1.50, a BET specific surface area of 35.9 to 180 m


2


/g and a pH value of not less than 8, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


, and




having a coat formed on at least a part of the surface of said acicular hematite particle, comprising at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon in amount of 0.05 to 50% by weight, calculated as Al or SiO


2


, based on the weight of said acicular hematite particles.




In a seventh aspect of the present invention, there are provided acicular hematite particles comprising an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35, a geometrical standard deviation of major axis diameter of not more than 1.50, a BET specific surface area of 35.9 to 180 m


2


/g and a pH value of not less than 8,




containing aluminum existing within the particle in an amount of 0.05 to 50% by weight, calculated as Al, based on the weight of said acicular hematite particles, and




containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


.




In an eighth aspect of the present invention, there are provided acicular hematite particles comprising an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35, a geometrical standard deviation of major axis diameter of not more than 1.50, a BET specific surface area of 35.9 to 180 m


2


/g and a pH value of not less than 8, containing aluminum existing within the particle in an amount of 0.05 to 50% by weight, calculated as Al, based on the weight of said acicular hematite particles, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


, and




having a coat formed on at least a part of the surface of said acicular hematite particle, comprising at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon in amount of 0.05 to 50% by weight, calculated as Al or SiO


2


, based on the weight of said acicular hematite particles.




In a ninth aspect of the present invention, there is provided acicular hematite particles comprising a geometrical standard deviation of major axis diameter of not more than 1.50, a geometrical standard deviation of minor axis diameter of not more than 1.30, a BET specific surface area of 40 to 150 m


2


/g, an average major axis diameter of 0.01 to 0.2 μm and a pH value of not less than 8, and




containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


.




In a tenth aspect of the present invention, there are provided acicular hematite particles comprising a geometrical standard deviation of major axis diameter of not more than 1.50, a geometrical standard deviation of minor axis diameter of not more than 1.30, a BET specific surface area of 40 to 150 m


2


/g, an average major axis diameter of 0.01 to 0.2 μm and a pH value of not less than 8, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


, and




having a coat formed on at least a part of the surface of said acicular hematite particle, comprising at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon in amount of 0.05 to 50% by weight, calculated as Al or SiO


2


, based on the weight of said acicular hematite particles.




In an eleventh aspect of the present invention, there are provided acicular hematite particles comprising a geometrical standard deviation of major axis diameter of not more than 1.50, a geometrical standard deviation of minor axis diameter of not more than 1.30, a BET specific surface area of 40 to 150 m


2


/g, an average major axis diameter of 0.01 to 0.2 μm and a pH value of not less than 8,




containing aluminum existing within the particle in an amount of 0.05 to 50% by weight, calculated as Al, based on the weight of said acicular hematite particles, and




containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


.




In a twelfth aspect of the present invention, there are provided acicular hematite particles comprising a geometrical standard deviation of major axis diameter of not more than 1.50, a geometrical standard deviation of minor axis diameter of not more than 1.30, a BET specific surface area of 40 to 150 m


2


/g, an average major axis diameter of 0.01 to 0.2 μm and a pH value of not less than 8, containing aluminum existing within the particle in an amount of 0.05 to 50% by weight, calculated as Al, based on the weight of said acicular hematite particles, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


, and




having a coat formed on at least a part of the surface of said acicular hematite particle, comprising at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon in amount of 0.05 to 50% by weight, calculated as Al or SiO


2


, based on the weight of said acicular hematite particles.




In a thirteenth aspect of the present invention, there is provided a magnetic recording medium comprising:




a non-magnetic base film;




a non-magnetic undercoat layer formed on said non-magnetic base film, comprising a binder resin and acicular hematite particles having an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35 and a pH value of not less than 8, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


; and




a magnetic coating film comprising a binder resin and magnetic acicular metal particles containing iron as a main component.




In a fourteenth aspect of the present invention, there is provided a magnetic recording medium comprising:




a non-magnetic base film;




a non-magnetic undercoat layer formed on said non-magnetic base film, comprising a binder resin and acicular hematite particles comprising an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35 and a pH value of not less than 8, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


, and




having a coat formed on at least a part of the surface of said acicular hematite particle, comprising at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon in amount of 0.05 to 50% by weight, calculated as Al or SiO


2


, based on the weight of said acicular hematite particles; and




a magnetic coating film comprising a binder resin and magnetic acicular metal particles containing iron as a main component.




In a fifteenth aspect of the present invention, there is provided a magnetic recording medium comprising:




a non-magnetic base film;




a non-magnetic undercoat layer formed on said non-magnetic base film, comprising a binder resin and acicular hematite particles comprising an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35 and a pH value of not less than 8,




containing aluminum existing within the particle in an amount of 0.05 to 50% by weight, calculated as Al, based on the weight of said acicular hematite particles, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


; and




a magnetic coating film comprising a binder resin and magnetic acicular metal particles containing iron as a main component.




In a sixteenth aspect of the present invention, there is provided a magnetic recording medium comprising:




a non-magnetic base film;




a non-magnetic undercoat layer formed on said non-magnetic base film, comprising a binder resin and acicular hematite particles comprising an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35 and a pH value of not less than 8, containing aluminum existing within the particle in an amount of 0.05 to 50% by weight, calculated as Al, based on the weight of said acicular hematite particles, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


, and




having a coat formed on at least a part of the surface of said acicular hematite particle, comprising at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon in amount of 0.05 to 50% by weight, calculated as Al or SiO


2


, based on the weight of said acicular hematite particles; and




a magnetic coating film comprising a binder resin and magnetic acicular metal particles containing iron as a main component.




In a seventeenth aspect of the present invention, there is provided a non-magnetic substrate comprising:




a non-magnetic base film; and




a non-magnetic undercoat layer formed on said non-magnetic base film, comprising a binder resin and acicular hematite particles having an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35 and a pH value of not less than 8, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


.




In an eighteenth aspect of the present invention, there is provided a non-magnetic substrate comprising:




a non-magnetic base film; and




a non-magnetic undercoat layer formed on said non-magnetic base film, comprising a binder resin and acicular hematite particles comprising an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35 and a pH value of not less than 8, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


, and




having a coat formed on at least a part of the surface of said acicular hematite particle, comprising at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon in amount of 0.05 to 50% by weight, calculated as Al or SiO


2


, based on the weight of said acicular hematite particles.




In a nineteenth aspect of the present invention, there is provided a non-magnetic substrate comprising:




a non-magnetic base film; and




a non-magnetic undercoat layer formed on said non-magnetic base film, comprising a binder resin and acicular hematite particles comprising an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35 and a pH value of not less than 8,




containing aluminum existing within the particle in an amount of 0.05 to 50% by weight, calculated as Al, based on the weight of said acicular hematite particles, and




containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


.




In a twentieth aspect of the present invention, there is provided a non-magnetic substrate comprising:




a non-magnetic base film; and




a non-magnetic undercoat layer formed on said non-magnetic base film, comprising a binder resin and acicular hematite particles comprising an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35 and a pH value of not less than 8, containing aluminum existing within the particle in an amount of 0.05 to 50% by weight, calculated as Al, based on the weight of said acicular hematite particles, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO


4


, and




having a coat formed on at least a part of the surface of said acicular hematite particle, comprising at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon in amount of 0.05 to 50% by weight, calculated as Al or SiO


2


, based on the weight of said acicular hematite particles.




DETAILED DESCRIPTION OF THE INVENTION




The present invention is explained in more detail below.




First, the acicular hematite particles for a non-magnetic undercoat layer of a magnetic recording medium according to the present invention are described.




The acicular hematite particles according to the present invention have substantially the same acicular shape as that of particles to be treated. The “acicular” shape may include not only a needle shape but also a spindle shape or a rice-ball shape. In addition, the lower limit of an aspect ratio of the particles (=average major axis diameter:average minor axis diameter, hereinafter referred to merely as “aspect ratio”) is usually 2:1, preferably 3:1. With the consideration of dispersibility of the particles in vehicle, the upper limit of the aspect ratio is preferably 20:1, more preferably 10:1. When the aspect ratio is less than 2:1, it may be difficult to obtain a coating film having a sufficient strength. On the other hand, when the aspect ratio is more than 20:1, the particles may be entangled with each other in vehicle, thereby causing a tendency that the dispersibility thereof may be deteriorated or the viscosity thereof may be increased.




The upper limit of the average major axis diameter of the acicular hematite particles according to the present invention is usually 0.295 μm. The lower limit of the average major axis diameter of the acicular hematite particles according to the present invention is usually 0.004 μm. If the upper limit of the average major axis diameter exceeds 0.295 μm, the surface smoothness of the coating film formed using such particles may be impaired because the particle size is large. On the other hand, if the lower limit of the average major axis diameter is less than 0.004 μm, the dispersion in the vehicle may be difficult because of the increase of the intermolecular force due to the fine particles. With the consideration of the dispersibility in the vehicle and the surface smoothness of the coating film, the upper limit thereof is preferably 0.275 μm, more preferably 0.200 μm, still more preferably 0.100 μm, and the lower limit thereof is preferably 0.008 μm, more preferably 0.010 μm, more preferably 0.020 μm.




The upper limit of the average minor axis diameter of the acicular hematite particles according to the present invention is usually 0.147 μm. The lower limit of the average minor axis diameter of the acicular hematite particles according to the present invention is usually 0.002 μm. If the upper limit of the average minor axis diameter exceeds 0.147 μm, the surface smoothness of the coating film formed using such particles may be impaired because the particle size is large. On the other hand, if the lower limit of the average minor axis diameter is less than 0.002 μm, the dispersion in the vehicle may be difficult because of the increase of the intermolecular force due to the fine particles. With the consideration of the dispersibility in the vehicle and the surface smoothness of the coating film, the upper limit thereof is preferably 0.123 μm, more preferably 0.100 μm, still more preferably 0.050 μm, and the lower limit thereof is preferably 0.004 μm, more preferably 0.005 μm, more preferably 0.010 μm.




The upper limit of the BET specific surface area (S


BET


) of the acicular hematite particles according to the present invention is usually 180 m


2


/g. The lower limit of the BET specific surface area (S


BET


) of the acicular hematite particles according to the present invention is usually 35.9 m


2


/g. If the upper limit thereof is more than 180 m


2


/g, the dispersion in the vehicle may be difficult because of the increase of the intermolecular force due to the fine particles. On the other hand, if the lower limit thereof is less than 35.9 m


2


/g, the acicular hematite particles may be coarse particles or large particles produced by sintering a particle and between particles, which are apt to exert a deleterious influence on the surface smoothness of the coating film. With the consideration of the dispersibility in the vehicle and the surface smoothness of the coating film, the upper limit thereof (S


BET


) is preferably 160 m


2


/g, more preferably 150 m


2


/g and the lower limit thereof (S


BET


) is preferably 38 m


2


/g, more preferably 40 m


2


/g.




The upper limit of the geometrical standard deviation of the major axis diameter of the acicular hematite particles according to the present invention is usually not more than 1.50. If the upper limit of the geometrical standard deviation of the major axis diameter exceeds 1.50, the coarse particles existent sometimes exert a deleterious influence on the surface smoothness of the coating film. With the consideration of the surface smoothness of the coating film, the upper limit thereof is preferably 1.45, more preferably not more than 1.40. From the point of view of industrial productivity, the lower limit thereof is preferably 1.01.




The upper limit of the geometrical standard deviation of the minor axis diameter of the acicular hematite particles according to the present invention is usually not more than 1.35. If the upper limit of the geometrical standard deviation of the minor axis diameter exceeds 1.35, the coarse particles existent sometimes exert a deleterious influence on the surface smoothness of the coating film. With the consideration of the surface smoothness of the coating film, the upper limit thereof is preferably 1.33, more preferably not more than 1.30, still more preferably not more than 1.28. From the point of view of industrial productivity, the lower limit thereof is preferably 1.01.




The acicular hematite particles for a non-magnetic undercoat layer of a magnetic recording medium according to the present invention have a high degree of densification. When the degree of densification is represented by a ratio value of the specific surface area (S


BET


) measured by a BET method to the surface area (S


BET


) calculated from the major axis diameter and the minor axis diameter which were measured from the particles in an electron micrograph of the acicular hematite particles (hereinafter referred to merely as “S


BET


/S


TEM


value”), the S


BET


/S


TEM


value is 0.5 to 2.5.




When the S


BET/S




TEM


value is less than 0.5, although the acicular hematite particles are highly densified, the particle diameter thereof may be increased due to sintering in each particle or between particles, so that a coating film formed using these particles, may not have a sufficient smooth surface. On the other hand, when the S


BET


/S


TEM


value is more than 2.5, the degree of densification of the particles is insufficient, so that many pores tend to be formed on the surface and inside of the particle, resulting in insufficient dispersibility of the particles in vehicle. With the consideration of the smooth surface of the coating film and the dispersibility in the vehicle, the S


BET


/S


TEM


value is preferably 0.7 to 2.0, more preferably 0.8 to 1.6.




The pH value of the acicular hematite particles when suspended in an aqueous solution (concentration: 50 g/liter), is not less than 8. If it is less than 8, the magnetic acicular metal particles containing iron as a main component contained in the magnetic recording layer formed on the non-magnetic undercoat layer are gradually corroded, which leads to a deterioration in the magnetic characteristics. In consideration of a corrosion preventive effect on the magnetic acicular metal particles containing iron as a main component, the lower limit of the pH value of the acicular hematite particles is preferably not less than 8.5, more preferably not less than 9.0. The upper limit of the pH value of the acicular hematite particles is preferably 11, more preferably 10.5.




The content of soluble sodium salt in the acicular hematite particles is not more than 300 ppm (calculated as Na). If it exceeds 300 ppm, the magnetic acicular metal particles containing iron as a main component contained in the magnetic recording layer formed on the non-magnetic undercoat layer are gradually corroded, thereby causing a deterioration in the magnetic characteristics. In addition, the dispersion property of the acicular hematite particles in the vehicle is easily impaired, and the preservation of the magnetic recording medium is deteriorated and chalking is sometimes caused in a highly humid environment. In consideration of a corrosion preventive effect on the magnetic acicular metal particles containing iron as a main component, the content of soluble sodium salt in the acicular hematite particles is preferably not more than 250 ppm, more preferably not more than 200 ppm, even more preferably not more than 150 ppm. From the point of view of industry such as productivity, the lower limit thereof is about 0.01 ppm.




The content of soluble sulfate in the acicular hematite particles is not more than 150 ppm (calculated as SO


4


). If it exceeds 150 ppm, the magnetic acicular metal particles containing iron as a main component contained in the magnetic recording layer formed on the non-magnetic undercoat layer are gradually corroded, thereby causing a deterioration in the magnetic properties. In addition, the dispersion property of the acicular hematite particles in the vehicle is easily impaired, and the preservation of the magnetic recording medium is deteriorated and chalking is sometimes caused in a highly humid environment. In consideration of a corrosion preventive effect on the magnetic acicular metal particles containing iron as a main component, the content of soluble sodium salt in the acicular hematite particles is preferably not more than 70 ppm, more preferably not more than 50 ppm. From the point of view of industry such as productivity, the lower limit thereof is about 0.01 ppm.




With the consideration of the durability of the magnetic recording medium having a non-magnetic undercoat layer containing such acicular hematite particles, it is preferable acicular hematite particles contain aluminum present substantially uniformly within the particle in an amount of 0.05 to 50% by weight (calculated as Al) based on the total weight of the acicular hematite particles. When the aluminum content exceeds 50% by weight, although a magnetic recording medium having the non-magnetic undercoat layer containing such acicular hematite particles has a sufficient durability, the durability-improving effect becomes saturated, so that it is meaningless to add aluminum more than necessary. From the point of view of durability-improving effect of a magnetic recording medium and industrial productivity, the aluminum content therein is preferably 0.1 to 30% by weight, more preferably 0.2 to 20% by weight (calculated as Al) based on the total weight of the particles.




Various properties of the acicular hematite particles which contain aluminum within the particle, such as aspect ratio, average major axis diameter, average minor axis diameter, BET specific surface area, geometrical standard deviation of major axis diameter, geometrical standard deviation of minor axis diameter and degree of densification are approximately equivalent in values to those of the acicular hematite particles in which aluminum is not contained within the particle.




The resin adsorptivity of the acicular hematite particles which contain aluminum within the particle according to the present invention is usually not less than 65%, preferably not less than 68%, more preferably not less than 70%. The upper limit thereof is preferably 95%.




At least a part of the surface of the acicular hematite particle which may contain aluminum within the particle according to the present invention may be coated with at least one selected from the group consisting of a hydroxide of aluminum, an oxide of aluminum, a hydroxide of silicon and an oxide of silicon. When the acicular hematite particles which are coated with the above-described coating material are dispersed in a vehicle, the treated particles have an affinity with the binder resin and it is more easy to obtain a desired dispersibility.




The amount of the hydroxide of aluminum, the oxide of aluminum, the hydroxide of silicon or the oxide of silicon used as the coating material is usually not less than 50% by weight, preferably 0.01 to 50% by weight (calculated as Al and/or SiO


2


) based on the total weight of the particles. If it is less than 0.01% by weight (calculated as Al and/or SiO


2


) based on the total weight of the particles, the dispersibility-improving effect by coating therewith may be insufficient. If the amount exceeds 50% by weight (calculated as Al and/or SiO


2


) based on the total weight of the particles, the dispersibility-improving effect by coating therewith becomes saturated, so that it is meaningless to add a coating material more than necessary. From the point of view of dispersibility in the vehicle and industrial productivity, the more preferable amount of coating material is 0.05 to 20% by weight (calculated as Al and/or SiO


2


) based on the total weight of the particles.




Various properties of the acicular hematite particles which are coated with above-mentioned coating material, such as aspect ratio, average major axis diameter, average minor axis diameter, BET specific surface area, geometrical standard deviation of major axis diameter, geometrical standard deviation of minor axis diameter and degree of densification are approximately equivalent in values to those of the acicular hematite particles in which the surfaces thereof is not coated with the above-mentioned coating material.




The process for producing the acicular hematite particles according to the present invention is exemplified as follows.




The acicular hematite particles for a non-magnetic undercoat layer of a magnetic recording medium according to the present invention are produced by the following processes (I) and (II).




(I) The acicular hematite particles according to the present invention can be obtained by subjecting acicular hematite particles to be treated to acid-dissolving treatment under specific conditions.




The acicular hematite particles to be treated can be produced by various methods. Examples of these methods may include a method of directly producing the hematite particles by a wet process; a method of producing akaganeite particles (β-FeOOH) and then heat-dehydrating the akaganeite particles; or the like. As an ordinary production method, there may be industrially preferably used a method of producing acicular goethite particles as a precursor of the acicular hematite particles by the following wet process and then heat-dehydrating the obtained acicular goethite particles.




An ordinary method of producing acicular goethite particles as one of precursors of the acicular hematite particles is described below.




As described hereinafter, the acicular goethite particles can be produced by passing an oxygen-containing gas through a suspension containing ferrous precipitates such as hydroxides of iron or iron carbonate which are obtained by reacting a ferrous salt with either alkali hydroxide, alkali carbonate or mixed alkali composed of alkali hydroxide and alkali carbonate.




Acicular goethite particles are produced by an ordinary method:




(A) a method of producing needle-shaped goethite particles comprising oxidizing a suspension having a pH value of not less than 11 and containing colloidal ferrous hydroxide particles which is obtained by adding not less than an equivalent of an alkali hydroxide solution to an aqueous ferrous salt solution, by passing an oxygen-containing gas thereinto at a temperature of not higher than 80° C.;




(B) a method of producing spindle-shaped goethite particles comprising oxidizing a suspension containing FeCO


3


which is obtained by reacting an aqueous ferrous salt solution with an aqueous alkali carbonate solution, by passing an oxygen-containing gas thereinto after aging the suspension, if necessary;




(C) a method of producing spindle-shaped goethite particles comprising oxidizing a suspension containing precipitates containing iron which is obtained by reacting an aqueous ferrous salt solution with an aqueous alkali carbonate solution and an alkali hydroxide solution, by passing an oxygen-containing gas thereinto after aging the suspension, if necessary;




(D) a method of growing needle-shaped seed goethite particles comprising oxidizing a ferrous hydroxide solution containing colloidal ferrous hydroxide particles which is obtained by adding less than an equivalent of an alkali hydroxide solution or an alkali carbonate solution to an aqueous ferrous salt solution, by passing an oxygen-containing gas thereinto, thereby producing needle-shaped seed goethite particles, adding not less than an equivalent of an alkali hydroxide solution to the Fe


2+


in the aqueous ferrous salt solution, to the aqueous ferrous salt solution containing the needle-shaped seed goethite particles, and passing an oxygen-containing gas into the aqueous ferrous salt solution;




(E) a method of growing needle-shaped seed goethite particles comprising oxidizing a ferrous hydroxide solution containing colloidal ferrous hydroxide particles which is obtained by adding less than an equivalent of an alkali hydroxide solution or an alkali carbonate solution to an aqueous ferrous salt solution, by passing an oxygen-containing gas thereinto, thereby producing needle-shaped seed goethite particles, adding not less than an equivalent of an aqueous alkali carbonate solution to the Fe


2+


in the aqueous ferrous salt solution, to the aqueous ferrous salt solution containing the needle-shaped seed goethite particles, and passing an oxygen-containing gas into the aqueous ferrous salt solution; and




(F) a method of growing needle-shaped seed goethite particles comprising oxidizing a ferrous hydroxide solution containing colloidal ferrous hydroxide particles which is obtained by adding less than an equivalent of an alkali hydroxide solution or an alkali carbonate solution to an aqueous ferrous salt solution, by passing an oxygen-containing gas thereinto, thereby producing needle-shaped seed goethite particles and growing the obtained needle-shaped seed goethite particles in an acidic or neutral region.




Elements other than Fe such as Ni, Zn, P and Si, which are generally added in order to enhance various properties of the particles such as the major axis diameter, the minor axis diameter and the aspect ratio, may be added during the reaction system for producing the goethite particles.




The acicular goethite particles obtained have an average major axial diameter of usually 0.005 to 0.4 μm, an average minor axial diameter of usually 0.0025 to 0.20 μm, a geometrical standard deviation of the major axis diameter of not more than 1.70, a geometrical standard deviation of the minor axis diameter of 1.37 to 1.50 and a BET specific surface area of about usually 50 to 250 m


2


/g, and contain soluble sodium salts of usually 300 to 1500 ppm (calculated as Na) and ordinarily soluble sulfates of 150 to 3000 ppm (calculated as SO


4


).




Alternatively, the acicular hematite particles to be treated which contain aluminum therewithin in an amount of 0.05 to 50% by weight (calculated as Al) based on the total weight of the particles, can be produced by containing aluminum in the acicular goethite particles by preliminarily adding an aluminum compound upon the above-mentioned production reaction of the acicular goethite particles.




Further, in the production reaction of the acicular goethite particles which contain aluminum within the particle, an aluminum compound may be added to at least one solution selected from suspensions containing a ferrous salt, alkali hydroxide, alkali carbonate, mixed alkali composed of alkali hydroxide and alkali carbonate, or ferrous precipitates such as hydroxides of iron or iron carbonate. It is preferred that the aluminum compound is added to an aqueous ferrous salt solution.




As the above-mentioned aluminum compounds, there may be used aluminum salts such as aluminum acetate, aluminum sulfate, aluminum chloride or aluminum nitrate, alkali aluminates such as sodium aluminate, alumina sol, aluminum hydroxide or the like.




The amount of the aluminum compound added is 0.05 to 50% by weight (calculated as Al) based on the total weight of the particles.




The obtained acicular goethite particles usually have an average major axial diameter of ordinarily 0.005 to 0.4 μm, an average minor axial diameter of ordinarily 0.0025 to 0.20 μm, a geometrical standard deviation of the major axis diameter of not more than 1.70, a geometrical standard deviation of the minor axis diameter of 1.37 to 1.50 and a BET specific surface area of about ordinarily 50 to 250 m


2


/g, contain aluminum in an amount of usually 0.05 to 50% by weight (calculated as Al) based on the total weight of the particles, and contain soluble sodium salts of usually 300 to 1500 ppm (calculated as Na) and soluble sulfates of usually 100 to 3000 ppm (calculated as SO


4


).




Next, there is described a process for producing acicular hematite particles to be treated, which may substantially uniformly containing aluminum within the particle.




The acicular hematite particles which may substantially uniformly contain aluminum within the particle may be produced by heat-dehydrating the above-mentioned acicular goethite particles which may substantially uniformly contain aluminum within the particle.




The temperature of the heat-dehydration is preferably 550 to 850° C. to obtain high-density acicular hematite particles which may substantially uniformly contain aluminum within the particle.




Especially, in the case where the heat-dehydration is conducted at an elevated temperature as high as not less than 550° C., it is preferred that the surface of the acicular goethite particle which may substantially uniformly contain aluminum within the particle, is coated with an anti-sintering agent prior to the heat-dehydration, as is well known in the art.




As the sintering preventive, sintering preventives generally used are usable. For example, phosphorus compounds such as sodium hexametaphosphate, polyphospholic acid and orthophosphoric acid, silicon compounds such as #3 water glass, sodium orthosilicate, sodium metasilicate and colloidal silica, boron compounds such as boric acid, aluminum compounds including aluminum salts such as aluminum acetate, aluminum sulfate, aluminum chloride and aluminum nitrate, alkali aluminate such as sodium aluminate, alumina sol and aluminum hydroxide, and titanium compounds such as titanyl sulfate may be exemplified.




The amount of the sintering preventive applied onto the surface of the acicular goethite particle is about 0.05 to 10% by weight based on the total weight of the particles, though the amount is varied depending upon kinds of sintering preventives used, pH value of the alkali aqueous solution or various conditions such as heat-treating temperature or the like.




The acicular goethite particles coated with a sintering preventive have the BET specific surface area (S


BET


) of usually about 50 to 250 m


2


/g. The coating treatment using a sintering preventive is composed of the steps of: adding a sintering preventive to an aqueous suspension containing the acicular goethite particles, mixing and stirring the resultant suspension, filtering out the particles, washing the particles with water, and drying the particles.




Meanwhile, as the acicular hematite particles to be treated, there may be preferably used high-density acicular hematite particles which may substantially uniformly contain aluminum within the particle. In the case of low-density acicular hematite particles, many dehydration pores are present within particles or on surfaces thereof. Therefore, upon subjecting the particles to the acid-dissolving treatment, the dissolution is initiated from the dehydration pores, so that the particle shape can be no longer maintained, resulting in deteriorated dispersibility of the obtained particles.




In order to obtain high-density acicular hematite particles which can maintain a particle shape of the acicular goethite particles, it is preferred that the acicular goethite particles which may substantially uniformly contain aluminum within the particle, are first heat-treated at a temperature as low as not less than 250° C. and less than 550° C. to form low-density acicular hematite particles which may contain aluminum which is present within the particle, and then the low-density hematite particles are heat-treated at an elevated temperature as high as 550 to 850° C.




If the temperature for heat-treating the goethite particles is less than 250° C., the dehydration reaction takes a long time. On the other hand, if the temperature is not less than 550° C., the dehydration reaction is abruptly brought out, so that it is difficult to retain the shapes because the sintering between particles is caused. The low-density acicular hematite particles obtained by heat-treating the acicular goethite particles at a low temperature are low-density particles having a large number of dehydration pores through which H


2


O is removed from the acicular goethite particles and the BET specific surface area thereof is about 1.2 to 2 times larger than that of the acicular goethite particles as the precursor.




The low-density acicular hematite particles obtained by heat-treating the acicular goethite particles coated with a sintering preventive at a temperature of not less than 250° C. and less than 550° C., have an average major axis diameter of usually 0.005 to 0.30 μm, an average minor axis diameter of usually 0.0025 to 0.15 μm, a geometrical standard deviation of a major axis diameter of usually not more than 1.70, a geometrical standard deviation of a minor axis diameter of usually 1.37 to 1.50 and a BET specific surface area (S


BET


) of usually about 70 to 350 m


2


/g, and contain ordinarily soluble sodium salts of usually 300 to 1500 ppm (calculated as Na) and ordinarily soluble sulfates of usually 100 to 3000 ppm (calculated as SO


4


).




The low-density acicular hematite particles containing aluminum which is present within the particle, obtained by heat-treating the acicular goethite particles coated with a sintering preventive at a temperature of not less than 250° C. and less than 550° C., have an average major axis diameter of usually 0.005 to 0.30 μm, an average minor axis diameter of usually 0.0025 to 0.15 μm, a geometrical standard deviation of a major axis diameter of usually not more than 1.70, a geometrical standard deviation of a minor axis diameter of usually 1.37 to 1.50 and a BET specific surface area (S


BET


) of usually about 70 to 350 m


2


/g, and containing aluminum in an amount of 0.05 to 50% by weight (calculated as Al) based on the total weight of the particles, and contain soluble sodium salts of usually 500 to 3000 ppm (calculated as Na) and soluble sulfates of usually 300 to 4000 ppm (calculated as SO


4


).




The low-density acicular hematite particles which may substantially uniformly contain aluminum within the particle, are then heat-treated at a temperature of usually 550 to 850° C., preferably 550 to 800° C. to obtain a high-density acicular hematite particles which may substantially uniformly contain aluminum within the particle. If the heat-treating temperature is less than 550° C., since the densification may be insufficient, a large number of dehydration pores may exist within and on the surface of the acicular hematite particles, so that the dispersion in the vehicle may become insufficient. Further, when the non-magnetic undercoat layer is formed from these particles, it may be difficult to obtain a coating film having a smooth surface. On the other hand, if the temperature exceeds 850° C., although the densification of the acicular hematite particles may be sufficient, since sintering is caused on and between particles, the particle size may increase, so that it may be difficult to obtain a coating film having a smooth surface.




The BET specific surface area of the high-density acicular hematite particles having the average major axis diameter of usually 0.005 to 0.30 μm, the average minor axis diameter of usually 0.0025 to 0.15 μm, the geometrical standard deviation of a major axis diameter of usually not more than 1.70 and the geometrical standard deviation of a minor axis diameter of usually 1.37 to 1.50, is usually about 35 to 180 m


2


/g. The high-density acicular hematite particles contain soluble sodium salts of usually 500 to 4000 ppm (calculated as Na) and soluble sulfates of usually 300 to 5000 ppm (calculated as SO


4


).




The BET specific surface area of the high-density acicular hematite particles having the average major axis diameter of usually 0.005 to 0.30 μm, the average minor axis diameter of usually 0.0025 to 0.15 μm, the geometrical standard deviation of a major axis diameter of usually not more than 1.70 and the geometrical standard deviation of a minor axis diameter of usually 1.37 to 1.50, and containing aluminum within the particle, is usually about 35 to 180 m


2


/g. The high-density acicular hematite particles contain soluble sodium salts of usually 500 to 4000 ppm (calculated as Na) and soluble sulfates of usually 300 to 5000 ppm (calculated as SO


4


), and contain aluminum in amount of 0.05 to 50% by weight (calculated as Al) based on the total weight of the particles.




The high-density acicular hematite particles which may substantially uniformly contain aluminum within the particle, are diaggregated by a dry-process, and formed into a slurry. The coarse particles thereof contained in the slurry are then deagglomerated by a wet-process. In the wet-deagglomeration, ball mill, sand grinder, colloid mill or the like is used until the coarse particles having a particle size of at least 44 μm are substantially removed. That is, the wet-pulverization is carried out until the amount of the coarse particles having a particle size of not less than 44 μm becomes to usually not more than 10% by weight, preferably not more than 5% by weight, more preferably 0% by weight based on the total weight of the particles. If the amount of the coarse particles having a particle size of not less than 44 μm is more than 10% by weight, the effect of treating the particles in an acid-dissolving treatment at the next step is not attained.




Next, there is described a process for producing acicular hematite particles having a specific geometrical standard deviation of the minor axis diameter.




The acicular hematite particles may be produced by subjecting a water suspension of acicular hematite particles as particles to be treated to an acid-dissolving treatment at an acid concentration of not less than 1.0 N, a pH value of not more than 3.0 and a temperature of 20 to 100° C. so as to dissolve 5 to 50% by weight of the acicular hematite particles based on the total weight of acicular hematite particles present in the water suspension, followed by washing with water; adding an aqueous alkali solution to the water suspension containing residual acicular hematite particles so as to adjust the pH value of the water suspension to not less than 13; and then heat-treating the water suspension at a temperature of 80 to 103° C., followed by filtering, washing with water and drying.




First, the acicular hematite particles to be treated with acid, are described below.




The particle shape of the hematite particles to be treated, is an acicular shape. The “acicular” shape may include not only a needle shape but also a spindle shape or a rice ball shape. In addition, the aspect ratio of the particles is usually 2:1 to 20:1.




The average major axis diameter of the acicular hematite particles to be treated, is usually 0.005 to 0.3 μm, preferably 0.02 to 0.28 μm.




The average minor axis diameter of the acicular hematite particles to be treated, is usually 0.0025 to 0.15 μm, preferably 0.01 to 0.14 μm.




The geometrical standard deviation of the major axis diameter of the acicular hematite particles to be treated, is usually not more than 1.70, and the geometrical standard deviation of the minor axis diameter of the acicular hematite particles to be treated, is usually 1.37 to 1.50.




The BET specific surface area (S


BET


) of the acicular hematite particles to be treated, is usually 35 to 180 m


2


/g.




The acicular hematite particles to be treated contain soluble sodium salts of usually 500 to 4000 ppm (calculated as Na) and soluble sulfates of usually 300 to 5000 ppm (calculated as SO


4


).




The acicular hematite particles to be treated, may contain aluminum in an amount of usually 0.05 to 50% by weight (calculated as Al) which is present within the particle.




Next, the acid-dissolving treatment of the acicular hematite particles to be treated is described in detail.




The concentration of the acicular hematite particles in the water suspension is usually 1 to 500 g/liter, preferably 10 to 250 g/liter. When the concentration of the acicular hematite particles in the water suspension is less than 1 g/liter, the amount of the particles treated is too small, which is industrially disadvantageous. On the other hand, when the concentration of the acicular hematite particles in the water suspension is more than 500 g/liter, it becomes difficult to evenly subject the particles to the acid-dissolving treatment.




As the acids, there may be used any of sulfuric acid, hydrochloric acid, nitric acid, sulfurous acid, chloric acid, perchloric acid and oxalic acid. With the consideration of corrosion or deterioration of a container in which a high-temperature treatment or a dissolving treatment is conducted, economy or the like, sulfuric acid is preferred.




The concentration of the acid is usually not less than 1.0 N, preferably not less than 1.2 N, more preferably not less than 1.5 N. The upper limit of concentration of the acid is preferably 5 N. When the acid concentration is less than 1.0 N, the dissolution of the acicular hematite particles requires an extremely long period of time and is, therefore, industrially disadvantageous.




Upon the acid-dissolving treatment, the initial pH value is usually not more than 3.0, preferably not more than 2.0, more preferably not more than 1.0. With the consideration of the dissolving time or the like, it is industrially preferred that the pH value is not more than 1.0. When the pH value is more than 3.0, the dissolution of the acicular hematite particles requires an extremely long period of time and is, therefore, industrially disadvantageous.




The temperature of the water suspension is usually 20 to 100° C., preferably 50 to 100° C., more preferably 70 to 100° C. When the temperature of the water suspension is less than 20° C., the dissolution of the acicular hematite particles requires an extremely long period of time and is, therefore, industrially disadvantageous. On the other hand, when the temperature of the water suspension is more than 100° C., the dissolution of the particles proceeds too rapidly, so that it becomes difficult to control the dissolving treatment. Further, in that case, the dissolving treatment requires a special apparatus such as autoclave, resulting in industrially disadvantageous process.




Incidentally, in the case where the acicular hematite particles to be treated have a relatively large average major axis diameter, i.e., in the range of 0.05 to 0.30 μm, it is preferred that the dissolving treatment is conducted under the hard conditions, e.g., at a pH value of not more than 1.0 and a temperature of 70 to 100° C. On the other hand, in the case where the acicular hematite particles to be treated have a relatively small average major axis diameter, i.e., in the range of 0.005 to 0.05 μm, it is preferred that the dissolving treatment is conducted under the soft conditions, e.g., at a pH value of 1.0 to 3.0 and a temperature of 20 to 70° C.




The dissolving treatment with acid may be conducted until the amount of the acicular hematite particles dissolved reaches 5 to 50% by weight, preferably 10 to 45% by weight, more preferably 15 to 40% by weight based on the total weight of the acicular hematite particles to be treated. When the amount of the acicular hematite particles dissolved is less than 5% by weight, the fine particle components may not be sufficiently removed by the dissolving treatment. On the other hand, when the amount of the acicular hematite particles dissolved is more than 50% by weight, the particles as a whole may be finely divided and the dissolving loss is increased, resulting in industrially disadvantageous process.




Incidentally, the aqueous solution in which iron salts are dissolved in the above dissolving treatment, is separated from the slurry by filtration. From the standpoint of the reuse of resources, the thus-separated iron salts may be used as a raw material of the ferrous salt used for the production of acicular goethite particles.




After completion of the above acid-dissolving treatment with acid, the acicular hematite particles remaining in the water suspension is filtered, washed with water and dried.




As the water-washing methods, there may be used those ordinarily used in industrial fields, such as a washing method by decantation, a washing method conducted according to a diluting process by using a filter thickener, a washing method of feeding water through a filter press, or the like.




(II) The acicular hematite particles according to the present invention are produced by heat-treating the specific acicular goethite particles which are produced by the afore-mentioned method, at a temperature of 100 to 200° C., whereby superfine goethite particles are adhered to the surface of the acicular goethite particles, and heat-treating at a temperature of 550 to 850° C.




As the acicular goethite particles as precursor, acicular goethite particles having an average major axis diameter of usually 0.01 to 0.25 μm and a geometrical standard deviation of a minor axis diameter of usually 1.37 to 1.50, are used. Especially, acicular goethite particles having an average major axis diameter of usually 0.01 to 0.25 μm, an average minor axis diameter of usually 0.05 to 0.17 μm, a geometrical standard deviation of a major axis diameter of usually not more than 1.70, a geometrical standard deviation of a minor axis diameter of usually 1.37 to 1.50, and a BET specific surface area (S


BET


) of usually 50 to 250 m


2


/g, containing soluble sodium salts of usually 500 to 1500 ppm (calculated as Na) and soluble sulfates of usually 150 to 3000 ppm (calculated as SO


4


), are preferable.




Also, the acicular goethite particles which substantially uniformly contain aluminum within the particle as starting particles, have an average major axis diameter of usually 0.01 to 0.25 μm and a geometrical standard deviation of a minor axis diameter of usually 1.37 to 1.50, are used. Especially, acicular goethite particles having an average major axis diameter of usually 0.01 to 0.25 μm, an average minor axis diameter of usually 0.05 to 0.17 μm, a geometrical standard deviation of a major axis diameter of usually not more than 1.70, a geometrical standard deviation of a minor axis diameter of usually 1.37 to 1.50, and a BET specific surface area (S


BET


) of usually 50 to 250 m


2


/g, and containing aluminum in amount of 0.05 to 50% by weight (calculated as Al) based on the total weight of the particles and containing soluble sodium salts of usually 500 to 1500 ppm (calculated as Na) and soluble sulfates of usually 150 to 3000 ppm (calculated as SO


4


), are preferable.




When the heating temperature is less than 100° C., it may be difficult to absorb a sufficient amount of the superfine goethite particles into the acicular goethite particles, thereby failing to obtain particles having a uniform particle size. On the other hand, when the heating temperature is more than 200° C., the acicular goethite particles is heat-dehydrated under such a condition that the superfine goethite particles still remain therein. As a result, the sintering between the particles is disadvantageously caused, thereby also failing to obtain particles having a uniform particle size. With the consideration of industrial productivity or the like, the heat-treating temperature is preferably 120 to 200° C.




The heat-treating time is preferably 5 to 60 minutes.




The acicular goethite particles obtained by heat-treating at a temperature of 100 to 200° C., have an average major axis diameter of usually 0.011 to 0.26 μm, and a geometrical standard deviation of minor axis diameter of usually not more than 1.30.




Especially, it is preferred that the acicular goethite particles obtained by heat-treating at a temperature of 100 to 200° C., have an average major axis diameter of usually 0.011 to 0.26 μm, an average minor axis diameter of usually 0.0055 to 0.13 μm, a geometrical standard deviation of major axis diameter of usually not more than 1.50, a geometrical standard deviation of minor axis diameter of usually not more than 1.30, and a BET specific surface area (S


BET


) of usually 50 to 250 m


2


/g, and contain soluble sodium salts of usually 300 to 1500 ppm (calculated as Na) and soluble sulfates of usually 150 to 3000 ppm (calculated as SO


4


).




Also, it is preferred that the acicular goethite particles which substantially uniformly contain aluminum within the particle as starting particles and are obtained by heat-treating at a temperature of 100 to 200° C., have an average major axis diameter of usually 0.011 to 0.26 and a geometrical standard deviation of a minor axis diameter of usually not more than 1.30, and containing aluminum in amount of 0.05 to 50% by weight (calculated as Al) based on the total weight of the particles.




Especially, the acicular goethite particles which substantially uniformly contain aluminum within the particle as starting particles and are obtained by heat-treating at a temperature of 100 to 200° C., have an average major axis diameter of usually 0.011 to 0.26, an average minor axis diameter of usually 0.0055 to 0.13 μm, a geometrical standard deviation of a major axis diameter of usually not more than 1.50, a geometrical standard deviation of a minor axis diameter of usually not more than 1.30, and a BET specific surface area (S


BET


) of usually 50 to 250 m


2


/g, and containing aluminum in amount of 0.05 to 50% by weight (calculated as Al) based on the total weight of the particles, and contain soluble sodium salts of usually 300 to 1500 ppm (calculated as Na) and soluble sulfates of usually 150 to 3000 ppm (calculated as SO


4


).




The obtained acicular goethite particles are heat-treated at 550 to 850° C., thereby producing acicular hematite particles.




Incidentally, as the acicular hematite particles according to the present invention, high-density acicular hematite particles produced by heat-treating acicular goethite particles at 100 to 200° C., heat-dehydrating the acicular goethite particles at 250 to 500° C., thereby obtaining low-density acicular hematite particles, and then heat-treating the obtained low-density acicular hematite particles at a temperature as high as 550 to 850° C., are preferable.




Next, the high-purification treatment of the acicular hematite particles is explained.




The high-density acicular hematite particles having a specific geometrical standard deviation of a minor axis diameter, which may substantially uniformly contain aluminum within the particle, are diaggregated by a dry-process, and formed into a slurry. The coarse particles thereof contained in the slurry are then deagglomerated by a wet-process. In the wet-deagglomeration, ball mill, sand grinder, colloid mill or the like is used until the coarse particles having a particle size of at least 44 μm are substantially removed. That is, the wet-pulverization is carried out until the amount of the coarse particles having a particle size of not less than 44 μm becomes to usually not more than 10% by weight, preferably not more than 5% by weight, more preferably 0% by weight based on the total weight of the particles. If the amount of the coarse particles having a particle size of not less than 44 μm is more than 10% by weight, the effect of treating the particles in a high-purification treatment at the next step is not attained.




The acicular hematite particles for a non-magnetic undercoat layer of a magnetic recording medium according to the present invention can be produced by adding an aqueous alkali solution to a water suspension containing acicular hematite particles so as to adjust the pH value of the water suspension to not less than 13, and then heat-treating the water suspension at 80 to 103° C., followed by filtering, washing with water and drying.




Upon the addition of the aqueous alkali solution, it is preferred that a filter cake obtained by filtering and water-washing the water suspension containing the acicular hematite particles, is preliminarily dispersed in water, thereby forming a water suspension again, or that the water suspension containing the acicular hematite particles is preliminarily washed with water by a decantation method.




The concentration of the alkaline suspension containing the acicular hematite particles is preferably 50 to 250 g/liter.




As the above-mentioned aqueous alkali solution, there may be used aqueous solutions containing alkali hydroxides such as sodium hydroxide, potassium hydroxide, calcium hydroxide or the like.




If the pH value of the aqueous alkali solution containing the acicular hematite particles is less than 13, it is difficult to effectively remove the solid crosslinking caused by the sintering preventive which exists on the surfaces of the acicular hematite particles, so that it is difficult to wash out the soluble sodium salt, soluble sulfate, etc. existing within and on the surfaces of the particles. The upper limit of the pH value is about 14. In consideration of the effect of removing the solid crosslinking caused by the sintering preventive which exists on the surfaces of the acicular hematite particles, the effect of washing out the soluble sodium slat, soluble sulfate, etc., and the effect of removing the alkali which adheres to the surfaces of acicular hematite particles in the process of treatment with the aqueous alkali solution, the preferable pH value is in the range of 13.1 to 13.8.




The heating temperature in the aqueous alkali suspension is preferably 80 to 103° C., more preferably 90 to 100° C. If the temperature is lower than 80° C., it is difficult to effectively remove the solid crosslinking caused by the sintering preventive which exists on the surfaces of the acicular hematite particles. If the heating temperature exceeds 103° C., although it is possible to effectively remove the solid crosslinking, since an autoclave is necessary or the treated solution boils under a normal pressure, it is not advantageous from the point of view of industry.




The acicular hematite particles heat-treated in the aqueous alkali suspension are thereafter filtered out and washed with water by an ordinary method so as to remove the soluble sodium salt and soluble sulfate which are washed out of the interiors and the surfaces of the particles and to remove the alkali adhered to the surfaces of the acicular hematite particles in the process of treatment with the aqueous alkali solution, and then dried.




As the method of washing the acicular hematite particles with water, a method generally industrially used such as a decantation method, a dilution method using a filter thickener and a method of passing water into a filter press is adopted.




If the soluble sodium salt and soluble sulfate which are contained within the acicular hematite particles are washed out with water, even if soluble sodium salt and soluble sulfate adhere to the surfaces when the surfaces of the acicular hematite particles are coated with a coating material, the soluble sodium salt and soluble sulfate can be easily removed by water washing.




The acicular hematite particles for a non-magnetic undercoat layer of a magnetic recording medium according to the present invention, may be coated with at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon, if required.




In order to coat the acicular hematite particles, an aluminum compound and/or a silicon compound is added to an aqueous suspension containing the acicular hematite particles, and mixed under stirring. After mixing and stirring, the pH value of the mixed solution is adjusted by using an alkali or acid, if necessary. The acicular hematite particles thus coated with at least one selected from the group consisting of a hydroxide of aluminum, an oxide of aluminum, a hydroxide of silicon and an oxide of silicon are then filtered out, washed with water, dried and pulverized. They may be further deaerated and compacted, if necessary.




As the aluminum compound for the coating, the same aluminum compounds as those described above as the sintering preventive are usable.




The amount of aluminum compound added is usually 0.01 to 50% by weight (calculated as Al) based on the total weight of the particles. If the amount is less than 0.01% by weight, the dispersibility-improving effect in the vehicle may be insufficient. On the other hand, if the amount exceeds 50% by weight, the coating dispersibility-improving effect becomes saturated, so that it is meaningless to add an aluminum compound more than necessary.




As the silicon compound, the same silicon compounds as those described above as the sintering preventive are usable.




The amount of silicon compound added is 0.01 to 50% by weight (calculated as SiO


2


) based on the total weight of the particles. If the amount is less than 0.01% by weight, the improvement of the dispersibility in the vehicle may be insufficient. On the other hand, if the amount exceeds 50.00% by weight, the coating dispersibility-improving effect becomes saturated, so that it is meaningless to add an silicon compound more than necessary.




When both an aluminum compound and a silicon compound are used, the amount thereof used is preferably 0.01 to 50% by weight (calculated as Al and SiO


2


) based on the total weight of the particles.




Next, the magnetic recording medium according to the present invention is described.




The magnetic recording medium according to the present invention comprises:




a non-magnetic base film;




a non-magnetic undercoat layer formed on the non-magnetic base film, comprising a binder resin and the acicular hematite particles; and




a magnetic coating film formed on the non-magnetic undercoat layer, comprising a binder resin and magnetic particles.




Firstly, the non-magnetic substrate having the non-magnetic undercoat layer according to the present invention is described.




The non-magnetic substrate according to the present invention comprises:




a non-magnetic base film; and




a non-magnetic undercoat layer formed on said non-magnetic base film, comprising a binder resin and the acicular hematite particles.




The non-magnetic substrate of the present invention is produced by forming a coating film on the base film and drying the coating film. The coating film is formed by applying a non-magnetic coating composition which contains the acicular hematite particles, a binder resin and a solvent, to the surface of the base film.




As the base film, the following materials which are at present generally used for the production of a magnetic recording medium are usable as a raw material: a synthetic resin such as polyethylene terephthalate, polyethylene, polypropylene, polycarbonate, polyethylene naphthalate, polyamide, polyamideimide and polyimide; foil and plate of a metal such as aluminum and stainless steel; and various kinds of paper. The thickness of the base film varies depending upon the material, but it is usually about 1.0 to 300 μm, preferably 2.0 to 200 μm.




In the case of a magnetic disc, polyethylene terephthalate is usually used as the base film, and the thickness thereof is usually 50 to 300 μm, preferably 60 to 200 μm.




In a magnetic tape, when polyethylene terephthalate is used as the base film, the thickness thereof is usually 3 to 100 μm, preferably 4 to 20 μm; when polyethylene naphthalate is used, the thickness thereof is usually 3 to 50 μm, preferably 4 to 20 μm; and when polyamide is used, the thickness thereof is usually 2 to 10 μm, preferably 3 to 7 μm.




As the binder resin used in the present invention, the following resins which are at present generally used for the production of a magnetic recording medium are usable: vinyl chloride-vinyl acetate copolymer, urethane resin, vinyl chloride-vinyl acetate-maleic acid copolymer, urethane elastomer, butadiene-acrylonitrile copolymer, polyvinyl butyral, cellulose derivative such as nitrocellulose, polyester resin, synthetic rubber resin such as polybutadiene, epoxy resin, polyamide resin, polyisocyanate, electron radiation curing acryl urethane resin and mixtures thereof. Each of these resin binders may contain a functional group such as —OH, —COOH, —SO


3


M, —OPO


2


M


2


and —NH


2


, wherein M represents H, Na or K. With the consideration of the dispersibility of the particles, a binder resin containing a functional group —COOH or —SO


3


M is preferable.




The mixing ratio of the acicular hematite particles with the binder resin is usually 5 to 2000 parts by weight, preferably 100 to 1000 parts by weight based on 100 parts by weight of the binder resin.




As the solvents, there may be used methyl ethyl ketone, toluene, cyclohexanone, methyl isobutyl ketone, tetrahydrofuran, a mixture of these solvents or the like.




The total amount of the solvent used is 50 to 1,000 parts by weight based on 100 parts by weight of the acicular hematite particles. When the amount of the solvent used is less than 50 parts by weight, the viscosity of the non-magnetic coating composition prepared therefrom becomes too high, thereby making it difficult to apply the non-magnetic coating composition. On the other hand, when the amount of the solvent used is more than 1,000 parts by weight, the amount of the solvent volatilized during the formation of the coating film becomes too large, thereby rendering the coating process industrially disadvantageous.




It is possible to add a lubricant, a polishing agent, an antistatic agent, etc. which are generally used for the production of a magnetic recording medium to the non-magnetic undercoat layer.




The thickness of the non-magnetic undercoat layer obtained by applying a non-magnetic coating composition on the surface of the base film and drying, is usually 0.2 to 10.0 μm, preferably 0.5 to 5.0 μm. If the thickness is less than 0.2 μm, not only it is impossible to ameliorate the surface roughness of the non-magnetic substrate but also the strength is insufficient. If the thickness is more than 10 μm, it is difficult to reduce the thickness of the magnetic recording medium.




In case of using the acicular hematite particles as defined in first aspect as non-magnetic particles, the non-magnetic substrate according to the present invention has a gloss (of the coating film) of usually 189 to 300%, preferably 194 to 300%, more preferably 198 to 300%; a surface roughness Ra (of the coating film) of usually 0.5 to 9.6 nm, preferably 0.5 to 9.1 nm, more preferably 0.5 to 8.6 nm; a Young's modulus (relative value to a commercially available video tape: and AV T-120 produced by Victor Company of Japan, Limited) of usually 120 to 160, preferably 121 to 160.




In case of using the acicular hematite particles as defined in second aspect as non-magnetic particles, the non-magnetic substrate according to the present invention has a gloss (of the coating film) of usually 191 to 300%, preferably 196 to 300%, more preferably 201 to 300%; a surface roughness Ra (of the coating film) of usually 0.5 to 9.4 nm, preferably 0.5 to 8.9 nm, more preferably 0.5 to 8.4 nm; a Young's modulus (relative value to a commercially available video tape: and AV T-120 produced by Victor Company of Japan, Limited) of usually 122 to 160, preferably 124 to 160.




In case of using the acicular hematite particles as defined in third aspect as non-magnetic particles, the non-magnetic substrate according to the present invention has a gloss (of the coating film) of usually 191 to 300%, preferably 196 to 300%, more preferably 201 to 300%; a surface roughness Ra (of the coating film) of usually 0.5 to 9.3 nm, preferably 0.5 to 8.8 nm, more preferably 0.5 to 8.3 nm; a Young's modulus (relative value to a commercially available video tape: and AV T-120 produced by Victor Company of Japan, Limited) of usually 122 to 160, preferably 124 to 160.




In case of using the acicular hematite particles as defined in fourth aspect as non-magnetic particles, the non-magnetic substrate according to the present invention has a gloss (of the coating film) of usually 193 to 300%, preferably 198 to 300%, more preferably 203 to 300%; a surface roughness Ra (of the coating film) of usually 0.5 to 9.1 nm, preferably 0.5 to 8.6 nm, more preferably 0.5 to 8.1 nm; a Young's modulus (relative value to a commercially available video tape: and AV T-120 produced by Victor Company of Japan, Limited) of usually 124 to 160, preferably 126 to 160.




In case of using the acicular hematite particles as defined in ninth aspect as non-magnetic particles, the non-magnetic substrate according to the present invention has a gloss (of the coating film) of usually 193 to 300%, preferably 198 to 300%, more preferably 203 to 300%; a surface roughness Ra (of the coating film) of usually 0.5 to 9.0 nm, preferably 0.5 to 8.5 nm, more preferably 0.5 to 8.0 nm; a Young's modulus (relative value to a commercially available video tape: and AV T-120 produced by Victor Company of Japan, Limited) of usually 124 to 160, preferably 126 to 160.




In case of using the acicular hematite particles as defined in tenth aspect as non-magnetic particles, the non-magnetic substrate according to the present invention has a gloss (of the coating film) of usually 195 to 300%, preferably 200 to 300%, more preferably 205 to 300%; a surface roughness Ra (of the coating film) of usually 0.5 to 8.8 nm, preferably 0.5 to 8.3 nm, more preferably 0.5 to 7.8 nm; a Young's modulus (relative value to a commercially available video tape: and AV T-120 produced by Victor Company of Japan, Limited) of usually 126 to 160, preferably 128 to 160.




In case of using the acicular hematite particles as defined in eleventh aspect as non-magnetic particles, the non-magnetic substrate according to the present invention has a gloss (of the coating film) of usually 196 to 300%, preferably 201 to 300%, more preferably 206 to 300%; a surface roughness Ra (of the coating film) of usually 0.5 to 8.7 nm, preferably 0.5 to 8.2 nm, more preferably 0.5 to 7.7 nm; a Young's modulus (relative value to a commercially available video tape: and AV T-120 produced by Victor Company of Japan, Limited) of usually 126 to 160, preferably 128 to 160.




In case of using the acicular hematite particles as defined in twelfth aspect as non-magnetic particles, the non-magnetic substrate according to the present invention has a gloss (of the coating film) of usually 198 to 300%, preferably 203 to 300%, more preferably 208 to 300%; a surface roughness Ra (of the coating film) of usually 0.5 to 8.5 nm, preferably 0.5 to 8.0 nm, more preferably 0.5 to 7.5 nm; a Young's modulus (relative value to a commercially available video tape: and AV T-120 produced by Victor Company of Japan, Limited) of usually 128 to 160, preferably 130 to 160.




The magnetic recording medium according to the present invention can be produced by applying a magnetic coating composition containing the magnetic particles, a binder resin and a solvent, on the non-magnetic undercoat layer, followed by drying, to form a magnetic recording layer thereon.




As the magnetic particles used in the present invention, magnetic particles containing iron as a main component are usable.




The magnetic acicular metal particles containing iron as a main ingredient used in the present invention comprises iron and at least one selected from the group consisting of Co, Al, Ni, P, Si, Zn, Ti, B, Nd, La and Y. Further, the following magnetic acicular metal particles containing iron as a main component may be exemplified.




1) Magnetic acicular metal particles containing iron as a main component comprises iron; and cobalt of usually 0.05 to 40% by weight, preferably 1.0 to 35% by weight, more preferably 3 to 30% by weight (calculated as Co) based on the weight of the magnetic acicular metal particles containing iron as a main component.




2) Magnetic acicular metal particles containing iron as a main component comprises iron; and aluminum of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as Al) based on the weight of the magnetic acicular metal particles containing iron as a main component.




3) Magnetic acicular metal particles containing iron as a main component comprises iron; cobalt of usually 0.05 to 40% by weight, preferably 1.0 to 35% by weight, more preferably 3 to 30% by weight (calculated as Co) based on the weight of the magnetic acicular metal particles containing iron as a main component; and aluminum of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as Al) based on the weight of the magnetic acicular metal particles containing iron as a main component.




4) Magnetic acicular metal particles containing iron as a main component comprises iron; cobalt of usually 0.05 to 40% by weight, preferably 1.0 to 35% by weight, more preferably 3 to 30% by weight (calculated as Co) based on the weight of the magnetic acicular metal particles containing iron as a main component; and at least one selected from the group consisting of Nd, La and Y of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as the corresponding element) based on the weight of the magnetic acicular metal particles containing iron as a main component.




5) Magnetic acicular metal particles containing iron as a main component comprises iron; aluminum of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as Al) based on the weight of the magnetic acicular metal particles containing iron as a main component; and at least one selected from the group consisting of Nd, La and Y of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as the corresponding element) based on the weight of the magnetic acicular metal particles containing iron as a main component.




6) Magnetic acicular metal particles containing iron as a main component comprises iron; cobalt of usually 0.05 to 40% by weight, preferably 1.0 to 35% by weight, more preferably 3 to 30% by weight (calculated as Co) based on the weight of the magnetic acicular metal particles containing iron as a main component; aluminum of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as Al) based on the weight of the magnetic acicular metal particles containing iron as a main component; and at least one selected from the group consisting of Nd, La and Y of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as the corresponding element) based on the weight of the magnetic acicular metal particles containing iron as a main component.




7) Magnetic acicular metal particles containing iron as a main component comprises iron; cobalt of usually 0.05 to 40% by weight, preferably 1.0 to 35% by weight, more preferably 3 to 30% by weight (calculated as Co) based on the weight of the magnetic acicular metal particles containing iron as a main component; and at least one selected from the group consisting of Ni, P, Si, Zn, Ti, Cu and B of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as the corresponding element) based on the weight of the magnetic acicular metal particles containing iron as a main component.




8) Magnetic acicular metal particles containing iron as a main component comprises iron; aluminum of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as Al) based on the weight of the magnetic acicular metal particles containing iron as a main component; and at least one selected from the group consisting of Ni, P, Si, Zn, Ti, Cu and B of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as the corresponding element) based on the weight of the magnetic acicular metal particles containing iron as a main component.




9) Magnetic acicular metal particles containing iron as a main component comprises iron; cobalt of usually 0.05 to 40% by weight, preferably 1.0 to 35% by weight, more preferably 3 to 30% by weight (calculated as Co) based on the weight of the magnetic acicular metal particles containing iron as a main component; aluminum of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as Al) based on the weight of the magnetic acicular metal particles containing iron as a main component; and at least one selected from the group consisting of Ni, P, Si, Zn, Ti, Cu and B of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as the corresponding element) based on the weight of the magnetic acicular metal particles containing iron as a main component.




10) Magnetic acicular metal particles containing iron as a main component comprises iron; cobalt of usually 0.05 to 40% by weight, preferably 1.0 to 35% by weight, more preferably 3 to 30% by weight (calculated as Co) based on the weight of the magnetic acicular metal particles containing iron as a main component; at least one selected from the group consisting of Nd, La and Y of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as the corresponding element) based on the weight of the magnetic acicular metal particles containing iron as a main component; and at least one selected from the group consisting of Ni, P, Si, Zn, Ti, Cu and B of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as the corresponding element) based on the weight of the magnetic acicular metal particles containing iron as a main component.




11) Magnetic acicular metal particles containing iron as a main component comprises iron; aluminum of usually y 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as Al) based on the weight of the magnetic acicular metal particles containing iron as a main component; at least one selected from the group consisting of Nd, La and Y of ordinarily 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as the corresponding element) based on the weight of the magnetic acicular metal particles containing iron as a main component; and at least one selected from the group consisting of Ni, P, Si, Zn, Ti, Cu and B of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as the corresponding element) based on the weight of the magnetic acicular metal particles containing iron as a main component.




12) Magnetic acicular metal particles containing iron as a main component comprises iron; cobalt of usually 0.05 to 40% by weight, preferably 1.0 to 35% by weight, more preferably 3 to 30% by weight (calculated as Co) based on the weight of the magnetic acicular metal particles containing iron as a main component; aluminum of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as Al) based on the weight of the magnetic acicular metal particles containing iron as a main component; at least one selected from the group consisting of Nd, La and Y of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as the corresponding element) based on the weight of the magnetic acicular metal particles containing iron as a main component; and at least one selected from the group consisting of Ni, P, Si, Zn, Ti, Cu and B of usually 0.05 to 10% by weight, preferably 0.1 to 7% by weight (calculated as the corresponding element) based on the weight of the magnetic acicular metal particles containing iron as a main component.




The iron content in the particles is the balance, and is preferably 50 to 99% by weight, more preferably 60 to 95% by weight (calculated as Fe) based on the weight of the magnetic acicular metal particles containing iron as a main component.




The magnetic acicular metal particles containing iron as a main component comprising (i) iron and Al; (ii) iron, cobalt and aluminum, (iii) iron, aluminum and at least one rare-earth metal such as Nd, La and Y, or (iv) iron, cobalt, aluminum and at least one rare-earth metal such as Nd, La and Y is preferable from the point of the durability of the magnetic recording medium.




Further, the magnetic acicular metal particles containing iron as a main component comprising iron, containing aluminum of 0.05 to 10% by weight (calculated as Al) which are present within the particle, and optionally containing at least one rare-earth metal such as Nd, La and Y, are more preferable.




With respect to the existing position of aluminum of usually 0.05 to 10% by weight (calculated as Al) based on the weight of the magnetic acicular metal particles containing iron as a main component, it may be contained only in the core and inside portions, or in the surface portion of the magnetic acicular metal particles containing iron as a main component. Alternatively, aluminum may be approximately uniformly contained in the magnetic acicular metal particles containing iron as a main component from the core portion to the surface. An aluminum-coating layer may be formed on the surfaces of the particles. In addition, any of these positions may be combined. In the consideration of the effect of improving the surface property of the magnetic recording layer or the durability of the magnetic recording medium, magnetic acicular metal particles containing iron as a main component uniformly containing aluminum from the core portion to the surface and coated with an aluminum-coating layer are more preferable.




When the content of aluminum is less than 0.05% by weight (calculated as Al), the adsorption of the resin to the magnetic acicular metal particles containing iron as a main component in the vehicle may not be said sufficient, so that it may be difficult to produce a magnetic recording layer or a magnetic recording medium having a high durability. When the content of aluminum exceeds 10% by weight, the effect of improving the durability of the magnetic recording layer or the magnetic recording medium is observed, but the effect is saturated and it is meaningless to add aluminum more than necessary. Furthermore, the magnetic characteristics of the magnetic acicular metal particles containing iron as a main component may be sometimes deteriorated due to an increase in the aluminum as a non-magnetic component. The existing amount of aluminum of the magnetic acicular metal particles containing iron as a main component is preferably 0.1 to 7% by weight.




It is still more preferable to produce a magnetic recording medium of the present invention using the magnetic acicular metal particles containing iron as a main component containing Al and a rare-earth metal such as Nd, La and Y therein, because the magnetic recording layer or magnetic recording medium produced is apt to have a more excellent durability. Especially, magnetic acicular metal particles containing iron as a main component containing Al and Nd therein are the even more preferable.




The magnetic acicular metal particles containing iron as a main component comprising iron and aluminum within the particles are produced, as is well known, by adding an aluminum compound at an appropriate stage during the above-described process for producing acicular goethite particles to produce acicular goethite particles containing aluminum at desired positions of the particles, and heat-treating, at a temperature of 300 to 500° C., the acicular goethite particles or the acicular hematite particles containing aluminum at desired positions within the particles which are obtained by dehydrating the acicular goethite particles.




The magnetic acicular metal particles containing iron as a main component coated with aluminum are produced by heat-treating, at a temperature of 300 to 500° C., the acicular goethite particles coated with an oxide or hydroxide of aluminum, or the acicular hematite particles coated with the oxide or hydroxide of aluminum which are obtained by dehydrating the acicular goethite particles.




The magnetic particles containing iron as a main component used in the present invention have an average major axial diameter of usually 0.01 to 0.50 μm, preferably 0.03 to 0.30 μm, an average minor axial diameter of usually 0.0007 to 0.17 μm, preferably 0.003 to 0.10 μm, and an aspect ratio of usually not less than 3:1, preferably not less than 5:1. The upper limit of the aspect ratio is usually 15:1, preferably 10:1 with the consideration of the dispersibility in the vehicle. The shape of the a magnetic particles containing iron as a main component may have not only acicular but also spindle-shaped, rice ball-shaped, cubic-shaped, plate-like shaped or the like.




The geometrical standard deviation of the major axis diameter of the magnetic particles used in the present invention is preferably not more than 2.50. If it exceeds 2.50, the coarse particles existent sometimes exert a deleterious influence on the surface smoothness of the magnetic recording layer. From the point of view of industrial productivity, the lower limit of the geometrical standard deviation of the major axis diameter is preferably 1.01.




As to the magnetic properties of the magnetic acicular metal particles containing iron as a main component used in the present invention, the coercive force is usually 800 to 3500 Oe, preferably 900 to 3500 Oe, more preferably 1000 to 3500 Oe, and the saturation magnetization is usually preferably 90 to 170 emu/g, preferably 100 to 170 emu/g, more preferably 110 to 170 emu/g with the consideration of the properties such as high-density recording.




With the consideration of the durability of the magnetic recording medium, it is preferred to use magnetic acicular metal particles containing iron as a main component, which contain aluminum, as magnetic particles. The resin adsorptivity of such magnetic acicular metal particles containing iron as a main component used in the present invention is usually not less than 65%, preferably not less than 68%, more preferably not less than 70%.




As the binder resin for the magnetic recording layer, the same binder resin as that used for the production of the non-magnetic undercoat layer is usable.




The mixing ratio of the magnetic acicular metal particles containing iron as a main component with the binder resin in the magnetic recording layer is usually 200 to 2000 parts by weight, preferably 300 to 1500 parts by weight based on 100 parts by weight of the binder resin.




As the solvents, the same solvent as that used for the production of the non-magnetic undercoat layer is usable.




The total amount of the solvent used is 65 to 1,000 parts by weight based on 100 parts by weight of the magnetic particles. When the amount of the solvent used is less than 65 parts by weight, the viscosity of the magnetic coating composition prepared therefrom becomes too high, thereby making it difficult to apply the magnetic coating composition. On the other hand, when the amount of the solvent used is more than 1,000 parts by weight, the amount of the solvent volatilized during the formation of the coating film becomes too large, thereby rendering the coating process industrially disadvantageous.




It is possible to add a lubricant, a polishing agent, an antistatic agent, etc., which are generally used for the production of a magnetic recording medium to the magnetic recording layer.




The thickness of the magnetic recording layer obtained by applying the magnetic coating composition on the surface of the non-magnetic undercoat layer and dried, is usually in the range of 0.01 to 5.0 μm. If the thickness is less than 0.01 μm, uniform coating may be difficult, so that unfavorable phenomenon such as unevenness on the coating surface is observed. On the other hand, when the thickness exceeds 5.0 μm, it may be difficult to obtain desired signal recording property due to an influence of diamagnetism. The preferable thickness is in the range of 0.05 to 1.0 μm.




The magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95; a gloss (of the coating film) of usually 192 to 300%; a surface roughness Ra (of the coating film) of usually not more than 9.8 nm; a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 120 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm


−1


.




In case of using the acicular hematite particles as defined in the first aspect as non-magnetic particles, the magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe, preferably 900 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95, preferably 0.87 to 0.95; a gloss (of the coating film) of usually 192 to 300%, preferably 197 to 300%; a surface roughness Ra (of the coating film) of usually not more than 9.8 nm, preferably 0.5 to 9.3 nm,; more preferably 0.5 to 8.8 nm, a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 120 to 160, preferably 122 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm


−1


, preferably 1.20 to 2.00 μm


−1


.




In case of using the acicular hematite particles as defined in the second aspect as non-magnetic particles, the magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe, preferably 900 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95, preferably 0.87 to 0.95; a gloss (of the coating film) of usually 194 to 300%, preferably 199 to 300%; a surface roughness Ra (of the coating film) of usually not more than 9.6 nm, preferably 0.5 to 9.1 nm, more preferably 0.5 to 8.6 nm; a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 122 to 160, preferably 124 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm





, preferably 1.20 to 2.00 μm


−1


.




In case of using the acicular hematite particles as defined in the first aspect as non-magnetic particles and magnetic acicular metal particles containing iron as a main component and aluminum which are present in and/or on the surface of the particle, the magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe, preferably 900 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95, preferably 0.87 to 0.95, a gloss (of the coating film) of usually 194 to 300%, preferably 199 to 300%; a surface roughness Ra (of the coating film) of usually not more than 9.6 nm, preferably 0.5 to 9.1 nm, more preferably 0.5 to 8.6 nm; a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 122 to 160, preferably 124 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm


−1


, preferably 1.20 to 2.00 μm





. As to the durability, the running durability thereof is usually not less than 22 minutes, preferably not less than 24 minutes. Also, the scratch resistance thereof is usually A or B, preferably A.




In case of using the acicular hematite particles as defined in the second aspect as non-magnetic particles and magnetic acicular metal particles containing iron as a main component and aluminum which are present in and/or on the surface of the particle, the magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe, preferably 900 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95, preferably 0.87 to 0.95, a gloss (of the coating film) of usually 196 to 300%, preferably 201 to 300%; a surface roughness Ra (of the coating film) of usually not more than 9.4 nm, preferably 0.5 to 8.9 nm, more preferably 0.5 to 8.4 nm; a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 124 to 160, preferably 126 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm


−1


, preferably 1.20 to 2.00 μm


−1


. As to the durability, the running durability thereof is usually not less than 23 minutes, preferably not less than 25 minutes. Also, the scratch resistance thereof is usually A or B, preferably A.




In case of using the acicular hematite particles as defined in the third aspect as non-magnetic particles, the magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe, preferably 900 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95, preferably 0.87 to 0.95, a gloss (of the coating film) of usually 194 to 300%, preferably 199 to 300%; a surface roughness Ra (of the coating film) of usually not more than 9.6 nm, preferably 0.5 to 9.1 nm, more preferably 0.5 to 8.6 nm; a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 122 to 160, preferably 124 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm


−1


, preferably 1.20 to 2.00 μm


−1


. As to the durability, the running durability thereof is usually not less than 22 minutes, preferably not less than 23 minutes. Also, the scratch resistance thereof is usually A or B, preferably A.




In case of using the acicular hematite particles as defined in the fourth aspect as non-magnetic particles, the magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe, preferably 900 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95, preferably 0.87 to 0.95, a gloss (of the coating film) of usually 196 to 300%, preferably 201 to 300%; a surface roughness Ra (of the coating film) of usually not more than 9.4 nm, preferably 0.5 to 8.9 nm, more preferably 0.5 to 8.4 nm; a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 124 to 160, preferably 126 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm


−1


, preferably 1.20 to 2.00 μm


−1


. As to the durability, the running durability thereof is usually not less than 23 minutes, preferably not less than 24 minutes. Also, the scratch resistance thereof is usually A or B, preferably A.




In case of using the acicular hematite particles as defined in the third aspect as non-magnetic particles and magnetic acicular metal particles containing iron as a main component and aluminum which are present in and/or on the surface of the particle, the magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe, preferably 900 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95, preferably 0.87 to 0.95, a gloss (of the coating film) of usually 196 to 300%, preferably 201 to 300%; a surface roughness Ra (of the coating film) of usually not more than 9.4 nm, preferably 0.5 to 8.9 nm, more preferably 0.5 to 8.4 nm; a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 124 to 160, preferably 126 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm


−1


, preferably 1.20 to 2.00 μm


−1


. As to the durability, the running durability thereof is usually not less than 23 minutes, preferably not less than 24 minutes. Also, the scratch resistance thereof is usually A or B, preferably A.




In case of using the acicular hematite particles as defined in the fourth aspect as non-magnetic particles and magnetic acicular metal particles containing iron as a main component and aluminum which are present in and/or on the surface of the particle, the magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe, preferably 900 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95, preferably 0.87 to 0.95, a gloss (of the coating film) of usually 198 to 300%, preferably 203 to 300%; a surface roughness Ra (of the coating film) of usually not more than 9.2 nm, preferably 0.5 to 8.7 nm, more preferably 0.5 to 8.2 nm; a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 126 to 160, preferably 127 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm


−1


, preferably 1.20 to 2.00 μm


−1


. As to the durability, the running durability thereof is usually not less than 24 minutes, preferably not less than 26 minutes. Also, the scratch resistance thereof is usually A or B, preferably A.




In case of using the acicular hematite particles as defined in the ninth aspect as non-magnetic particles, the magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe, preferably 900 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95, preferably 0.87 to 0.95, a gloss (of the coating film) of usually 196 to 300%, preferably 201 to 300%; a surface roughness Ra (of the coating film) of usually not more than 9.4 nm, preferably 0.5 to 8.9 nm, more preferably 0.5 to 8.4 nm; a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 124 to 160, preferably 126 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm


−1


, preferably 1.20 to 2.00 μm


−1


.




In case of using the acicular hematite particles as defined in the tenth aspect as non-magnetic, the magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe, preferably 900 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95, preferably 0.87 to 0.95, a gloss (of the coating film) of usually 198 to 300%, preferably 203 to 300%; a surface roughness Ra (of the coating film) of usually not more than 9.2 nm, preferably 0.5 to 8.7 nm, more preferably 0.5 to 8.2 nm; a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 126 to 160, preferably 128 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm


−1


, preferably 1.20 to 2.00 μm


−1


.




In case of using the acicular hematite particles as defined in the ninth aspect as non-magnetic particles and magnetic acicular metal particles containing iron as a main component and aluminum which are present in and/or on the surface of the particle, the magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe, preferably 900 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95, preferably 0.87 to 0.95, a gloss (of the coating film) of usually 198 to 300%, preferably 203 to 300%; a surface roughness Ra (of the coating film) of usually not more than 9.2 nm, preferably 0.5 to 8.7 nm, more preferably 0.5 to 8.2 nm; a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 126 to 160, preferably 128 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm


−1


, preferably 1.20 to 2.00 μm


−1


. As to the durability, the running durability thereof is usually not less than 24 minutes, preferably not less than 26 minutes. Also, the scratch resistance thereof is usually A or B, preferably A.




In case of using the acicular hematite particles as defined in the tenth aspect as non-magnetic particles and magnetic acicular metal particles containing iron as a main component and aluminum which are present in and/or on the surface of the particle, the magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe, preferably 900 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95, preferably 0.87 to 0.95, a gloss (of the coating film) of usually 200 to 300%, preferably 205 to 300%; a surface roughness Ra (of the coating film) of usually not more than 9.0 nm, preferably 0.5 to 8.5 nm, more preferably 0.5 to 8.0 nm; a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 128 to 160, preferably 130 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm


−1


, preferably 1.20 to 2.00 μm


−1


. As to the durability, the running durability thereof is usually not less than 25 minutes, preferably not less than 27 minutes. Also, the scratch resistance thereof is usually A or B, preferably A.




In case of using the acicular hematite particles as defined in the eleventh aspect as non-magnetic particles, the magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe, preferably 900 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95, preferably 0.87 to 0.95, a gloss (of the coating film) of usually 198 to 300%, preferably 203 to 300%; a surface roughness Ra (of the coating film) of usually not more than 9.2 nm, preferably 0.5 to 8.7 nm, more preferably 0.5 to 8.2 nm; a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 126 to 160, preferably 128 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm


−1


, preferably 1.20 to 2.00 μm


−1


. As to the durability, the running durability thereof is usually not less than 24 minutes, preferably not less than 26 minutes. Also, the scratch resistance thereof is usually A or B, preferably A.




In case of using the acicular hematite particles as defined in the twelfth aspect as non-magnetic, the magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe, preferably 900 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95, preferably 0.87 to 0.95, a gloss (of the coating film) of usually 200 to 300%, preferably 205 to 300%; a surface roughness Ra (of the coating film) of usually not more than 9.0 nm, preferably 0.5 to 8.5 nm, more preferably 0.5 to 8.0 nm; a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 128 to 160, preferably 130 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm


−1


, preferably 1.20 to 2.00 μm


−1


. As to the durability, the running durability thereof is usually not less than 25 minutes, preferably not less than 27 minutes. Also, the scratch resistance thereof is usually A or B, preferably A.




In case of using the acicular hematite particles as defined in the eleventh aspect as non-magnetic particles and magnetic acicular metal particles containing iron as a main component and aluminum which are present in and/or on the surface of the particle, the magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe, preferably 900 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95, preferably 0.87 to 0.95, a gloss (of the coating film) of usually 200 to 300%, preferably 205 to 300%; a surface roughness Ra (of the coating film) of usually not more than 9.0 nm, preferably 0.5 to 8.5 nm, more preferably 0.5 to 8.0 nm; a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 128 to 160, preferably 130 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm


−1


, preferably 1.20 to 2.00 μm


−1


. As to the durability, the running durability thereof is usually not less than 25 minutes, preferably not less than 27 minutes. Also, the scratch resistance thereof is usually A or B, preferably A.




In case of using the acicular hematite particles as defined in the twelfth aspect as non-magnetic particles and magnetic acicular metal particles containing iron as a main component and aluminum which are present in and/or on the surface of the particle, the magnetic recording medium according to the present invention has a coercive force of usually 800 to 3500 Oe, preferably 900 to 3500 Oe; a squareness (residual magnetic flux density Br/saturation magnetic flux density Bm) of usually 0.86 to 0.95, preferably 0.87 to 0.95, a gloss (of the coating film) of usually 202 to 300%, preferably 207 to 300%; a surface roughness Ra (of the coating film) of usually not more than 8.8 nm, preferably 0.5 to 8.3 nm, more preferably 0.5 to 7.8 nm; a Young's modulus (relative value to a commercially available video tape: AV T-120 produced by Victor Company of Japan, Limited) of usually 130 to 160, preferably 132 to 160; and a linear adsorption coefficient (of the coating film) of usually 1.10 to 2.00 μm


−1


, preferably 1.20 to 2.00 μm


−1


. As to the durability, the running durability thereof is usually not less than 26 minutes, preferably not less than 28 minutes. Also, the scratch resistance thereof is usually A or B, preferably A.




The magnetic recording medium according to the present invention shows an anti-corrosion property of not more than 10.0%, preferably not more than 9.5% when expressed by he percentage (%) of change in coercive force thereof, and also shows an anti-corrosion property of not more than 10.0%, preferably not more than 9.5% when expressed by the percentage (%) of change in saturation magnetic flux density thereof.




The important feature of the present invention lies in such a fact that when the acicular hematite particles are acid-dissolving treatment, there can be obtained acicular hematite particles which have such a uniform particle size as being expressed by the geometrical standard deviation of major axis diameter of not more than 1.50 and the geometrical standard deviation of minor axis diameter of preferably not more than 1.35, and are, in particular, excellent in particle size distribution of minor axis diameter thereof.




The reason why the acicular hematite particles according to the present invention can exhibit a uniform particle size, is considered, such that by acid-treating acicular hematite particles in the strongly acidic solution, superfine hematite particles can be removed therefrom, whereby it is possible to obtain acicular goethite particles having a uniform particle size with respect to both major axis diameter and minor axis diameter thereof, because the amount of the superfine hematite particles be reduced.




Further, another important feature of the present invention lies in such a fact that when the acicular goethite particles are heat-treated at a temperature of 100 to 200° C. before subjecting to heat-dehydration treatment, there can be obtained acicular hematite particles which have such a uniform particle size as being expressed by the geometrical standard deviation of major axis diameter of not more than 1.50 and the geometrical standard deviation of minor axis diameter of preferably not more than 1.30, and are, in particular, excellent in particle size distribution of minor axis diameter thereof.




The reason why the acicular hematite particles according to the present invention can exhibit a uniform particle size, is considered, such that by heat-treating acicular goethite particles at a temperature of 100 to 200° C., superfine goethite particles can be absorbed into the acicular goethite particles, whereby it is possible to obtain acicular goethite particles having a uniform particle size with respect to both major axis diameter and minor axis diameter thereof, and further since the amount of the superfine goethite particles be reduced, the sintering between the particles due to the presence of the superfine goethite particles is unlikely to occur upon the subsequent heat-dehydration treatment, whereby it is possible to obtain acicular hematite particles which still maintain the uniform particle size of the acicular goethite particles.




In the magnetic recording medium according to the present invention, when the acicular hematite particles of the present invention are used as non-magnetic particles for non-magnetic undercoat layer, there can be obtained such a magnetic recording medium having a small light transmittance, a more excellent smooth surface and a high strength.




The reason why the magnetic recording medium according to the present invention can exhibit a more excellent smooth surface, is considered by the present inventors, such that by the synergistic effect of such a uniform particle size as being expressed by the geometrical standard deviation of major axis diameter of not more than 1.50 and the geometrical standard deviation of minor axis diameter of not more than 1.35 which results in less amount of coarse or fine particles, and the BET specific surface area of 35.9 to 180 m


2


/g which results in less amount of dehydration pores in the particles or on the surfaces of the particles, the acicular hematite particles according to the present invention can exhibit a more excellent dispersibility in vehicle, so that the obtained non-magnetic undercoat layer can have a more excellent smooth surface.




The another reason why the surface smoothness of the magnetic recording medium is excellent is considered as follows. Since it is possible to sufficiently remove the soluble sodium and the soluble sulfate, which agglomerate acicular hematite particles by firmly crosslinking, the agglomerates are separated into substantially discrete particles by washing the particles with water, so that acicular hematite particles having an excellent dispersion in the vehicle are obtained.




It has been found that the deterioration in magnetic properties of the magnetic acicular metal particles containing iron as a main component and dispersed in the magnetic layer, is considerably influenced by the pH value of non-magnetic particles in the non-magnetic undercoat layer and by the content of soluble sodium salts and soluble sulfates contained in the non-magnetic particles.




That is, as described above, the acicular goethite particles used as a precursor have been produced by various methods. However, in any method, in the case where ferrous sulfate is used as a main raw material for the production of the acicular goethite particles, a large amount of sulfate [SO


4




2−


] is necessarily present in a reacted slurry.




In particular, when the goethite particles are produced in an acid solution, water-soluble sulfates such as Na


2


SO


4


are produced simultaneously, and the reaction mother liquor contains alkali metals such as K


+


, NH


4




+


, Na


+


or the like, so that precipitates containing alkali metals or sulfates tend to be formed. The thus-formed precipitates are represented by the formula of RFe


3


(SO


4


) (OH)


6


, where R is K


+


, NH


4




+


or Na


+


. Such precipitates are composed of insoluble sulfur-containing iron salts and, therefore, cannot be removed merely by an ordinary water-washing method. The insoluble salts are converted into soluble sodium salts or soluble sulfates by the subsequent heat-treatment. However, the soluble sodium salts or the soluble sulfates cause the acicular hematite particles to be cross-linked with each other by the action of a sintering preventive which is added as an essential component for preventing the deformation of the acicular hematite particles and the sintering therebetween in the high-temperature treatment for high densification, and are strongly bonded to the inside or the surface of the acicular hematite particles. Thus, the agglomeration of the acicular hematite particles are further accelerated by the soluble sodium salts or the soluble sulfates. As a result, it becomes extremely difficult to remove especially such soluble sodium salts or soluble sulfates enclosed within the particles or the agglomerated particles, by an ordinary water-washing method.




In the case where the acicular goethite particles are produced in an aqueous alkali solution using ferrous sulfate and sodium hydroxide, a sulfate (Na


2


SO


4


) is simultaneously produced, and NaOH is contained in the reacted slurry. Since Na


2


SO


4


and NaOH both are water-soluble, it is considered that these compounds can be essentially removed by sufficiently washing the acicular goethite particles with water. However, in general, the acicular goethite particles are deteriorated in water-washing efficiency due to a low crystallizability thereof, so that even when the acicular goethite particles are washed with water by an ordinary method, water-soluble components such as soluble sulfates [SO


4




2−


] or soluble sodium salts [Na


+


] still remain in the acicular goethite particles. Further, as described above, these water-soluble components cause the acicular hematite particles to be cross-linked with each other by the action of the sintering preventive, and are strongly bonded to the inside or the surface of the acicular hematite particles, thereby further accelerating the agglomeration of the acicular hematite particles. As a result, it also becomes extremely difficult to remove, especially, such soluble sodium salts or soluble sulfates enclosed within the particles or the agglomerated particles by an ordinary water-washing method.




As described above, it is considered that when the high-density hematite particles containing the soluble sodium salts or the soluble sulfates which are strongly bonded to the inside or the surface of the particles and to the inside of the agglomerated particles through the sintering preventive, are wet-pulverized to deagglomerate coarse particles, then the pH value of the slurry containing the high-density hematite particles is adjusted to not less than 13 and the slurry is heat-treated at not less than 80° C., the aqueous alkali solution can be sufficiently immersed into the high-density hematite particles, so that the bonding force of the sintering preventive strongly bonded to the inside or the surface of the particles and to the inside of the agglomerated particles is gradually weakened, whereby the sintering preventive is released from the inside or the surface of the particles and the inside of the agglomerated particles and simultaneously the water-soluble sodium salts or the water-soluble sulfates tend to be readily removed by washing with water.




In addition, the reason why the deterioration in magnetic properties due to the corrosion of the magnetic acicular metal particles containing iron as a main component and dispersed in the magnetic recording layer, can be suppressed, is considered, such that the amount of water-soluble components such as the soluble sodium salts or the soluble sulfates which accelerate the corrosion of metals contained in the acicular hematite particles for non-magnetic undercoat layer, is reduced and the particles have a pH value as high as not less than 8, so that the corrosion of the acicular hematite particles containing iron as a main component can be prevented from proceeding.




In the magnetic recording medium according to the present invention, when the acicular hematite particles containing aluminum in specific amount within the particle of the present invention are used as non-magnetic particles for non-magnetic undercoat layer, there can be obtained such a magnetic recording medium having a small light transmittance, a more excellent smooth surface, a high strength and a high durability.




The reason why the strength and the durability of the magnetic recording medium is more enhanced is considered that by using the acicular hematite particles containing aluminum uniformly within the particle, the resin adsorptivity of the acicular hematite particles to the binder resin in the vehicles are enhanced due to the use of the above-described particles, as will be shown in later-described examples, the degree of adhesion of the acicular hematite particles in the non-magnetic undercoat layer or the non-magnetic undercoat layer itself to the base film is enhanced; and the increase in adsorptivity of the binder resin for the magnetic particles in the coating composition by using as magnetic particles, the magnetic acicular metal particles containing iron as a main component and further containing aluminum, which results in increase in adhesion between the magnetic particles in the magnetic recording layer and the non-magnetic undercoat layer or between the magnetic recording layer itself and the non-magnetic undercoat layer.




As described in Examples hereinafter, in the case where the acicular hematite particles according to the present invention is used as non-magnetic particles for the non-magnetic undercoat layer, since these particles contain less amount of fine particle components and, therefore, can show an excellent dispersibility in vehicle, there can be obtained such a non-magnetic undercoat layer having an excellent strength and an excellent smooth surface. Further, in the case where a magnetic recording medium is produced by using the non-magnetic undercoat layer, there can be obtained such a magnetic recording medium which can exhibit a low light transmittance, an excellent smooth surface and a high strength, and whose magnetic properties can be prevented from being deteriorated due to the corrosion of the magnetic acicular metal particles containing iron as a main component and dispersed in the magnetic recording layer, since the pH value of the acicular hematite particles used as non-magnetic particles is low and the amount of the soluble sodium salts or the soluble sulfates contained is reduced. Therefore, the acicular hematite particles according to the present invention are suitable as non-magnetic particles for a non-magnetic undercoat layer of a high-density magnetic recording medium.




As described above, the magnetic recording medium according to the present invention can exhibit a low light transmittance, a smooth surface and a high strength, and can be prevented from being deteriorated in magnetic properties due to the corrosion of the magnetic acicular particles containing iron as a main component and dispersed in the magnetic recording layer. Therefore, the magnetic recording medium according to the present invention is suitable as a high-density magnetic recording medium.




Further, in the magnetic recording medium according to the present invention, in the case where specific acicular hematite particles are used as non-magnetic particles for the non-magnetic undercoat layer, there can be obtained such a non-magnetic undercoat layer having a high strength and an excellent smooth surface, because the acicular hematite particles used as non-magnetic particles contain less amount of fine particle components, and have a pH value as high as not less than 8 and an excellent dispersibility in vehicle due to less content of the soluble salts. Consequently, when the magnetic recording medium is produced by using the above-mentioned non-magnetic undercoat layer and using as magnetic particles for the magnetic recording layer, the magnetic acicular metal particles containing iron as a main component and further containing a predetermined amount of Al, there can be obtained such a magnetic recording medium which can exhibit a low light transmittance, an excellent smooth surface, a high strength and an excellent durability, and can be prevented from being deteriorated in magnetic properties due to the corrosion of the magnetic acicular metal particles containing iron as a main component and dispersed in the magnetic recording layer. Therefore, the magnetic recording medium according to the present invention is suitable as a high-density magnetic recording medium.











EXAMPLES




The present invention is described in more detail by Examples and Comparative Examples, but the Examples are only illustrative and, therefore, not intended to limit the scope of the present invention.




Various properties were evaluated by the following methods.




(1) The residue on sieve after the wet-pulverization was obtained by measuring the concentration of the slurry after pulverization by a wet-process in advance, and determining the quantity of the solid content on the sieve remaining after the slurry equivalent to 100 g of the particles content was passed through the sieve of 325 meshes (mesh size: 44 μm).




(2) The average major axis diameter and the average minor axis diameter of the acicular particles are expressed by the average values of 350 particles measured in the photograph obtained by magnifying an electron micrograph (×30000) by 4 times in the vertical and horizontal directions, respectively.




(3) The aspect ratio is the ratio of the average major axis diameter and the average minor axis diameter.




(4) The geometrical standard deviation for particle size distribution of the major axis diameter and minor axis diameter was obtained by the following method.




The major axis diameters and minor axis diameters of the particles were measured from the magnified electron microphotograph in the above-mentioned (2). The actual major axis diameters and minor axis diameters of the particles and the number of particles were obtained from the calculation on the basis of the measured values. On logarithmico-normal probability paper, the major axis diameters or minor axis diameters were plotted at regular intervals on the abscissa-axis and the accumulative number of particles belonging to each interval of the major axis diameters or minor axis diameters was plotted by percentage on the ordinate-axis by a statistical technique. The major axis diameters or minor axis diameters corresponding to the number of particles of 50% and 84.13%, respectively, were read from the graph, and each geometrical standard deviation was measured from the following formulae:




Geometrical standard deviation of the major axis diameter or minor axis diameter={major axis diameter (μm) or




minor axis diameter (μm) corresponding to 84.13% under integration sieve}/{major axis diameter or minor axis diameter (geometrical average diameter) corresponding to 50% under integration sieve}.




The more the geometrical standard deviation nears 1.0, the more excellent the particle size distribution of the major axis diameters and minor axis diameters of the particles.




(5) The specific surface area is expressed by the value measured by a BET method.




(6) The degree of densification of the particles is represented by S


BET


/S


TEM


value as described above.




S


BET


is a specific surface area measured by the above-described BET method.




S


TEM


is a value calculated from the average major axis diameter d cm and the average minor axis diameter w cm measured from the electron microphotograph described in (2) on the assumption that a particle is a rectangular parallellopiped in accordance with the following formula:








S




TEM


(


m




2




/g


)={(4


·d·w+


2


w




2


)/(


d·w




2


·ρ


p


)}×10


−4








wherein ρ


p


is the true specific gravity of the hematite particles, and 5.2 g/cm


3


was used.




(7) The content of each of Al, Si, P, and Nd in and/or on the particle was measured according to JIS K0119 using “fluorescent X-ray spectroscopy device 3063 M” (manufactured by Rigaku Denki Kogyo Co., Ltd.).




(8) The pH value of the particles was measured as follows.




5 g of a sample was weighed and placed in a 300-ml conical flask. 100 ml of boiling pure water was added into the flask and the contents thereof were heated and maintained in a boiling condition for about 5 minutes. Thereafter, the flask was plugged and allowed to stand for cooling up to an ordinary temperature. After boiling pure water was added in such an amount corresponding to the weight loss and the flask was plugged again, the contents of the flask were shaken and mixed for one minute and then allowed to stand for 5 minutes, thereby obtaining a supernatant. The pH value of the thus obtained supernatant was measured according to JIS Z 8802-7, and the pH value of the particles was expressed by the measured value.




(9) The content of soluble sodium salts and the content of soluble sulfates were determined by filtering the supernatant prepared for the above measurement of the pH value of the particles using a filter paper No. 5, and measuring amounts of Na


+


and SO


4




2−


in the filtrate by an inductively coupled plasma atomic emission spectrometry device (manufactured by Seiko Denshi Kogyo Co., Ltd.).




(10) The resin adsorptivity of the particles represents the degree at which a resin is adsorbed to the particles. The closer to 100% the value obtained in the following manner, the firmer the resin adsorptivity to the particles surfaces in the vehicle and the more favorable.




The resin adsorptivity Wa was first obtained. 20 g of particles and 56 g of a mixed solvent (27.0 g of methyl ethyl ketone, 16.2 g of toluene, and 10.8 g of cyclohexanone) with 2 g of a vinyl chloride-vinyl acetate copolymer having a sodium sulfonate group dissolved therein were charged into a 100-ml polyethylene bottle together with 120 g of 3 mmφ steel beads. The particles and the solvent were mixed and dispersed by a paint shaker for 60 minutes.




Thereafter, 50 g of the coating composition was taken out, and charged into a 50-ml settling cylinder. The solid content was separated from the solvent portion by the centrifugalization at a rate of 10000 rpm for 15 minutes. The concentration of the solid resin content contained in the solvent portion was determined by a gravimetric method and the resin content existing in the solid portion was determined by deducting the obtained resin content from the amount of the resin charged as the resin adsorptivity Wa (mg/g) to the particles.




The total quantity of separated solid content was taken into a 100 ml-tall beaker, and 50 g of a mixed solvent (25.0 g of methyl ethyl ketone, 15.0 g of toluene, and 10.0 g of cyclohexanone) was added thereto. The obtained mixture was to ultrasonic dispersion for 15 minutes, and the thus-obtained suspension was charged into a 50-ml settling cylinder. The solid content was separated from the solvent portion by centrifuging them at a rate of 10000 rpm for 15 minutes. The concentration of the solid resin content contained in the solvent portion was measured so as to determine the resin content dissolved from the resin which had been adsorbed to the particle surfaces into the solvent phase.




The process from the step of taking the solid content into the 100 ml-tall beaker to the determination of the resin content dissolved into the solvent phase was repeated twice. The total quantity We (mg/g) of resin content dissolved into the solvent phase in the three cycles was obtained, and the value calculated in accordance with the following formula is expressed as the resin adsorptivity T(%):








T


(%)=[(


Wa−We


)/


Wa]×


100.






(11) The viscosity of the coating composition was obtained by measuring the viscosity of the coating composition at 25° C. at a shear rate D of 1.92 sec


−1


by using “E type viscometer EMD-R” (manufactured by Tokyo Keiki, Co., Ltd.).




(12) The gloss of the surface of the coating film of each of the non-magnetic undercoat layer and the magnetic coating layer was measured at an angle of incidence of 45° by “glossmeter UGV-5D” (manufactured by Suga Shikenki, Co., Ltd.).




(13) The surface roughness Ra is expressed by the average value of the center-line average roughness of the profile curve of the surface of the coating film by using “Surfcom-575A” (manufactured by Tokyo Seimitsu Co., Ltd.).




(14) The strength of the coating film was expressed the Young's modulus obtained by “Autograph” (produced by Shimazu Seisakusho Co., Ltd.). The Young's modulus was expressed by the ratio of the Young's modulus of the coating film to that of a commercially available video tape “AV T-120” (produce by Victor Company of Japan, Limited). The higher the relative value, the more favorable.




(15) The magnetic properties of the magnetic particles and magnetic recording medium were measured under an external magnetic field of 10 kOe by “Vibration Sample Magnetometer VSM-3S-15 (manufactured by Toei Kogyo, Co., Ltd.)”.




(16) The change with the passage of time in magnetic properties of the magnetic recording medium due to the corrosion of the magnetic acicular metal particles containing iron as a main component, which are dispersed in the magnetic coating film, was determined as follows.




The magnetic recording medium was allowed to stand at a temperature of 60° C. and a relative humidity of 90% for 14 days. The coercive force values and the saturation magnetization values of the magnetic recording medium before and after the keeping test were measured, and the difference between the measured values before and after the keeping test was divided by the value before the keeping test, thereby obtaining an amount of change in each magnetic property which was expressed by a percentage.




(17) The light transmittance is expressed by the linear adsorption coefficient calculated by substituting the light transmittance measured by using “UV-Vis Recording Spectrophotometer UV-2100” (manufactured by Shimazu Seisakusho, Ltd.) for the following formula. The larger the value, the more difficult it is for the magnetic recording medium to transmit light:




Linear adsorption coefficient (μm





)={1n (1/t)}/FT wherein t represents a light transmittance (−) at λ=900 nm, and FT represents thickness (μm) of the coating film used for the measurement.




(18) The durability of the magnetic medium was evaluated by the following running durability and the scratch resistance.




The running durability was evaluated by the actual operating time under the conditions that the load was 200 gw and the relative speed of the head and the tape was 16 m/s by using “Media Durability Tester MDT-3000” (manufactured by Steinberg Associates). The longer the actual operating time, the higher the running durability.




The scratch resistance was evaluated by observing through the microscope the surface of the magnetic tape after running and visually judging the degree of scratching. Evaluation was divided into the following four ranks.




A: No scratch




B: A few scratches




C: Many scratches




D: Great many scratches




(19) The thickness of each of the base film, the non-magnetic undercoat layer and the magnetic coating film constituting the magnetic recording medium was measured in the following manner by using “Digital Electronic Micrometer R351C” (manufactured by Anritsu Corp.)




The thickness (A) of a base film was first measured. Similarly, the thickness (B) (B=the sum of the thicknesses of the base film and the non-magnetic undercoat layer) of a non-magnetic substrate obtained by forming a non-magnetic undercoat layer on the base film was measured. Furthermore, the thickness (C) (C=the sum of the thicknesses of the base film, the non-magnetic undercoat layer and the magnetic recording layer) of a magnetic recording medium obtained by forming a magnetic recording layer on the non-magnetic substrata was measured. The thickness of the non-magnetic undercoat layer is expressed by (B)−(A), and the thickness of the magnetic recording layer is expressed by (C)−(B).




Example 1




<Production of spindle-shaped hematite Particles>




1200 g of spindle-shaped goethite particles obtained by the above production method (B) of goethite particles using a ferrous sulfate aqueous solution and a sodium carbonate aqueous solution (average major axis diameter: 0.171 μm, average minor axis diameter: 0.0213 μm, aspect ratio: 8.0:1, geometrical standard deviation of major axis diameter: 1.34, geometrical standard deviation of minor axis diameter: 1.39, BET specific surface area: 151.6 m


2


/g, content of soluble sodium salts: 701 ppm (calculated as Na), content of soluble sulfate: 422 ppm (calculated as SO


4


), pH value: 6.7) were suspended in water so as to obtain a slurry, and the concentration of the solid content was adjusted to 8 g/liter. 150 liter of the slurry was heated to 60° C. and the pH value of the slurry was adjusted to 10.0 by adding a 0.1-N aqueous NaOH solution.




To the alkali slurry was gradually added 36 g of #3 water glass as a sintering preventive, and after the end of addition, the resultant mixture was aged for 60 minutes. The pH value of the slurry was then adjusted to 6.0 by adding a 0.1-N acetic acid solution. Thereafter, the particles were filtered out, washed with water, dried and pulverized by an ordinary method, thereby producing spindle-shaped goethite particles coated with an oxide of silicon. The silicon content was 0.78% by weight (calculated as SiO


2


).




1000 g of the spindle-shaped goethite particles obtained were charged into a stainless steel rotary furnace, and heat-dehydrated in the air at 350° C. for 40 minutes while rotating the furnace, to obtain low-density spindle-shaped hematite particles. The thus obtained low-density spindle-shaped hematite particles had an average major axis diameter of 0.145 μm, an average minor axis diameter of 0.0193 μm, an aspect ratio of 7.5:1, a geometrical standard deviation of major axis diameter of 1.34, a geometrical standard deviation of minor axis diameter of 1.39, a BET specific surface area of 176.5 m


2


/g and a S


BET


/S


TEM


value of 4.15. The content of soluble sodium salt of the low-density spindle-shaped hematite particles was 1717 ppm (calculated as Na) and the content of soluble sulfate was 1011 ppm (calculated as SO


4


). The pH value of the low-density spindle-shaped hematite particles was 6.3.




850 g of the low-density spindle-shaped hematite particles were then charged into a ceramic rotary furnace, and heat-treated in the air at 610° C. for 30 minutes while rotating the furnace so as to fill in dehydration pores. The resultant high-density spindle-shaped hematite particles had an average major axis diameter of 0.137 μm, an average minor axis diameter of 0.0190 μm, an aspect ratio of 7.2:1, a geometrical standard deviation of major axis diameter of 1.35, a geometrical standard deviation of minor axis diameter of 1.40, a BET specific surface area (S


BET


) of 55.3 m


2


/g and a S


BET


/S


TEM


value of 1.28. The silicon content was 0.85% by weight (calculated as SiO


2


). The content of soluble sodium salt of the high-density spindle-shaped hematite particles was 2626 ppm (calculated as Na) and the content of soluble sulfate was 3104 ppm (calculated as SO


4


). The pH value of the high-density spindle-shaped hematite particles was 5.3.




After 800 g of the high-density spindle-shaped hematite particles obtained were roughly pulverized by a Nara mill in advance, the obtained high-density spindle-shaped hematite particles were charged into 4.7 liter of pure water and deagglomerated by a homomixer (manufactured by Tokushu-kika Kogyo, CO., Ltd.) for 60 minutes.




The slurry of the high-density spindle-shaped hematite particles obtained was then dispersed for 3 hours at an axial rotation frequency of 2000 rpm while being circulated by a horizontal SGM (Dispermat SL, manufactured by S. C. Adichem, CO., Ltd.). The high-density spindle-shaped hematite particles in the slurry remaining on a sieve of 325 meshes (mesh size: 44 μm) was 0% by weight.




<Dissolving treatment with acid>




The slurry of the high-density spindle-shaped hematite particles obtained was mixed with water, thereby adjusting the concentration of the slurry to 100 g/liter. A 70% aqueous sulfuric acid solution was added to 7 liter of the slurry under stirring so as to adjust the sulfuric acid concentration to 1.3 N and the pH value to 0.65. The slurry was then heated to 80° C. under stirring, and was held for 5 hours at 80° C., thereby dissolving 29.7% by weight of the spindle-shaped hematite particles based on the total weight of the spindle-shaped hematite in the slurry.




The slurry was filtered to separate a filtrate (aqueous acid solution of iron sulfate) therefrom. The slurry from which the filtrate had been separated, was then washed with water by a decantation method and the pH value of the slurry was adjusted to 5.0. When the concentration of the slurry at this point was checked so as to ensure the accuracy, it was 68 g/liter.




2 liter of the obtained slurry was filtered through a Buchner filter, and pure water was passed until the electric conductivity of the filtrate became not more than 30 μs. The high-density spindle-shaped hematite particles were then dried by an ordinary method and pulverized so as to obtain the high-density spindle-shaped hematite particles. The high-density spindle-shaped hematite particles obtained had an average major axis diameter of 0.131 μm, an average minor axis diameter of 0.0181 μm, an aspect ratio of 7.2:1, a geometric standard deviation of major axis diameter of 1.35, a geometric standard deviation of major axis diameter of 1.33, a BET specific surface area (S


BET


) of 58.1 m


2


/g and a S


BET


/S


TEM


value of 1.28. The content of soluble sodium salt of the high-density spindle-shaped hematite particles was 138 ppm (calculated as Na) and the content of soluble sulfate was 436 ppm (calculated as SO


4


). The pH value of the high-density spindle-shaped hematite particles was 4.8.




S<Treatment of spindle-shaped hematite particles in an aqueous alkali solution>




The concentration of the high-density spindle-shaped hematite particles in the slurry was adjusted to 50 g/liter, and 5 liter of the slurry was adjusted to pH value 13.6 by adding 6N-aqueous NaOH solution. The resulting slurry was then heated to 95° C. under stirring, and was held for 3 hours at 95° C.




The resultant slurry was then washed with water by a decantation method and the pH value of the slurry was adjusted to 10.5. The concentration of the slurry at this point was 98 g/liter.




The high-density spindle-shaped hematite particles were filtered out from 1 liter of the obtained slurry through a Buchner filter, and the purified water was passed into the filtrate until the electric conductivity of the filtrate became not more than 30 μs. The high-density spindle-shaped hematite particles were then dried by an ordinary method and pulverized to obtain the target high-density spindle-shaped hematite particles. The high-density spindle-shaped hematite particles obtained had an average major axial diameter of not more than 0.131 μm, a minor axial diameter of 0.0181 μm, and a specific ratio of 7.2:1. The geometric standard deviation of major axial diameter was 1.35, the geometric standard deviation of minor axial diameter was 1.33, the BET specific surface (S


BET


) was 57.8 m


2


/g, the S


BET


/S


TEM


value was 1.27. The content of soluble sodium salt of the high-density spindle-shaped hematite particles was 99 ppm (calculated as Na) and the content of soluble sulfate was 21 ppm (calculated as SO


4


). The pH value of the high-density spindle-shaped hematite particles was 9.3.




Example 2




<Production of non-magnetic substrate: Formation of non-magnetic undercoat layer on base film>




12 g of the high-density spindle-shaped hematite particles obtained in Example 1 were mixed with a binder resin solution (30% by weight of vinyl chloride-vinyl acetate copolymer resin having a sodium sulfonate group and 70% by weight of cyclohexanone) and cyclohexanone, and each of the obtained mixtures (solid content: 72% by weight) was kneaded by a plast-mill for 30 minutes.




Each of the thus-obtained kneaded material was charged into a 140 ml-glass bottle together with 95 g of 1.5 mm glass beads, a binder resin solution (30% by weight of polyurethane resin having a sodium sulfonate group and 70% by weight of a solvent (methyl ethyl ketone : toluene=1:1)), cyclohexanone, methyl ethyl ketone and toluene, and the obtained mixture was mixed and dispersed by a paint shaker for 6 hours to obtain a non-magnetic coating composition. The viscosity of the obtained coating film composition was 367 cP.




The thus-obtained non-magnetic coating composition containing the high-density spindle-shaped hematite particles was as follows:






















High-density spindle-shaped




100




parts by weight







hematite particles







Vinyl chloride-vinyl acetate




10




parts by weight







copolymer resin having a sodium







sulfonate group







Polyurethane resin having a




10




parts by weight







sodium sulfonate group







Cyclohexanone




44.6




parts by weight







Methylethyl ketone




111.4




parts by weight







Toluene




66.9




parts by weight















The non-magnetic coating composition obtained was applied to a polyethylene terephthalate film of 12 μm thick to a thickness of 55 μm by an applicator, and the coating film was then dried, thereby forming a non-magnetic undercoat layer. The thickness of the non-magnetic undercoat layer was 3.5 μm.




The non-magnetic undercoat layer produced from the high-density spindle-shaped hematite particles as the non-magnetic particles had a gloss of 204%, and a surface roughness Ra of 6.6 nm. The Young's modulus (relative value) thereof was 124.




Example 3




<Production of magnetic recording medium: Formation of magnetic recording layer>




12 g of magnetic acicular metal particles containing iron as a main component (average major axis diameter: 0.120 μm, average minor axis diameter: 0.0154 μm, a geometrical standard deviation of major axis diameter of 1.37, aspect ratio: 7.8:1, coercive force value: 1896 Oe, saturation magnetization value: 133.8 emu/g, pH value: 9.7), 1.2 g of a polishing agent (AKP-30: trade name, produced by Sumitomo Chemical Co., Ltd.), 0.12 g of carbon black (#3250B, trade name, produced by Mitsubishi Chemical Corp.), a binder resin solution (30% by weight of vinyl chloride-vinyl acetate copolymer resin having a sodium sulfonate group and 70% by weight of cyclohexanone) and cyclohexanone were mixed to obtain a mixture (solid content: 78% by weight). The mixture was further kneaded by a plast-mill for 30 minutes to obtain a kneaded material.




The thus-obtained kneaded material was charged into a 140 ml-glass bottle together with 95 g of 1.5 mm glass beads, a binder resin solution (30% by weight of polyurethane resin having a sodium sulfonate group and 70% by weight of a solvent (methyl ethyl ketone : toluene=1:1)), cyclohexanone, methyl ethyl ketone and toluene, and the mixture was mixed and dispersed by a paint shaker for 6 hours. Then, the lubricant and hardening agent were added to the mixture, and the resultant mixture was mixed and dispersed by a paint shaker for 15 minutes.




The thus-obtained magnetic coating composition was as follows:






















Magnetic acicular metal




100




parts by weight







particles containing iron as a







main component







Vinyl chloride-vinyl acetate




10




parts by weight







copolymer resin having a sodium







sulfonate group







Polyurethane resin having a




10




parts by weight







sodium sulfonate group







Polishing agent (AKP-30)




10




parts by weight







Carbon black (#3250B)




3.0




parts by weight







Lubricant (myristic acid:butyl




3.0




parts by weight







stearate = 1:2)







Hardening agent (polyisocyanate)




5.0




parts by weight







Cyclohexanone




65.8




parts by weight







Methyl ethyl ketone




164.5




parts by weight







Toluene




98.7




parts by weight















The magnetic coating composition obtained was applied to the non-magnetic undercoat layer to a thickness of 15 μm by an applicator, and the magnetic recording medium obtained was oriented and dried in a magnetic field, and then calendered. The magnetic recording medium was then subjected to a curing reaction at 60° C. for 24 hours, and thereafter slit into a width of 0.5 inch, thereby obtaining a magnetic tape. The thickness of the respective magnetic recording layer was 1.1




The coercive force Hc of the magnetic tape produced by forming a magnetic recording layer on the non-magnetic undercoat layer was 1986 Oe, the squareness (Br/Bm) thereof was 0.87, the gloss thereof was 220%, the surface roughness Ra thereof was 6.2 nm, the Young's modulus (relative value) thereof was 128, the linear absorption coefficient thereof was 1.24 μm


−1


.




The percentages of change in coercive force and saturation magnetization which represent an anti-corrosion is property of the magnetic tape, were 4.3% and 4.6%, respectively.




Example 4




<Production of magnetic recording medium: Formation of magnetic recording layer>




The same procedure as defined in Example 3 was conducted except that the magnetic particles were changed to magnetic acicular metal particles (average major axis diameter: 0.115 μm, average minor axis diameter: 0.0145 μm, a geometric standard deviation of major axis diameter of 1.36, aspect ratio: 7.9:1, coercive force: 1909 Oe, saturation magnetization: 133.8 emu/g, aluminum content of 2.85% by weight, calculated as Al, (1.26% by weight, calculated as Al, of aluminum in the central portion, 0.84% by weight, calculated as Al, of aluminum in the surface layer portion, and 0.75% by weight, calculated as Al, of aluminum on the surface coating), Nd content of 0.12% by weight, resin adsorptivity: 81.6%), thereby producing a magnetic tape.




The thickness of the magnetic coating film was 1.0 μm.




The thus obtained magnetic tape had a coercive force Hc of 1980 Oe, a squareness (Br/Bm) of 0.88, a gloss of 223%, a surface roughness Ra of 6.4 nm, a Young's modulus (relative value) of coating film of 128, a linear absorption coefficient of 1.24 μm


−1


, a running durability of 28.9 minutes and a scratch resistance of A.




The percentages of change in coercive force and saturation magnetization which represent an anti-corrosion property of the magnetic tape, were 4.6% and 2.7%, respectively.




Example 5




<Production of single-shaped hematite particles>




1200 g of spindle-shaped goethite particles obtained by the above production method (B) of goethite particles using a ferrous sulfate aqueous solution, a sodium carbonate aqueous solution and aluminum sulfate aqueous solution, and containing aluminum in an amount of 1.12% by weight (calculated as Al) based on the total weight of the particles, uniformly within the particles (average major axis diameter: 0.167 μm, average minor axis diameter: 0.0196 μm, aspect ratio: 8.5:1, geometrical standard deviation of major axis diameter: 1.32, geometrical standard deviation of minor axis diameter: 1.40, BET specific surface area: 165.3 m


2


/g, content of soluble sodium salts: 1821 ppm (calculated as Na), content of soluble sulfate: 2162 ppm (calculated as SO


4


), pH value: 6.8) were suspended in water so as to obtain a slurry, and the concentration of the solid content was adjusted to 8 g/liter. 150 liter of the slurry was heated to 60° C. and the pH value of the slurry was adjusted to 10.0 by adding a 0.1-N aqueous NaOH solution.




To the alkali slurry was gradually added 24 g of #3 water glass as a sintering preventive, and after the end of addition, the resultant mixture was aged for 60 minutes. The pH value of the slurry was then adjusted to 6.0 by adding a 0.1-N acetic acid solution. Thereafter, the particles were filtered out, washed with water, dried and pulverized by an ordinary method, thereby producing spindle-shaped goethite particles which substantially uniformly contain aluminum within the particle, coated with an oxide of silicon. The silicon content was 0.52% by weight (calculated as SiO


2


) based on the total weight of the particles.




1000 g of the spindle-shaped goethite particles which substantially uniformly contain aluminum within the particle, obtained were charged into a stainless steel rotary furnace, and heat-dehydrated in the air at 350° C. for 40 minutes while rotating the furnace, to obtain low-density spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle. The thus obtained low-density spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle, had an average major axial diameter of 0.143 μm, an average minor axial diameter of 0.0191 μm, a geometric standard deviation of major axis diameter of 1.32, a geometric standard deviation of minor axis diameter of 1.40, an aspect ratio of 7.5:1, a BET specific surface area (S


BET


) of 188.9 m


2


/g and a S


BET


/S


TEM


value of 4.40. The low-density spindle-shaped hematite particles contained soluble sodium salts of 1682 ppm (calculated as Na) and soluble sulfates of 976 ppm (calculated as SO


4


). The aluminum content was 1.23% by weight (calculated as Al), the pH value of the low-density spindle-shaped hematite particles was 6.1. The SiO


2


content thereof was 0.57% by weight (calculated as SiO


2


) based on the total weight of the particles.




850 g of the low-density spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle, were then charged into a ceramic rotary furnace, and heat-treated in the air at 650° C. for 30 minutes while rotating the furnace so as to fill in dehydration pores. The resultant high-density spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle, had an average major axial diameter of 0.141 μm, an average minor axial diameter of 0.0192 μm, a geometric standard deviation of major axis diameter of 1.33, a geometric standard deviation of minor axis diameter of 1.41, an aspect ratio of 7.3:1, a BET specific surface area (S


BET


) of 56.1 m


2


/g and a S


BET


/S


TEM


value of 1.31. The silicon content was 0.57% by weight (calculated as SiO


2


) and the aluminum content was 1.23% by weight (calculated as Al). The content of soluble sodium salt of the high-density spindle-shaped hematite particles was 2538 ppm (calculated as Na) and the content of soluble sulfate was 2859 ppm (calculated as SO


4


). The pH thereof was 5.6.




After 800 g of the high-density spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle, obtained were roughly pulverized by a Nara mill in advance, the obtained high-density spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle, were charged into 4.7 liter of pure water and deagglomerated by a homomixer (manufactured by Tokushu-kika Kogyo, CO., Ltd.) for 60 minutes.




The slurry of the high-density spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle, obtained was then dispersed for 3 hours at an axial rotation frequency of 2000 rpm while being circulated by a horizontal SGM (Dispermat SL, manufactured by S. C. Adichem, CO., Ltd.). The high-density spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle, in the slurry remaining on a sieve of 325 meshes (mesh size: 44 μm) was 0% by weight.




<Dissolving treatment with acid>




The slurry of the high-density spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle, obtained was mixed with water, thereby adjusting the concentration of the slurry to 100 g/liter. A 70% aqueous sulfuric acid solution was added to 7 liter of the slurry under stirring so as to adjust the sulfuric acid concentration to 1.3N and the pH value to 0.58. The slurry was then heated to 80° C. under stirring, and was held for 5 hours at 80° C., thereby dissolving 29.5% by weight of the high density spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle, based on the total weight of the high-density spindle-shaped hematite particles in the slurry.




The slurry was filtered to separate a filtrate (aqueous acid solution of iron sulfate) therefrom. The slurry from which the filtrate had been separated, was then washed with water by a decantation method and the pH value of the slurry was adjusted to 5.0. When the concentration of the slurry at this point was checked so as to ensure the accuracy, it was 68 g/liter.




A part of the water-washed slurry obtained was separated and filtered through a Buchner filter, and pure water was passed until the electric conductivity of the filtrate became not more than 30 μs. The resultant particles were then dried by an ordinary method and pulverized so as to obtain the high-density spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle. The high-density spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle, obtained had an average major axis diameter of 0.133 μm, an average minor axis diameter of 0.0182 μm, an aspect ratio of 7.3:1, a geometric standard deviation of major axis diameter of 1.34, a geometric standard deviation of minor axis diameter of 1.33, a BET specific surface area (S


BET


) of 60.3 m


2


/g, a S


BET


/S


TEM


value of 1.34, an aluminum content of 1.23% by weight (calculated as Al). The content of soluble sodium salt of the high-density spindle-shaped hematite particles was 131 ppm (calculated as Na) and the content of soluble sulfate was 424 ppm (calculated as SO


4


). The pH value of the high-density spindle-shaped hematite particles was 4.9.




<Treatment of high-density spindle-shaped hematite particles in an aqueous alkali solution>




The concentration of the high-density spindle-shaped hematite particles in the slurry was adjusted to 50 g/liter, and 5 liter of the slurry was adjusted to pH value 13.6 by adding a 6N-aqueous NaOH solution. The resulting slurry was then heated to 95° C. under stirring, and was held for 3 hours at 95° C.




The resultant slurry was then washed with water by a decantation method and the pH value of the slurry was adjusted to 10.5. The concentration of the slurry at this point was 98 g/liter.




The particles were filtered out from the obtained slurry of 1 liter through a Buchner filter, and the purified water was passed into the filtrate until the electric conductivity of the filtrate became not more than 30 μs. The particles were then dried by an ordinary method and pulverized to obtain the target high-density spindle-shaped hematite particles. The high-density spindle-shaped hematite particles obtained had an average major axial diameter of not more than 0.133 μm, a minor axial diameter of 0.0182 μm, and a specific ratio of 7.3:1. The geometric standard deviation of major axial diameter was 1.33, the geometric standard deviation of minor axial diameter was 1.34, the BET specific surface (S


BET


) was 60.1 m


2


/g, the S


BET


/S


TEM


value was 1.33. The aluminum content was 1.23% by weight (calculated as Al). The content of soluble sodium salt of the high-density spindle-shaped hematite particles was 97 ppm (calculated as Na) and the content of soluble sulfate was 20 ppm (calculated as SO


4


). The pH value of the high-density spindle-shaped hematite particles was 9.4, and the resin adsorptivity thereof was 72.5%.




Example 6




<Production of non-magnetic substrate: Formation of non-magnetic undercoat layer on base film>




The same procedure as defined in Example 2 was conducted except that the spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle, obtained in Example 5 were used instead of the spindle-shaped hematite particles, thereby obtaining a non-magnetic undercoat layer.




The thickness of the non-magnetic undercoat layer was 3.5 μm.




The thus obtained non-magnetic undercoat layer had a gloss of 212%, a surface roughness Ra of 6.1 nm, and a Young's modulus (relative value) of coating film of 127.




Example 7




<Production of magnetic recording medium: Formation of magnetic recording layer>




The same procedure as defined in Example 3 was conducted except that magnetic acicular metal particles containing iron as a main component and further containing aluminum in amounts of 1.24% by weight (calculated as Al) at a central portion of particle; 0.83% by weight (calculated as Al) at a surface portion thereof; and 0.94% by weight (calculated as Al) in a coating layer formed on the surface of particle (average major axis diameter: 0.112 μm, average minor axis diameter: 0.0147 μm, geometrical standard deviation of major axis diameter: 1.36, aspect ratio: 7.6:1, coercive force: 1908 Oe, saturation magnetization: 136.3 emu/g, resin adsorptivity: 82.0%) were used, thereby obtaining a magnetic coating composition.




The thus obtained magnetic coating composition was applied onto the non-magnetic undercoat layer obtained in Example 6 in the same manner as in Example 3, thereby forming a magnetic recording layer and producing a magnetic tape.




The thickness of the magnetic coating film was 1.1 μm.




The thus obtained magnetic tape had a coercive force Hc of 1983 Oe, a squareness (Br/Bm) of 0.87, a gloss of 234%, a surface roughness Ra of 6.1 nm, a Young's modulus (relative value) of coating film of 131, a linear absorption coefficient of 1.24 μm


−1


, a running durability of 29.2 minutes, and a scratch resistance of A.




Changes in the coercive force and the saturation magnetic flux density Bit with passage time were 4.5% and 2.6%, respectively.




Example 8




<Production of spindle-shaped hematite particles>




1200 g of spindle-shaped goethite particles obtained by the above production method (B) of goethite particles using a ferrous sulfate aqueous solution and a sodium carbonate aqueous solution (average major axis diameter: 0.0812 μm, geometrical standard deviation of major axis diameter: 1.53, average minor axis diameter: 0.0110 μm, geometrical standard deviation of minor axis diameter: 1.37, aspect ratio: 7.4:1, BET specific surface area: 168.9 m


2


/g, soluble sodium salt content: 1212 ppm (calculated as Na), soluble sulfate content: 1816 ppm (calculated as SO


4


), pH value: 6.8) were suspended in water so as to obtain a slurry, and the concentration of the solid content was adjusted to 8 g/liter. 150 liter of the slurry was heated to 60° C. and the pH value of the slurry was adjusted to 10.0 by adding a 0.1-N aqueous NaOH solution.




To the alkali slurry was gradually added 36.0 g of #3 water glass as a sintering preventive, and after the end of addition, the resultant mixture was aged for 60 minutes. The pH value of the slurry was then adjusted to 6.0 by adding a 0.1-N acetic acid solution. Thereafter, the particles were filtered out, washed with water, dried and pulverized by an ordinary method, thereby producing spindle-shaped goethite particles coated with an oxide of silicon. The silicon content was 0.78% by weight (calculated as SiO


2


).




The spindle-shaped goethite particles obtained were charged into a heat-treatment metal furnace, and heat-treated therein at 150° C. for 30 minutes, thereby absorbing superfine goethite particles present within the spindle-shaped goethite particles, into the spindle-shaped goethite particles.




The thus obtained spindle-shaped goethite particles were charged again into the heat treatment metal furnace, and heat-dehydrated therein at 320° C. for 30 minutes, thereby obtaining low-density spindle-shaped hematite particles. The thus obtained low-density spindle-shaped hematite particles had an average major axis diameter of 0.0736 μm, a geometrical standard deviation of major axis diameter of 1.38, an average minor axis diameter of 0.0118 μm, a geometrical standard deviation of minor axis diameter of 1.16, an aspect ratio of 6.1:1, a BET specific surface area of 190.3 m


2


/g, a S


BET


/S


TEM


value of 2.70. The silicon content was 0.78% by weight (calculated as SiO


2


). The content of soluble sodium salt of the low-density spindle-shaped hematite particles was 1826 ppm (calculated as Na) and the content of soluble sulfate was 2512 ppm (calculated as SO


4


). The pH value of the low-density spindle-shaped hematite particles was 6.1.




850 g of the low-density spindle-shaped hematite particles were then charged into a ceramic rotary furnace, and heat-treated in the air at 650° C. for 30 minutes while rotating the furnace so as to fill in dehydration pores. The resultant high-density spindle-shaped hematite particles had an average major axis diameter of 0.0727 μm, a geometrical standard deviation of major axis diameter of 1.38, an average minor axis diameter of 0.0120 μm, a geometrical standard deviation of minor axis diameter of 1.17, an aspect ratio of 6.1:1, a BET specific surface area (S


BET


) of 86.8 m


2


/g, a S


BET


/S


TEM


value of 1.25. The silicon content was 0.87% by weight (calculated as SiO


2


). The content of soluble sodium salt of the high-density spindle-shaped hematite particles was 2121 ppm (calculated as Na) and the content of soluble sulfate was 2832 ppm (calculated as SO


4


). The pH value of the high-density spindle-shaped hematite particles was 5.8.




<Treatment of high-density spindle-shaped hematite particles in an aqueous alkali solution>




The concentration of the high-density spindle-shaped hematite particles in the slurry was adjusted to 50 g/liter, and 5 liter of the slurry was adjusted to pH value 13.4 by adding a 6N-aqueous NaOH solution. The resulting slurry was then heated to 95° C. under stirring, and was held for 3 hours at 95° C.




The resultant slurry was then washed with water by a decantation method and the pH value of the slurry was adjusted to 10.5. The concentration of the slurry at this point was 98 g/liter.




The particles were filtered out through a Buchner filter, and the purified water was passed into the filtrate until the electric conductivity of the filtrate became not more than 30 μs. The particles were then dried by an ordinary method and pulverized to obtain the target high-density spindle-shaped hematite particles. The high-density spindle-shaped hematite particles obtained had an average major axial diameter of 0.0726 μm, a minor axial diameter of 0.0120 μm, and a specific ratio of 6.1. The geometric standard deviation of major axial diameter was 1.38, the geometric standard deviation of minor axial diameter was 1.17, the BET specific surface (S


BET


) was 86.2 m


2


/g, the S


BET


/S


TEM


value was 1.24. The content of soluble sodium salt of the high-density spindle-shaped hematite particles was 86 ppm (calculated as Na) and the content of soluble sulfate was 32 ppm (calculated as SO


4


). The pH value of the high-density spindle-shaped hematite particles was 9.0, and the resin adsorptivity thereof was 75.1%.




Example 9




<Production of non-magnetic substrate: Formation of nonmagnetic undercoat layer on base film>




The same procedure as defined in Example 2 was conducted except that the high-density spindle-shaped hematite particles obtained in Example 8 were used instead of the spindle-shaped hematite particles, thereby obtaining a non-magnetic undercoat layer. The thickness of the non-magnetic undercoat layer was 3.4 μm.




The thus obtained non-magnetic undercoat layer had a gloss of 208%, a surface roughness Ra of 6.4 nm, and a Young's modulus (relative value) of coating film of 134.




Example 10




<Production of magnetic recording medium: Formation of magnetic recording layer>




The same procedure as defined in Example 3 was conducted except that the magnetic particles were changed to magnetic acicular metal particles containing iron as a main component (average major axis diameter: 0.103 μm, average minor axis diameter: 0.0152 μm, a geometric standard deviation of major axis diameter of 1.38, aspect ratio: 6.8:1, coercive force: 1910 Oe, saturation magnetization: 136 emu/g), and that the non-magnetic undercoat layer obtained in Example 9 was used, thereby producing a magnetic tape.




The thickness of the magnetic coating film was 1.0 μm.




The thus obtained magnetic tape had a coercive force Hc of 1991 Oe, a squareness (Br/Bm) of 0.88, a gloss of 235%, a surface roughness Ra of 5.8 nm, a Young's modulus (relative value) of coating film of 137, a linear absorption coefficient of 1.26 μm


−1


, a running durability of 298 minutes and a scratch resistance of A.




Changes in the coercive force and the saturation magnetic flux density Bm with passage time were 4.6% and 3.8%, respectively.




Example 11




<Production of magnetic recording medium: Formation of magnetic recording layer>




The same procedure as defined in Example 3 was conducted except that the magnetic particles were changed to magnetic acicular metal particles (average major axis diameter: 0.115 μm, average minor axis diameter: 0.0145 μm, a geometric standard deviation of major axis diameter of 1.36, aspect ratio: 7.9:1, coercive force: 1909 Oe, saturation magnetization: 133.8 emu/g,,aluminum content of 2.85% by weight, calculated as Al, (1.26% by weight, calculated as Al, of aluminum in the central portion, 0.84% by weight, calculated as Al, of aluminum in the surface layer portion, and 0.75% by weight, calculated as Al, of aluminum on the surface coating), Nd content of 0.12% by weight, resin adsorptivity: 81.6%), and that the non-magnetic undercoat layer obtained in Example 9 was used, thereby producing a magnetic tape.




The thickness of the magnetic coating film was 1.0 μm.




The thus obtained magnetic tape had a coercive force Hc of 1985 Oe, a squareness (Br/Bm) of 0.89, a gloss of 238%, a surface roughness Ra of 5.6 nm, a Young's modulus (relative value) of coating film of 138, a linear absorption coefficient of 1.27 μm


−1


, a running durability of not less than 30 minutes and a scratch resistance of A.




Changes in the coercive force and the saturation magnetic flux density Bm with passage time were 2.8% and 2.6%, respectively.




Example 12




<Production of spindle-shaped hematite Particles>




1200 g of spindle-shaped goethite particles obtained by the above production method (B) of goethite particles using a ferrous sulfate aqueous solution, a sodium carbonate aqueous solution and aluminum sulfate aqueous solution (average major axis diameter: 0.0846 μm, geometrical standard deviation of major axis diameter: 1.49, average minor axis diameter: 0.0115 μm, geometrical standard deviation of minor axis diameter: 1.38, aspect ratio: 7.4:1, BET specific surface area: 161.6 m


2


/g, aluminum content: 2.12% by weight (calculated as Al), soluble sodium salt content: 1168 ppm (calculated as Na), soluble sulfate content: 1721 ppm (calculated as SO


4


), pH value: 6.0) were suspended in water so as to obtain a slurry, and the concentration of the solid content was adjusted to 8 g/liter. 150 liter of the slurry was heated to 60° C. and the pH value of the slurry was adjusted to 10.0 by adding a 0.1-N aqueous NaOH solution.




To the alkali slurry was gradually added 42.0 g of #3 water glass as a sintering preventive, and after the end of addition, the resultant mixture was aged for 60 minutes. The pH value of the slurry was then adjusted to 6.0 by adding a 0.1-N acetic acid solution. Thereafter, the particles were filtered out, washed with water, dried and pulverized by an ordinary method, thereby producing spindle-shaped goethite particles which substantially uniformly contain aluminum within the particle, coated with an oxide of silicon. The silicon content was 0.90% by weight (calculated as SiO


2


).




The spindle-shaped goethite particles which substantially uniformly contain aluminum within the particle, obtained were charged into a heat treatment metal furnace, and heat-treated therein at 140° C. for 30 minutes, thereby absorbing superfine goethite particles present within the spindle-shaped goethite particles, into the spindle-shaped goethite particles.




The thus obtained spindle-shaped goethite particles which substantially uniformly contain aluminum within the particle, were charged again into the heat treatment metal furnace, and heat-dehydrated therein at 340° C. for 30 minutes, thereby obtaining low-density spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle. The thus obtained low-density spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle, had an average major axis diameter of 0.0793 μm, a geometrical standard deviation of major axis diameter of 1.37, an average minor axis diameter of 0.0119 μm, a geometrical standard deviation of minor axis diameter of 1.23, an aspect ratio of 6.7:1, a BET specific surface area (S


BET


) of 181.0 m


2


/g, a S


BET


/S


TEM


value of 2.60. The silicon content was 0.99% by weight (calculated as SiO


2


) and the aluminum content was 2.35% by weight (calculated as Al). The content of soluble sodium salt of the low-density spindle-shaped hematite particles was 1465 ppm (calculated as Na) and the content of soluble sulfate was 1965 ppm (calculated as SO


4


). The pH value of the low-density spindle-shaped hematite particles was 5.9.




850 g of the low-density spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle, were then charged into a ceramic rotary furnace, and heat-treated in the air at 650° C. for 30 minutes while rotating the furnace so as to fill in dehydration pores. The resultant high-density spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle, had an average major axis diameter of 0.0753 μm, a geometrical standard deviation of major axis diameter of 1.37, an average minor axis diameter of 0.0122 μm, a geometrical standard deviation of minor axis diameter of 1.24, an aspect ratio of 6.2:1, a BET specific surface area (S


BET


) of 83.8 m


2


/g, a S


BET


/S


TEM


value of 1.23. The silicon content was 1.00% by weight (calculated as SiO


2


) and the aluminum content was 2.35% by weight (calculated as Al). The silicon content was 1.00% by weight (calculated as SiO


2


). The content of soluble sodium salt of the high-density spindle-shaped hematite particles was 1612 ppm (calculated as Na) and the content of soluble sulfate was 2101 ppm (calculated as SO


4


). The pH value of the high-density spindle-shaped hematite particles was 5.7.




<Treatment of high-density spindle-shaped hematite particles in an aqueous alkali solution>




The concentration of the high-density spindle-shaped hematite particles in the slurry was adjusted to 50 g/liter, and 5 liter of the slurry was adjusted to pH value 13.8 by adding a 6N-aqueous NaOH solution. The resulting slurry was then heated to 95° C. under stirring, and was held for 3 hours at 95° C.




The resultant slurry was then washed with water by a decantation method and the pH value of the slurry was adjusted to 10.5. The concentration of the slurry at this point was 98 g/liter.




The particles were filtered out through a Buchner filter, and the purified water was passed into the filtrate until the electric conductivity of the filtrate became not more than 30 μs. The particles were then dried by an ordinary method and pulverized to obtain the target high-density spindle-shaped hematite particles. The high-density spindle-shaped hematite particles obtained had an average major axial diameter of 0.0752 μm, a minor axial diameter of 0.0122 μm, and a specific ratio of 6.2. The geometric standard deviation of major axial diameter was 1.37, the geometric standard deviation of minor axial diameter was 1.24, the BET specific surface (S


BET


) was 83.4 m


2


/g, the S


BET


/S


TEM


value was 1.22. The content of soluble sodium salt of the high-density spindle-shaped hematite particles was 63 ppm (calculated as Na) and the content of soluble sulfate was 21 ppm (calculated as SO


4


). The pH value of the high-density spindle-shaped hematite particles was 9.1, and the resin adsorptivity thereof was 79.6%.




Example 13




<Production of non-magnetic substrate: Formation of non-magnetic undercoat layer on base film>




The same procedure as defined in Example 2 was conducted except that the spindle-shaped hematite particles which substantially uniformly contain aluminum within the particle, obtained in Example 12 were used instead of the spindle-shaped hematite particles, thereby obtaining a non-magnetic undercoat layer.




The thickness of the magnetic coating film was 3.5 μm.




The thus obtained non-magnetic undercoat layer had a gloss of 218%, a surface roughness Ra of 6.2 nm, and a Young's modulus (relative value) of coating film of 135.




Example 14




<Production of magnetic recording medium: Formation of magnetic recording layer>




The same procedure as defined in Example 3 was conducted except that the magnetic particles were changed to acicular magnetic metal particles (average major axis diameter: 0.110 μm, average minor axis diameter: 0.0146 μm, a geometric standard deviation of major axis diameter of 1.38, aspect ratio: 7.5:1, coercive force: 1943 Oe, saturation magnetization: 132 emu/g), and that the non-magnetic undercoat layer obtained in Example 13 was used, thereby producing a magnetic tape.




The thickness of the magnetic coating film was 1.0 μm.




The thus obtained magnetic tape had a coercive force Hc of 1989 Oe, a squareness (Br/Bm) of 0.88, a gloss of 238%, a surface roughness Ra of 5.8 nm, a Young's modulus (relative value) of coating film of 136, a linear absorption coefficient of 1.27 μm


−1


, a running durability of not less than 30 minutes and a scratch resistance of A.




Changes in the coercive force and the saturation magnetic flux density Bm with passage time were 2.8% and 2.1%, respectively.




Example 15




<Production of magnetic recording medium: Formation of magnetic recording layer>




The same procedure as defined in Example 3 was conducted except that the magnetic particles were changed to magnetic acicular metal particles (average major axis diameter: 0.115 μm, average minor axis diameter: 0.0145 pm, a geometric standard deviation of major axis diameter of 1.36, aspect ratio: 7.9:1, coercive force: 1909 Oe, saturation magnetization: 133.8 emu/g, aluminum content of 2.85% by weight, calculated as Al, (1.26% by weight, calculated as Al, of aluminum in the central portion, 0.84% by weight, calculated as Al, of aluminum in the surface layer portion, and 0.75% by weight, calculated as Al, of aluminum on the surface coating), Nd content of 0.12% by weight, resin adsorptivity: 81.6%), and that the non-magnetic undercoat layer obtained in Example 13 was used, thereby producing a magnetic tape.




The thickness of the magnetic coating film was 1.0 μm.




The thus obtained magnetic tape had a coercive force Hc of 1990 Oe, a squareness (Br/Bm) of 0.89, a gloss of 243%, a surface roughness Ra of 5.4 nm, a Young's modulus (relative value) of coating film of 138, a linear absorption coefficient of 1.26 μm


−1


, a running durability of not less than 30 minutes and a scratch resistance of A.




Changes in the coercive force and the saturation magnetic flux density Bm with passage time were 1.8% and 1.6%, respectively.




<Kinds of acicular goethite particles>




Precursor 1 to 6:




Various properties of acicular goethite particles as a precursor of acicular hematite particles are shown in Table 1.




Examples 16 to 22 and Comparative Examples 1 to 6




<Production of low-density acicular hematite particles>




Low-density acicular hematite particles were obtained in the same way as in Example 1 except for varying the kind of acicular goethite particles as a precursor, the kind and amount added of sintering preventive, and heat-dehydration temperature and time. Incidentally, the particles obtained in Comparative Example 4 were acicular goethite particles.




The main producing conditions and various properties are shown in Tables 2 to 3.




Examples 23 to 29 and Comparative Examples 7 to 11




<Production of high-density acicular hematite particles>




High-density acicular hematite particles were obtained in the same way as in Example 1 except for varying the kind of low-density acicular hematite particles, and heat-treating temperature and time for high densification.




The main producing conditions and various properties are shown in Tables 4 to 5.




Examples 30 to 36 and Comparative Examples 12 to 13




<Acid-dissolving treatment of acicular hematite particles>




Acicular hematite particles were obtained in the same way as in Example 1 except for varying the kind of high-density acicular hematite particles, use or non-use of the wet pulverization, the acid concentration, the pH value of slurry, and the heating temperature and time.




The main producing conditions and various properties are shown in Tables 6 to 7.




Examples 37 to 43 and Reference Examples 1 to 2




<Heat-treatment of acicular hematite particles in alkaline suspension>




The same procedure as defined in Example 1 was conducted except that kind of acicular hematite particles, pH value of slurry, heating temperature and heating time were varied, thereby obtaining acicular hematite particles.




Main production conditions and various properties are shown in Tables 8 and 9.




Example 44




<Surface-coating treatment of acicular hematite particles>




The concentration of the slurry having a pH value of 10.5 which was obtained in Example 37 by washing the slurry heat-treated in the alkaline suspension, with water by a decantation method, was 50 g/liter. 4 liters of the water-washed slurry was heated again to 60° C., and then mixed with 74.1 ml of 1.0N sodium aluminate aqueous solution (corresponding to 1.0% by weight calculated as Al based on the weight of the acicular hematite particles). After maintaining the slurry at that temperature for 30 minutes, the pH value of the slurry was adjusted to 8.0 using an aqueous acetic acid solution. Next, the slurry was sequentially subjected to filtration, washing with water, drying and pulverization in the same manner as in Example 1, thereby obtaining acicular hematite particles whose surfaces were coated with a hydroxide of aluminum.




Main production conditions and various properties are shown in Tables 10 and 11.




Examples 45 to 50




Acicular hematite particles coated with a coating material by an ordinary method were obtained in the same way as in Example 44 except for varying the kind of acicular hematite particles and the kind and amount of the coating material.




The main producing conditions and various properties are shown in Tables 10 and 11, respectively.




Examples 51 to 64. Comparative Examples 14 to 22 and Reference Examples 3 to 11




<Production of non-magnetic substrate: Formation of non-magnetic undercoat layer on non-magnetic base film>




By using the acicular hematite particles obtained in Example 30 to 50, Comparative Examples 1, 3 and 7 to 13 and Reference Examples 1 to 2, non-magnetic undercoat layers were formed in the same way as in Example 2.




The main producing conditions and various properties are shown in Tables 12 and 13, respectively.




<Production of magnetic recording medium: Formation of magnetic coating film>




Magnetic particles used for forming the magnetic recording layers and various properties thereof are shown in Table 14.




Examples 65 to 78, Comparative Examples 23 to 31 and Reference Examples 12 to 20




Magnetic recording media were produced in the same way as in Example 3 except for varying the kind of non-magnetic substrate and the kind of magnetic particles.




The main producing conditions and various properties are shown in Tables 15 and 16.




Examples 79 to 92, Comparative Examples 32 to 40 and Reference Examples 21 to 29




Magnetic recording media were produced in the same way as in Example 4 except for varying the kind of non-magnetic substrate and the kind of magnetic particles.




The main producing conditions and various properties are shown in Tables 17 and 18.




<Kinds of acicular goethite particles which substantially uniformly contain aluminum within the particle >




Precursor 7 to 13:




Various properties of acicular goethite particles as a precursor of acicular hematite particles are shown in Table 19.




Examples 93 to 99 and Comparative Examples 41 to 46




<Production of low-density acicular hematite particles which substantially uniformly contain aluminum within the particle>




Low-density acicular hematite particles were obtained in the same way as in Example 5 except for varying the kind of acicular goethite particles as a precursor, the kind and amount added of sintering preventive, and heat-dehydration temperature and time. Incidentally, the particles obtained in Comparative Example 44 were acicular goethite particles.




The main producing conditions and various properties are shown in Tables 20 to 21.




Examples 100 to 106 and Comparative Examples 47 to 51




<Production of high-density acicular hematite Particles which substantially uniformly contain aluminum within the Particle>




High-density acicular hematite particles were obtained in the same way as in Example 5 except for varying the kind of low-density acicular hematite particles, and heat-treating temperature and time for high densification.




The main producing conditions and various properties are shown in Tables 22 to 23.




Examples 107 to 113 and Comparative Examples 52 to 53




<Acid-dissolving treatment of acicular hematite particles which substantially uniformly contain aluminum within the particle>




Acicular hematite particles were obtained in the same way as in Example 5 except for varying the kind of high-density acicular hematite particles, use or non-use of the wet pulverization, the acid concentration, the pH value of slurry, and the heating temperature and time.




The main producing conditions and various properties are shown in Tables 24 to 25.




Examples 114 to 120 and Reference Examples 30 to 31




<Heat-treatment of acicular hematite Particles in alkaline suspension>




The same procedure as defined in Example 5 was conducted except that kind of acicular hematite particles, pH value of slurry, heating temperature and heating time were varied, thereby obtaining acicular hematite particles.




Main production conditions and various properties are shown in Tables 26 and 27.




Example 121




<Surface coating of acicular hematite particles which substantially uniformly contain aluminum within the particle>




The concentration of the slurry having a pH value of 10.5 which was obtained in Example 114 by washing the slurry heat-treated in the alkaline suspension, with water by a decantation method, was 50 g/liter. 4 liters of the water-washed slurry was heated again to 60° C., and then mixed with 74.1 ml of 1.ON sodium aluminate aqueous solution (corresponding to 1.0% by weight calculated as Al based on the weight of the acicular hematite particles). After maintaining the slurry at that temperature for 30 minutes, the pH value of the slurry was adjusted to 8.0 using an aqueous acetic acid solution. Next, the slurry was sequentially subjected to filtration, washing with water, drying and pulverization in the same manner as in Example 5, thereby obtaining acicular hematite particles whose surfaces were coated with a hydroxide of aluminum.




Main production conditions and various properties are shown in Tables 28 and 29.




Examples 122 to 127




Acicular hematite particles coated with a coating material by an ordinary method were obtained in the same way as in Example 121 except for varying the kind of acicular hematite particles and the kind and amount of the coating material.




The main producing conditions and various properties are shown in Tables 28 and 29.




Examples 128 to 141. Comparative Examples 54 to 62 and Reference Examples 32 to 40




<Production of non-magnetic substrate: Formation of non-magnetic undercoat layer on non-magnetic base film>




By using the acicular hematite particles obtained in Example 107 to 127 and Comparative Examples 41, 43 and 47 to 53 and Reference Examples 30 to 31, non-magnetic undercoat layers were formed in the same way as in Example 2.




The main producing conditions and various properties are shown in Tables 30 and 31.




Examples 142 to 155. Comparative Examples 63 to 71 and Reference Examples 41 to 49




<Production of magnetic recording medium: Formation of magnetic coating film>




Magnetic recording media were produced in the same way as in Example 3 except for varying the kind of non-magnetic substrate and the kind of magnetic particles.




The main producing conditions and various properties are shown in Tables 32 and 33.




<Kind of acicular goethite particles>




Goethite Particles 1 to 2:




Acicular goethite particles 1 and 2 as precursors having properties shown in Table 34 were prepared.




Goethite particles 3 to 5:




Acicular goethite particles 3 to 5 which were subjected to a sintering preventing treatmnent, were obtained in the same way as in Example 8 except for varying the kind of starting particles and the element and amount of sintering preventive.




Various properties of the obtained acicular goethite particles are shown in Table 35.




<Heat treatment>




Goethite particles 6 to 9:




Acicular goethite particles 6 to 9 were obtained in the same way as in Example 8 except for varying the kind of acicular goethite particles as precursors and the heat-treating temperature and time.




The main producing conditions are shown in Table 36 and various properties of the obtained acicular goethite particles are shown in Table 37.




<Production of low-density acicular hematite particles>




Hematite particles 1 to 4:




Low-density acicular hematite particles 1 to 4 were obtained in the same way as in Example 8 except for varying the kind of acicular goethite particles as precursors and the heat-dehydrating temperature and time.




The main producing conditions are shown in Table 38 and various properties of the obtained low-density acicular hematite particles are shown in Table 39.




<Production of high-density acicular hematite particles>




Hematite particles 5 to 13:




High-density acicular hematite particles were obtained in the same way as in Example 8 except for varying the kind of particles to be treated and the heat-treating temperature and time.




The main producing conditions are shown in Table 40 and various properties of the obtained high-density hematite particles are shown in Table 41.




Examples 156 to 159 and Reference Examples 50 to 51




<Heat-treatment of acicular hematite particles in alkaline suspension>




The same procedure as defined in Example 1 was conducted except that kind of acicular hematite particles, pH value of slurry, heating temperature and heating time were varied, thereby obtaining acicular hematite particles.




Main production conditions and various properties are shown in Tables 42 and 43.




Examples 160




<Surface coating treatment of acicular hematite particles>




After 700 g of the high-density acicular hematite particles obtained in the Example 156 were roughly pulverized by a Nara mill in advance, the obtained particles were charged into 7 liters of pure water and diagglomerated by a homomixer (manufactured by Tokushu-kika Kogyo, CO., Ltd.) for 60 minutes.




The slurry of the acicular hematite particles obtained was then dispersed for 6 hours at an axial rotation frequency of 2000 rpm while being circulated by a horizontal sand grinder (Dispermat SL, manufactured by S. C. Adichem, Co., Ltd.).




The pH value of the obtained slurry containing the acicular hematite particles was adjusted to 4.0 by using a 0.1 N acetic acid aqueous solution. By adding water to the slurry, the concentration of the resultant slurry was adjusted to 45 g/liter. 10 liter of the slurry was re-heated to 60° C., and 500 ml (equivalent to 3.0% by weight (calculated as Al) based on the acicular hematite particles) of a 1.0 mol/liter aqueous aluminum acetate solution was added to the slurry, and the mixture was held for 30 minutes. Thereafter, the pH value of the mixture was adjusted to 7.1 by using aqueous sodium hydroxide solution. After holding the mixture for 30 minutes, the particles were then filtered out, washed with water, dried and, thereby obtaining acicular hematite particles coated with a hydroxide of aluminum.




The main producing conditions and various properties are shown in Tables 44 and 45.




Examples 161 to 163




Acicular hematite particles coated with a coating material were obtained in the same way as in Example 160 except for varying the kind of acicular hematite particles to be treated, the pH value before coating, the kind and amount of additives, and the final pH value.




The main producing conditions are shown in Table 44 and various properties of the obtained acicular hematite particles are shown in Table 45.




Examples 164 to 171 Comparative Examples 72 to 76 and Reference Examples 52 to 53




<Production of non-magnetic substrate: Formation of non-magnetic undercoat layer on non-magnetic base film>




By using the acicular hematite particles 9 to 13 and the non-magnetic particles obtained in Example 156 to 163 and Reference Examples 50 to 51, non-magnetic undercoat layers were formed in the same way as in Example 2.




The main producing conditions and various properties of the obtained non-magnetic undercoat layers are shown in Table 46.




Examples 172 to 183. Comparative Examples 77 and 81 and Reference examples 54 to 55




<Production of magnetic recording medium: Formation of magnetic coating film>




Magnetic recording media were produced in the same way as in Example 3 except for varying the kind of non-magnetic substrate and the kind of magnetic particles.




The main producing conditions and various properties of the obtained magnetic recording media are shown in Table 47.




<Kind of acicular goethite particles which substantially uniformly contain aluminum within the particle>




Goethite particles 10 to 11:




Acicular goethite particles 10 and 11 as precursors having properties shown in Table 48 were prepared.




Goethite particles 12 to 14:




Acicular goethite particles 12 to 14 which were subjected to a sintering preventing treatment, were obtained in the same way as in Example 12 except for varying the kind of acicular goethite particles as precursors and the element and amount of sintering preventive.




Various properties of the obtained acicular goethite particles are shown in Table 49.




<Heat treatment>




Goethite particles 15 to 18:




Acicular goethite particles 15 to 18 were obtained in the same way as in Example 12 except for varying the kind of starting particles and the heat-treating conditions.




The main producing conditions are shown in Table 50 and various properties of the obtained acicular goethite particles are shown in Table 51.




<Production of low-density acicular hematite particles which substantially uniformly contain aluminum within the particle>




Hematite Particles 14 to 17:




Low-density acicular hematite particles 14 to 17 were obtained in the same way as in Example 12 except for varying the kind of acicular goethite particles as precursors and the heat-dehydrating temperature and time.




The main producing conditions are shown in Table 52 and various properties of the obtained low-density acicular hematite particles are shown in Table 53.




<Production of high-density acicular hematite particles which substantially uniformly contain aluminum within the particle >Hematite particles 18 to 26:




High-density acicular hematite particles were obtained in the same way as in Example 12 except for varying the kind of particles to be treated and the heat-treating temperature and time.




The main producing conditions are shown in Table 54 and various properties of the obtained high-density acicular hematite particles are shown in Table 55.




Examples 184 to 187 and Reference Examples 56 to 457




<Heat-treatment of acicular hematite particles in alkaline suspension>




The same procedure as defined in Example 12 was conducted except that kind of acicular hematite particles, use or non-use of heat-treatment in alkaline suspension, pH value of slurry, heating temperature and heating time were varied, thereby obtaining acicular hematite particles.




Main production conditions and various properties are shown in Tables 56 and 57.




Example 188




<Surface coating treatment of acicular hematite particles>




After 700 g of the high-density acicular hematite particles obtained in the Example 184 were roughly pulverized by a Nara mill in advance, the obtained particles were charged into 7 liters of pure water and diagglomerated by a homomixer (manufactured by Tokushu-kika Kogyo, CO., Ltd.) for 60 minutes.




The slurry of the acicular hematite particles obtained was then dispersed for 6 hours at an axial rotation frequency of 2000 rpm while being circulated by a horizontal sand grinder (Dispermat SL, manufactured by S.C. Adichem, CO., Ltd.).




The pH value of the obtained slurry containing the acicular hematite particles was adjusted to 4.0 by using a 0.1 N acetic acid aqueous solution. By adding water to the slurry, the concentration of the resultant slurry was adjusted to 45 g/liter. 10 liter of the slurry was re-heated to 60° C., and 500 ml (equivalent to 3.0% by weight (calculated as Al) based on the acicular hematite particles) of a 1.0 mol/liter aqueous aluminum acetate solution was added to the slurry, and the mixture was held for 30 minutes. Thereafter, the pH value of the mixture was adjusted to 7.0 by using aqueous sodium hydroxide solution. After holding the mixture for 30 minutes, the particles were then filtered out, washed with water, dried and, thereby obtaining acicular hematite particles coated with a hydroxide of aluminum.




The main producing conditions and various properties are shown in Tables 58 and 59.




Examples 189 to 191




Acicular hematite particles coated with a coating material were obtained in the same way as in Example 188 except for varying the kind of particles to be treated, the pH value before coating, the kind and amount of additives, and the final pH value.




The main producing conditions are shown in Table 58 and various properties of the obtained acicular hematite particles are shown in Table 59.




Example 192 to 199. Comparative Examples 82 to 986 and Reference examples 58 to 59




<Production of non-magnetic substrate: Formation of non-magnetic undercoat layer on non-magnetic base film>




By using the acicular hematite particles 22 to 26 and the non-magnetic particles obtained in Example 184 to 191, and Reference Examples 56 to 57, non-magnetic undercoat layers were formed in the same way as in Example 2.




The main producing conditions and various properties of the obtained non-magnetic undercoat layers are shown in Table 60.




Examples 200 to 211. Comparative Examples 87 and 91 and Reference examples 60 to 61




<Production of magnetic recording medium: Formation of magnetic coating film>




Magnetic recording media were produced in the same way as in Example 3 except for varying the kind of non-magnetic substrate and the kind of magnetic particles.




The main producing conditions and various properties of the obtained magnetic recording media are shown in Table 61.















TABLE 1













Properties of acicular goethite particles
















Production





Geometrical







method of





standard







acicular




Average major




deviation of






Kind of




goethite




axial diameter




major axial






Precursor




particles




(μm)




diameter (−)









Precursor




(B)




0.181




1.32






1






Precursor




(C)




0.230




1.31






2






Precursor




(D)




0.251




1.28






3






Precursor




(A)




0.200




1.36






4






Precursor




(E)




0.160




1.35






5






Precursor




(F)




0.271




1.32






6
















Properties of acicular goethite particles


















Geometrical










standard








Average minor




deviation of







Kind of




axial diameter




minor axial




Aspect ratio







Precursor




(μm)




diameter (−)




(−)











Precursor




0.0229




1.38




7.9:1







1







Precursor




0.0277




1.37




8.3:1







2







Precursor




0.0285




1.38




8.8:1







3







Precursor




0.0225




1.40




8.9:1







4







Precursor




0.0210




1.38




7.6:1







5







Precursor




0.0319




1.38




8.5:1







6


















Properties of acicular goethite particles


















Soluble




Soluble









sodium salt




sulfate







BET specific




(calculated




(calculated




pH






Kind of




surface area




as Na)




as SO


4


)




value






Precursor




(m


2


/g)




(ppm)




(ppm)




(−)









Precursor




138.2




678




387




6.8






1






Precursor




98.6




412




1,234




5.3






2






Precursor




86.1




612




823




6.3






3






Precursor




81.8




986




343




8.2






4






Precursor




163.8




789




546




6.6






5






Precursor




65.1




423




751




6.0






6

























TABLE 2













Kind of




Anti-sintering treatment















Examples and




acicular






Amount






Comparative




goethite





Calcu-




added






Examples




particles




Kind




lated as




(wt %)









Example 16




Particles




Water glass #3




SiO


2






1.0







obtained in







Example 1






Example 17




Precursor 1




Water glass #3




SiO


2






2.0








Phosphoric acid




P




1.0






Example 18




Precursor 2




Phosphoric acid




P




2.5






Example 19




Precursor 3




Sodium hexa-




P




1.8








metaphosphate






Example 20




Precursor 4




Water glass #3




SiO


2






3.0






Example 21




Precursor 5




Sodium hexa-




P




1.0








metaphosphate






Example 22




Precursor 6




Water glass #3




SiO


2






3.5








Phosphoric acid




P




1.5






Comparative




Particles





















Example 1




obtained in







Example 1






Comparative




Particles





















Example 2




obtained in







Example 1






Comparative




Particles




Water glass #3




SiO


2






1.0






Example 3




obtained in







Example 1






Comparative




Particles




Phosphoric acid




P




1.0






Example 4




obtained in







Example 1






Comparative




Particles




Phosphoric acid




P




1.5






Example 5




obtained in







Example 1






Comparative




Precursor 6




Water glass #3




SiO


2






1.5






Example 6


















Examples and









Comparative




Heat-dehydration















Examples




Temperature (° C.)




Time (min)











Example 16




330




60







Example 17




360




30







Example 18




340




60







Example 19




310




120







Example 20




360




75







Example 21




330




90







Example 22




380




60







Comparative




310




60







Example 1







Comparative




340




30







Example 2







Comparative




320




60







Example 3







Comparative

















Example 4







Comparative




350




60







Example 5







Comparative




330




60







Example 6

























TABLE 3













Properties of low-density acicular hematite particles
















Average




Geometrical




Average




Geometrical






Examples




major




standard




minor




standard






and




axial




deviation of




axial




deviation of






Comparative




diameter




major axial




diameter




minor axial






Examples




(μm)




diameter (−)




(μm)




diameter (−)









Example 16




0.142




1.37




0.0192




1.38






Example 17




0.153




1.35




0.0196




1.38






Example 18




0.199




1.34




0.0246




1.38






Example 19




0.213




1.31




0.0250




1.38






Example 20




0.168




1.39




0.0195




1.41






Example 21




0.126




1.36




0.0172




1.37






Example 22




0.230




1.35




0.0291




1.39






Comparative




0.139




1.37




0.0194




1.38






Example 1






Comparative




0.138




1.37




0.0197




1.38






Example 2






Comparative




0.141




1.36




0.0191




1.38






Example 3






Comparative


























Example 4






Comparative




0.142




1.37




0.0191




1.38






Example 5






Comparative




0.230




1.35




0.0291




1.38






Example 6















Examples




Properties of low-density acicular hematite particles















and




Aspect






S


BET


/S


TEM








Comparative




ratio




S


BET






S


TEM






value






Examples




(−)




(m


2


/g)




(m


2


/g)




(−)









Example 16




7.4:1




151.6




42.8




3.54






Example 17




7.8:1




179.4




41.8




4.30






Example 18




8.1:1




143.0




33.2




4.31






Example 19




8.5:1




123.7




32.6




3.80






Example 20




8.6:1




143.7




41.7




3.44






Example 21




7.3:1




196.6




47.8




4.12






Example 22




7.9:1




110.5




28.1




3.93






Comparative




7.2:1




146.8




42.4




3.46






Example 1






Comparative




7.0:1




130.6




41.8




3.12






Example 2






Comparative




7.4:1




168.6




43.0




3.92






Example 3






Comparative


























Example 4






Comparative




7.4:1




163.2




43.0




3.80






Example 5






Comparative




7.9:1




 91.2




28.1




3.24






Example 6
















Properties of low-density acicular hematite particles

















Soluble










sodium




Soluble








salt




sulfate






Examples




Amount of sintering




(calcu-




(calcu-






and




preventive




lated as




lated as




pH
















Comparative




Calcu-




Content




Na)




SO


4


)




value






Examples




lated as




(wt %)




(ppm)




(ppm)




(−)









Example 16




SiO


2






1.09




1,653




  925




6.0






Example 17




SiO


2






2.77




1,561




1,110




5.9







P




1.07






Example 18




P




2.73




1,356




1,610




6.1






Example 19




P




1.95




1,282




1,583




6.6






Example 20




SiO


2






3.21




2,582




  632




7.8






Example 21




P




1.10




1,376




  652




5.6






Example 22




SiO


2






3.81




1,168




3,265




4.8







P




1.64






Comparative














  726




  586




5.7






Example 1






Comparative














  832




  612




5.6






Example 2






Comparative




SiO


2






1.09




1,231




1,010




5.8






Example 3






Comparative














2,663




  713




7.5






Example 4






Comparative




P




1.64




1,183




1,121




6.1






Example 5






Comparative




SiO


2






1.63




1,216




  892




6.4






Example 6



























TABLE 4














Kind of










low-density




Heat treatment for high







Examples and




acicular




densification
















Comparative




hematite




Temperature




Time







Examples




particles




(° C.)




(min)











Example 23




Example 16




680




60







Example 24




Example 17




690




30







Example 25




Example 18




720




20







Example 26




Example 19




660




60







Example 27




Example 20




640




30







Example 28




Example 21




680




60







Example 29




Example 22




730




30







Comparative




Comparative




680




20







Example 7




Example 2







Comparative




Comparative




670




30







Example 8




Example 4







Comparative




Comparative




450




60







Example 9




Example 5







Comparative




Comparative




850




20







Example 10




Example 6







Comparative




Comparative




680




30







Example 11




Example 6

























TABLE 5













Properties of high-density acicular hematite particles
















Average




Geometrical




Average




Geometrical







major




standard




minor




standard






Examples and




axial




deviation of




axial




deviation of






Comparative




diameter




major axial




diameter




minor axial






Examples




(μm)




diameter (−)




(μm)




diameter (−)









Example 23




0.136




1.37




0.0195




1.39






Example 24




0.152




1.36




0.0200




1.38






Example 25




0.197




1.35




0.0249




1.39






Example 26




0.211




1.33




0.0252




1.38






Example 27




0.166




1.41




0.0195




1.42






Example 28




0.126




1.36




0.0173




1.38






Example 29




0.231




1.36




0.0296




1.40






Comparative




0.070




1.83




0.0330




1.68






Example 7






Comparative




0.126




1.64




0.0228




1.61






Example 8






Comparative




0.142




1.37




0.0191




1.39






Example 9






Comparative




0.100




1.71




0.0263




1.38






Example 10






Comparative




0.229




1.36




0.0292




1.38






Example 11















Examples




Properties of high-density acicular hematite particles















and




Aspect






S


BET


/S


TEM








Comparative




ratio




S


BET






S


TEM






value






Examples




(−)




(m


2


/g)




(m


2


/g)




(−)









Example 23




7.0:1




50.4




42.3




1.19






Example 24




7.6:1




52.5




41.0




1.28






Example 25




7.9:1




41.4




32.8




1.26






Example 26




8.4:1




41.4




32.3




1.28






Example 27




8.5:1




53.6




41.8




1.28






Example 28




7.3:1




55.1




47.5




1.16






Example 29




7.8:1




42.9




27.7




1.55






Comparative




2.1:1




14.6




28.8




0.51






Example 7






Comparative




5.5:1




26.7




36.8




0.73






Example 8






Comparative




7.4:1




111.6 




43.0




2.60






Example 9






Comparative




3.8:1




25.6




33.1




0.77






Example 10






Comparative




7.8:1




41.3




28.0




1.47






Example 11
















Properties of high-density acicular hematite particles

















Soluble










sodium




Soluble








salt




sulfate







Amount of sintering




(calcu-




(calcu-






Examples and




preventive




lated as




lated as




pH
















Comparative




Calcu-




Content




Na)




SO


4


)




value






Examples




lated as




(wt %)




(ppm)




(ppm)




(−)









Example 23




SiO


2






1.08




2,382




2,652




5.5






Example 24




SiO


2






2.76




2,265




2,783




4.9







P




1.07






Example 25




P




2.73




1,982




3,326




5.6






Example 26




P




1.95




1,765




3,273




5.1






Example 27




SiO


2






3.22




3,039




1,076




7.5






Example 28




P




1.11




2,162




2,765




4.6






Example 29




SiO


2






3.82




1,963




2,838




4.3







P




1.65






Comparative














1,365




1,863




5.8






Example 7






Comparative














1,462




1,921




6.1






Example 8






Comparative




P




1.64




1,763




2,563




5.1






Example 9






Comparative




SiO


2






1.63




2,762




3,362




4.8






Example 10






Comparative




SiO


2






1.64




2,562




2,863




5.5






Example 11



























TABLE 6














Kind of high-









Examples and




density acicular




Wet-pulverization
















Comparative




hematite




Use or




Residue on







Examples




particles




non-use




sieve (wt %)











Example 30




Example 23




used




0







Example 31




Example 24




used




0







Example 32




Example 25




used




0







Example 33




Example 26




used




0







Example 34




Example 27




used




0







Example 35




Example 28




used




0







Example 36




Example 29




used




0







Comparative




Particles




used




0







Example 12




obtained in








Example 1







Comparative




Comparative




used




0







Example 13




Example 11
















Examples




Acid-dissolving treatment
















and





Concent-




Tempera-





pH






Comparative




Kind of




ration




ture




Time




value






Examples




acid




(N)




(° C.)




(Hr)




(−)









Example 30




Sulfuric




1.4




90




3.0




0.68







acid






Example 31




Sulfuric




1.5




85




5.5




0.56







acid






Example 32




Sulfuric




2.0




90




5.0




0.32







acid






Example 33




Sulfuric




1.5




75




7.0




0.74







acid






Example 34




Sulfuric




1.2




70




2.0




0.81







acid






Example 35




Sulfuric




1.3




90




1.0




0.91







acid






Example 36




Sulfuric




1.5




85




8.0




0.70







acid






Comparative




Sulfuric




3.2E−05




80




5.0




4.5 






Example 12




acid






Comparative




Sulfuric




3.8E−04




80




7.0




3.8 






Example 13




acid
























TABLE 7













Properties of acicular hematite particles washed







with water after acid-dissolving treatment

















Geometrical





Geometrical







Average




standard




Average




standard






Examples




major




deviation of




minor




deviation of






and




axial




major axial




axial




minor axial






Comparative




diameter




diameter




diameter




diameter






Examples




(μm)




(−)




(μm)




(−)









Example 30




0.130




1.34




0.0188




1.33






Example 31




0.143




1.32




0.0181




1.32






Example 32




0.175




1.31




0.0216




1.33






Example 33




0.200




1.31




0.0235




1.31






Example 34




0.164




1.39




0.0193




1.34






Example 35




0.126




1.35




0.0173




1.32






Example 36




0.193




1.32




0.0238




1.34






Comparative




0.136




1.37




0.0195




1.38






Example 12






Comparative




0.230




1.36




0.0296




1.38






Example 13
















Properties of acicular hematite particles washed






Examples




with water after acid-dissolving treatment
















and




Aspect




Amount






S


BET


/S


TEM








Comparative




ratio




dissolved




S


BET






S


TEM






value






Examples




(−)




(wt %)




(m


2


/g)




(m


2


/g)




(−)









Example 30




6.9:1




26.5




55.4




43.9




1.26






Example 31




7.9:1




35.6




58.1




45.2




1.29






Example 32




8.1:1




41.2




46.6




37.8




1.23






Example 33




8.5:1




21.6




43.2




34.7




1.25






Example 34




8.5:1




10.2




57.8




42.2




1.37






Example 35




7.3:1




 6.8




56.2




47.5




1.18






Example 36




8.1:1




49.6




46.6




34.3




1.36






Comparative




7.0:1




 0.3




51.0




42.3




1.21






Example 12






Comparative




7.8:1




 1.2




41.8




27.7




1.51






Example 13
















Properties of acicular hematite particles washed







with water after acid-dissolving treatment

















Soluble sodium









Examples




salt




Soluble sulfate







and




(calculated as




(calculated as







Comparative




Na)




SO


4


)




pH value







Examples




(ppm)




(ppm)




(−)











Example 30




126




326




4.6







Example 31




141




412




5.3







Example 32




 98




512




5.1







Example 33




121




286




5.3







Example 34




 68




211




5.1







Example 35




111




268




4.6







Example 36




123




312




4.5







Comparative




368




512




5.0







Example 12







Comparative




346




536




4.8







Example 13

























TABLE 8












Kind of








acicular hematite




Heat treatment in aqueous






Examples




particles




alkali solution















and




subjected to acid-




pH








Reference




dissolving




value




Temperature




Time






Examples




treatment




(−)




(° C.)




(min)









Example 37




Example 30




13.5




90




180






Example 38




Example 31




13.8




85




120






Example 39




Example 32




13.1




95




180






Example 40




Example 33




13.5




98




240






Example 41




Example 34




13.3




80




120






Example 42




Example 35




13.5




90




300






Example 43




Example 36




13.6




85




 90






Reference




Example 30




 9.5




90




180






Example 1






Reference




Example 30




13.1




45




180






Example 2
























TABLE 9













Properties of acicular hematite particles washed







with water after heat-treatment in aqueous alkali solution
















Average




Geometrical




Average




Geometrical






Examples




major




standard




minor




standard






and




axial




deviation of




axial




deviation of






Reference




diameter




major axial




diameter




minor axial






Examples




(μm)




diameter (−)




(μm)




diameter (−)









Example 37




0.130




1.34




0.0188




1.33






Example 38




0.143




1.33




0.0180




1.32






Example 39




0.174




1.31




0.0216




1.33






Example 40




0.201




1.31




0.0235




1.31






Example 41




0.163




1.38




0.0192




1.34






Example 42




0.126




1.35




0.0173




1.33






Example 43




0.194




1.32




0.0238




1.33






Reference




0.130




1.34




0.0188




1.38






Example 1






Reference




0.130




1.34




0.0188




1.39






Example 2
















Properties of acicular hematite particles washed






Examples




with water after heat-treatment in aqueous alkali solution















and







S


BET


/S


TEM








Reference




Aspect




S


BET






S


TEM






value






Examples




ratio (−)




(m


2


/g)




(m


2


/g)




(−)









Example 37




6.9:1




55.2




43.9




1.26






Example 38




7.9:1




58.3




45.4




1.28






Example 39




8.1:1




46.7




37.8




1.23






Example 40




8.6:1




43.4




34.6




1.25






Example 41




8.5:1




58.1




42.4




1.37






Example 42




7.3:1




56.6




47.5




1.19






Example 43




8.2:1




47.0




34.3




1.37






Reference




6.9:1




55.5




43.9




1.26






Example 1






Reference




6.9:1




55.6




43.9




1.27






Example 2
















Properties of acicular hematite particles washed







with water after heat-treatment in aqueous alkali solution














Examples




Soluble sodium




Soluble sulfate







and




salt




(calculated as






Reference




(calculated as Na)




SO


4


)




pH value






Examples




(ppm)




(ppm)




(−)









Example 37




116 




13




9.1






Example 38




98




 6




9.3






Example 39




86




12




8.9






Example 40




68




31




8.7






Example 41




72




 1




9.3






Example 42




96




 3




9.0






Example 43




121 




10




9.5






Reference




116 




286 




7.6






Example 1






Reference




106 




182 




7.8






Example 2
























TABLE 10













Surface treatment















Kind of acicular





Amount







hematite





added







particles heat-




Kind of




(calculated







treated in




surface




as Al or







aqueous alkali




treatment




SiO


2


)






Examples




solution




material




(wt %)









Example 44




Example 37




Sodium aluminate




1.0






Example 45




Example 38




Water glass #3




0.5






Example 46




Example 39




Aluminum sulfate




2.0








Water glass #3




1.0






Example 47




Example 40




Aluminum acetate




5.0






Example 48




Example 41




Sodium aluminate




1.0








Colloidal silica




1.5






Example 49




Example 42




Colloidal silica




3.0






Example 50




Example 43




Sodium aluminate




12.0 

















Coating material














Coating amount







(calculated as Al or







SiO


2


)















Examples




Kind*




(wt %)











Example 44




A




0.99







Example 45




S




0.49







Example 46




A




1.95








S




0.98







Example 47




A




4.78







Example 48




A




0.98








S




1.47







Example 49




S




2.90







Example 50




A




10.75 













Note











*“A” represents a hydroxide of aluminum.











 “S” represents an oxide of silicon.























TABLE 11













Properties of acicular hematite particles washed







with water after surface treatment

















Geometrical





Geometrical







Average




standard




Average




standard







major




deviation of




minor




deviation of







axial




major axial




axial




minor axial







diameter




diameter




diameter




diameter






Examples




(μm)




(−)




(μm)




(−)









Example 44




0.130




1.34




0.0189




1.33






Example 45




0.143




1.33




0.0180




1.32






Example 46




0.174




1.31




0.0216




1.33






Example 47




0.200




1.31




0.0235




1.31






Example 48




0.164




1.38




0.0192




1.34






Example 49




0.126




1.35




0.0173




1.33






Example 50




0.194




1.32




0.0239




1.32

















Properties of acicular hematite particles washed








with water after surface treatment





















S


BET


/S


TEM










Aspect




S


BET






S


TEM






value







Examples




ratio (−)




(m


2


/g)




(m


2


/g)




(−)











Example 44




6.9:1




55.8




43.7




1.28







Example 45




7.9:1




58.0




45.4




1.28







Example 46




8.1:1




47.0




37.8




1.24







Example 47




8.5:1




43.5




34.7




1.26







Example 48




8.5:1




57.9




42.4




1.37







Example 49




7.3:1




56.0




47.5




1.18







Example 50




8.1:1




45.5




34.2




1.33

















Properties of acicular hematite particles washed







with water after surface treatment

















Soluble sodium










salt




Soluble sulfate








(calculated as




(calculated as








Na)




SO


4


)




pH value







Examples




(ppm)




(ppm)




(−)











Example 44




86




2




9.3







Example 45




63




3




9.1







Example 46




52




5




8.9







Example 47




32




8




9.0







Example 48




16




10 




8.8







Example 49




72




12 




9.1







Example 50




68




6




9.4


























TABLE 12













Production of non-magnetic








coating composition




Non-magnetic

















Kind of




Weight ratio




coating








acicular




of particles




composition








hematite




to resin




Viscosity







Examples




particles




(−)




(cP)











Example 51




Example 37




5.0




358







Example 52




Example 38




5.0




384







Example 53




Example 39




5.0




384







Example 54




Example 40




5.0




205







Example 55




Example 41




5.0




358







Example 56




Example 42




5.0




435







Example 57




Example 43




5.0




333







Example 58




Example 44




5.0




333







Example 59




Example 45




5.0




310







Example 60




Example 46




5.0




384







Example 61




Example 47




5.0




230







Example 62




Example 48




5.0




218







Example 63




Example 49




5.0




192







Example 64




Example 50




5.0




179


















Properties of non-magnetic undercoat layer





















Surface




Young's










roughness




modulus








Thickness




Gloss




Ra




(relative







Examples




(μm)




(%)




(nm)




value)











Example 51




3.5




210




6.4




122







Example 52




3.5




198




6.8




121







Example 53




3.5




206




6.4




126







Example 54




3.3




201




6.8




131







Example 55




3.4




215




6.0




124







Example 56




3.5




218




5.6




122







Example 57




3.5




215




5.7




133







Example 58




3.4




211




5.6




125







Example 59




3.3




206




6.0




126







Example 60




3.4




210




6.2




129







Example 61




3.3




209




6.8




139







Example 62




3.5




219




6.3




128







Example 63




3.5




223




5.0




124







Example 64




3.5




218




6.8




136


























TABLE 13













Production of non-magnetic
















Comparative




coating composition




Non-magnetic
















Examples




Kind of




Weight ratio




coating







and




acicular




of particles




composition







Reference




hematite




to resin




Viscosity







Examples




particles




(−)




(cP)











Comparative




Comparative




5.0




8,320  







Example 14




Example 1







Comparative




Comparative




5.0




10,880  







Example 15




Example 3







Comparative




Comparative




5.0




435







Example 16




Example 7







Comparative




Comparative




5.0




563







Example 17




Example 8







Comparative




Comparative




5.0




5,760  







Example 18




Example 9







Comparative




Comparative




5.0




230







Example 19




Example 10







Comparative




Comparative




5.0




384







Example 20




Example 11







Comparative




Comparative




5.0




435







Example 21




Example 12







Comparative




Comparative




5.0




410







Example 22




Example 13







Reference




Example 30




5.0




384







Example 3







Reference




Example 31




5.0




410







Example 4







Reference




Example 32




5.0




435







Example 5







Reference




Example 33




5.0




205







Example 6







Reference




Example 34




5.0




384







Example 7







Reference




Example 35




5.0




358







Example 8







Reference




Example 36




5.0




410







Example 9







Reference




Reference




5.0




384







Example 10




Example 1







Reference




Reference




5.0




358







Example 11




Example 2



















Comparative




Properties of non-magnetic undercoat layer


















Examples






Surface




Young's







and






roughness




modulus







Reference




Thickness




Gloss




Ra




(relative







Examples




(μm)




(%)




(nm)




value)











Comparative




3.6




128




21.6




108







Example 14







Comparative




3.8




 86




42.6




 96







Example 15







Comparative




3.5




141




19.8




109







Example 16







Comparative




3.5




176




12.4




113







Example 17







Comparative




3.6




121




27.6




105







Example 18







Comparative




3.5




159




16.6




109







Example 19







Comparative




3.4




186




9.6




116







Example 20







Comparative




3.5




188




9.3




118







Example 21







Comparative




3.5




176




13.1




115







Example 22







Reference




3.5




203




6.8




121







Example 3







Reference




3.4




193




7.0




122







Example 4







Reference




3.3




201




6.8




125







Example 5







Reference




3.4




196




7.6




135







Example 6







Reference




3.3




211




6.4




123







Example 7







Reference




3.5




216




5.8




121







Example 8







Reference




3.4




209




6.1




131







Example 9







Reference




3.5




204




6.8




121







Example 10







Reference




3.5




206




6.6




121







Example 11

























TABLE 14













Properties of acicular magnetic metal particles







containing iron as main component


















Geometrical








Average




Average




standard







major




minor




deviation of






Kind of




axial




axial




major axial




Aspect






magnetic




diameter




diameter




diameter




ratio






particles




(μm)




(μm)




(−)




(−)









Magnetic metal




0.110




0.0150




1.36




7.3:1






particles (a)






Magnetic metal




0.098




0.0134




1.35




7.3:1






particles (b)






Magnetic metal




0.101




0.0144




1.38




7.0:1






particles (c)






Magnetic metal




0.125




0.0184




1.35




6.8:1






particles (d)






Magnetic metal




0.127




0.0177




1.39




7.2:1






particles (e)






Magnetic metal




0.105




0.0148




1.36




7.1:1






particles (f)
















Properties of acicular magnetic metal particles







containing iron as main component
















Kind of




Coercive




Saturation








magnetic




force (Hc)




magnetization




pH value







particles




(Oe)




(emu/g)




(−)











Magnetic metal




1,915




131.6




9.5







particles (a)







Magnetic metal




1,938




130.5




10.1 







particles (b)







Magnetic metal




2,065




128.9




10.0 







particles (c)







Magnetic metal




1,896




130.8




9.8







particles (d)







Magnetic metal




1,915




135.6




9.5







particles (e)







Magnetic metal




1,680




128.3




9.9







particles (f)

















Properties of acicular magnetic metal particles







containing iron as main component







Content of Al
















Kind of




Central




Surface




Surface







magnetic




Portion




portion




coating layer







particles




(wt %)




(wt %)




(wt %)











Magnetic metal




2.61




1.36




0.01







particles (a)







Magnetic metal




1.32




2.84




0.01







particles (b)







Magnetic metal




1.38




2.65




0.78







particles (c)







Magnetic metal




0.01




0.01




0.01







particles (d)







Magnetic metal




0.01




0.01




0.01







particles (e)







Magnetic metal




0.01




0.01




0.01







particles (f)


















Properties of acicular magnetic metal particles







Kind of




containing iron as main component













magnetic




Content of Nd




Resin adsorption






particles




(wt %)




(%)









Magnetic metal




0.01




72.5






particles (a)






Magnetic metal




0.36




80.1






particles (b)






Magnetic metal




2.78




83.6






particles (c)






Magnetic metal




0.01




57.6






particles (d)






Magnetic metal




0.01




56.5






particles (e)






Magnetic metal




0.01




58.1






particles (f)

























TABLE 15













Production of magnetic recording medium




















Weight








Kind of





ratio of








non-





particles








magnetic




Kind of magnetic




to resin







Examples




substrate




particles




(−)











Example 65




Example 51




Particles used in




5.0









Example 3







Example 66




Example 52




Magnetic metal




5.0









particles (e)







Example 67




Example 53




Magnetic metal




5.0









particles (e)







Example 68




Example 54




Magnetic metal




5.0









particles (e)







Example 69




Example 55




Magnetic metal




5.0









particles (f)







Example 70




Example 56




Magnetic metal




5.0









particles (f)







Example 71




Example 57




Magnetic metal




5.0









particles (f)







Example 72




Example 58




Particles used in




5.0









Example 3







Example 73




Example 59




Magnetic metal




5.0









particles (e)







Example 74




Example 60




Magnetic metal




5.0









particles (e)







Example 75




Example 61




Magnetic metal




5.0









particles (e)







Example 76




Example 62




Magnetic metal




5.0









particles (f)







Example 77




Example 63




Magnetic metal




5.0









particles (f)







Example 78




Example 64




Magnetic metal




5.0









particles (f)


















Properties of magnetic recording medium



















Thickness











of magnetic




Coercive




Br/Bm








layer




force (Hc)




value




Gloss







Examples




(μm)




(Oe)




(−)




(%)











Example 65




1.1




1,975




0.87




225







Example 66




1.1




1,986




0.87




219







Example 67




1.1




1,990




0.88




221







Example 68




1.0




1,982




0.88




215







Example 69




1.1




1,781




0.88




238







Example 70




1.0




1,785




0.88




241







Example 71




1.1




1,780




0.89




231







Example 72




1.0




1,978




0.88




231







Example 73




1.1




1,980




0.87




230







Example 74




1.0




1,983




0.87




228







Example 75




1.1




1,991




0.88




233







Example 76




1.0




1,780




0.89




240







Example 77




1.1




1,778




0.89




243







Example 78




1.0




1,785




0.89




246

















Properties of magnetic recording medium













Corrosion resistance



















Linear




Percen-










absorp-




tage of




Percen-







Surface




Young's




tion




change in




tage of







rough-




modulus




coeffi-




coercive




change







ness Ra




(relative




cient




force




in Bm






Examples




(nm)




value)




(μm


−1


)




(%)




(%)









Example 65




6.2




124




1.22




4.6




4.2






Example 66




7.0




126




1.24




3.8




4.2






Example 67




6.6




125




1.25




3.2




3.9






Example 68




6.8




126




1.27




2.8




3.1






Example 69




6.2




127




1.24




3.1




2.8






Example 70




6.0




126




1.24




4.1




4.9






Example 71




6.2




128




1.23




3.9




3.5






Example 72




5.8




123




1.26




2.6




2.8






Example 73




6.0




126




1.24




1.6




1.3






Example 74




6.5




130




1.23




2.1




1.5






Example 75




5.6




143




1.28




1.6




3.2






Example 76




6.2




130




1.23




2.6




1.6






Example 77




5.8




126




1.22




1.1




2.8






Example 78




5.6




136




1.26




1.3




2.6

























TABLE 16













Production of magnetic recording medium

















Comparative






Weight







Examples






ratio of







and




Kind of non-





particles







Reference




magnetic




Kind of magnetic




to resin







Examples




substrate




particles




(−)











Comparative




Comparative




Magnetic metal




5.0







Example 23




Example 14




particles (e)







Comparative




Comparative




Magnetic metal




5.0







Example 24




Example 15




particles (e)







Comparative




Comparative




Magnetic metal




5.0







Example 25




Example 16




particles (e)







Comparative




Comparative




Magnetic metal




5.0







Example 26




Example 17




particles (e)







Comparative




Comparative




Magnetic metal




5.0







Example 27




Example 18




particles (e)







Comparative




Comparative




Magnetic metal




5.0







Example 28




Example 19




particles (f)







Comparative




Comparative




Magnetic metal




5.0







Example 29




Example 20




particles (f)







Comparative




Comparative




Magnetic metal




5.0







Example 30




Example 21




particles (f)







Comparative




Comparative




Magnetic metal




5.0







Example 31




Example 22




particles (f)







Reference




Reference




Magnetic metal




5.0







Example 12




Example 3




particles (e)







Reference




Reference




Magnetic metal




5.0







Example 13




Example 4




particles (e)







Reference




Reference




Magnetic metal




5.0







Example 14




Example 5




particles (e)







Reference




Reference




Magnetic metal




5.0







Example 15




Example 6




particles (e)







Reference




Reference




Magnetic metal




5.0







Example 16




Example 7




particles (e)







Reference




Reference




Magnetic metal




5.0







Example 17




Example 8




particles (f)







Reference




Reference




Magnetic metal




5.0







Example 18




Example 9




particles (f)







Reference




Reference




Magnetic metal




5.0







Example 19




Example 10




particles (f)







Reference




Reference




Magnetic metal




5.0







Example 20




Example 11




particles (f)

















Properties of magnetic recording medium

















Comparative




Thickness










Examples




of







and




magnetic




Coercive




Br/Bm







Reference




layer




force (Hc)




value




Gloss







Examples




(μm)




(Oe)




(−)




(%)











Comparative




1.3




1,958




0.74




136







Example 23







Comparative




1.2




1,941




0.78




121







Example 24







Comparative




1.1




1,975




0.83




171







Example 25







Comparative




1.0




1,969




0.84




186







Example 26







Comparative




1.3




1,953




0.76




158







Example 27







Comparative




1.1




1,775




0.82




183







Example 28







Comparative




1.1




1,768




0.85




194







Example 29







Comparative




1.0




1,732




0.85




193







Example 30







Comparative




1.1




1,763




0.84




180







Example 31







Reference




1.1




1,980




0.87




217







Example 12







Reference




1.1




1,983




0.87




212







Example 13







Reference




1.0




1,985




0.87




213







Example 14







Reference




1.1




1,982




0.87




210







Example 15







Reference




1.0




1,988




0.88




226







Example 16







Reference




1.1




1,780




0.88




226







Example 17







Reference




1.1




1,782




0.88




214







Example 18







Reference




1.0




1,775




0.88




211







Example 19







Reference




1.0




1,781




0.88




216







Example 20
















Comparative




Properties of magnetic recording medium














Examples






Linear






and




Surface





absorption






Reference




roughness Ra




Young's modulus




coefficient






Examples




(nm)




(relative value)




(μm


−1


)









Comparative




18.8




116




1.03






Example 23






Comparative




26.5




100




1.10






Example 24






Comparative




14.4




113




1.18






Example 25






Comparative




10.2




116




1.16






Example 26






Comparative




16.6




109




1.06






Example 27






Comparative




11.2




114




1.12






Example 28






Comparative




8.2




119




1.19






Example 29






Comparative




8.4




119




1.16






Example 30






Comparative




10.2




117




1.13






Example 31






Reference




6.8




123




1.23






Example 12






Reference




6.8




125




1.24






Example 13






Reference




6.4




128




1.22






Example 14






Reference




7.2




136




1.28






Example 15






Reference




6.8




125




1.26






Example 16






Reference




6.0




124




1.24






Example 17






Reference




5.9




135




1.22






Example 18






Reference




6.3




124




1.23






Example 19






Reference




6.2




124




1.23






Example 20


















Comparative




Properties of magnetic recording medium








Examples




Corrosion resistance















and




Percentage of change




Percentage of change







Reference




in coercive force




in Bm







Examples




(%)




(%)











Comparative




46.3




36.5







Example 23







Comparative




53.6




32.1







Example 24







Comparative




46.0




36.8







Example 25







Comparative




39.3




31.5







Example 26







Comparative




39.8




29.6







Example 27







Comparative




41.6




32.0







Example 28







Comparative




23.8




21.8







Example 29







Comparative




19.6




17.8







Example 30







Comparative




23.9




25.6







Example 31







Reference




15.6




18.2







Example 12







Reference




18.2




17.6







Example 13







Reference




18.6




18.8







Example 14







Reference




14.8




16.1







Example 15







Reference




11.8




13.6







Example 16







Reference




15.1




16.8







Example 17







Reference




12.9




18.1







Example 18







Reference




12.1




14.6







Example 19







Reference




11.6




10.9







Example 20


























TABLE 17













Production of magnetic recording medium




















Weight










ratio of








Kind of non-





particles








magnetic




Kind of magnetic




to resin







Examples




substrate




particles




(−)











Example 79




Example 51




Particles used in




5.0









Example 4







Example 80




Example 52




Magnetic metal




5.0









particles (a)







Example 81




Example 53




Magnetic metal




5.0









particles (a)







Example 82




Example 54




Magnetic metal




5.0









particles (b)







Example 83




Example 55




Magnetic metal




5.0









particles (b)







Example 84




Example 56




Magnetic metal




5.0









particles (c)







Example 85




Example 57




Magnetic metal




5.0









particles (c)







Example 86




Example 58




Particles used in




5.0









Example 4







Example 87




Example 59




Magnetic metal




5.0









particles (a)







Example 88




Example 60




Magnetic metal




5.0









particles (a)







Example 89




Example 61




Magnetic metal




5.0









particles (b)







Example 90




Example 62




Magnetic metal




5.0









particles (b)







Example 91




Example 63




Magnetic metal




5.0









particles (c)







Example 92




Example 64




Magnetic metal




5.0









particles (c)


















Properties of magnetic recording medium



















Thickness











of








magnetic




Coercive




Br/Bm








layer




force (Hc)




value




Gloss







Examples




(μm)




(Oe)




(−)




(%)











Example 79




1.1




1,976




0.87




226







Example 80




1.0




1,981




0.87




221







Example 81




1.1




1,986




0.87




223







Example 82




1.0




2,000




0.87




214







Example 83




1.0




1,997




0.88




235







Example 84




1.1




2,138




0.88




240







Example 85




1.0




2,145




0.88




233







Example 86




1.1




1,978




0.88




230







Example 87




1.1




1,990




0.88




235







Example 88




1.0




1,984




0.88




226







Example 89




1.0




1,998




0.89




234







Example 90




1.0




2,006




0.89




241







Example 91




1.1




2,135




0.90




245







Example 92




1.0




2,141




0.89




245

















Properties of magnetic recording medium


















Linear










absorp-







Surface




Young's




tion




Durability

















rough-




modulus




coeffi-




Running








ness Ra




(relative




cient




time




Scratch






Examples




(nm)




value)




(μm


−1


)




(min)




resistance









Example 79




6.0




126




1.23




29.8




A






Example 80




6.8




128




1.24




22.6




B






Example 81




6.4




128




1.25




23.2




B






Example 82




6.8




130




1.27




26.5




A






Example 83




6.4




131




1.26




23.8




B






Example 84




6.0




131




1.25




≧30




A






Example 85




6.3




130




1.24




≧30




A






Example 86




6.1




127




1.24




≧30




A






Example 87




6.0




130




1.25




27.2




B






Example 88




6.8




132




1.25




28.8




A






Example 89




6.2




135




1.27




29.6




A






Example 90




5.8




136




1.27




≧30




A






Example 91




5.7




133




1.25




≧30




A






Example 92




5.7




133




1.24




≧30




A

















Properties of magnetic recording medium








Corrosion resistance

















Percentage of change




Percentage of change







Examples




in coercive force (%)




in B


m


(%)











Example 79




3.6




3.2







Example 80




4.9




4.8







Example 81




4.2




4.3







Example 82




2.1




2.5







Example 83




3.1




2.6







Example 84




3.6




3.8







Example 85




3.5




3.7







Example 86




3.3




3.0







Example 87




3.9




2.8







Example 88




3.7




3.0







Example 89




1.6




2.8







Example 90




1.3




2.6







Example 91




3.1




4.0







Example 92




2.8




3.8


























TABLE 18













Production of magnetic recording medium

















Comparative






Weight







Examples






ratio of







and




Kind of non-





particles







Reference




magnetic




Kind of magnetic




to resin







Examples




substrate




particles




(−)











Comparative




Comparative




Magnetic metal




5.0







Example 32




Example 14




particles (a)







Comparative




Comparative




Magnetic metal




5.0







Example 33




Example 15




particles (a)







Comparative




Comparative




Magnetic metal




5.0







Example 34




Example 16




particles (a)







Comparative




Comparative




Magnetic metal




5.0







Example 35




Example 17




particles (a)







Comparative




Comparative




Magnetic metal




5.0







Example 36




Example 18




particles (a)







Comparative




Comparative




Magnetic metal




5.0







Example 37




Example 19




particles (d)







Comparative




Comparative




Magnetic metal




5.0







Example 38




Example 20




particles (d)







Comparative




Comparative




Magnetic metal




5.0







Example 39




Example 21




particles (d)







Comparative




Comparative




Magnetic metal




5.0







Example 40




Example 22




particles (d)







Reference




Reference




Magnetic metal




5.0







Example 21




Example 3




particles (a)







Reference




Reference




Magnetic metal




5.0







Example 22




Example 4




particles (a)







Reference




Reference




Magnetic metal




5.0







Example 23




Example 5




particles (a)







Reference




Reference




Magnetic metal




5.0







Example 24




Example 6




particles (a)







Reference




Reference




Magnetic metal




5.0







Example 25




Example 7




particles (a)







Reference




Reference




Magnetic metal




5.0







Example 26




Example 8




particles (d)







Reference




Reference




Magnetic metal




5.0







Example 27




Example 9




particles (d)







Reference




Reference




Magnetic metal




5.0







Example 28




Example 10




particles (d)







Reference




Reference




Magnetic metal




5.0







Example 29




Example 11




particles (d)


















Properties of magnetic recording medium


















Comparative




Thickness










Examples




of







and




magnetic




Coercive




Br/Bm







Reference




layer




force (Hc)




value




Gloss







Examples




(μm)




(Oe)




(−)




(%)











Comparative




1.2




1,957




0.78




135







Example 32







Comparative




1.3




1,961




0.76




118







Example 33







Comparative




1.1




1,968




0.82




173







Example 34







Comparative




1.1




1,963




0.84




182







Example 35







Comparative




1.2




1,954




0.78




161







Example 36







Comparative




1.1




1,863




0.84




178







Example 37







Comparative




1.0




1,871




0.85




190







Example 38







Comparative




1.1




1,878




0.85




189







Example 39







Comparative




1.0




1,876




0.83




182







Example 40







Reference




1.1




1,981




0.87




218







Example 21







Reference




1.2




1,986




0.87




213







Example 22







Reference




1.1




1,983




0.87




210







Example 23







Reference




1.2




1,988




0.87




205







Example 24







Reference




1.1




1,983




0.87




218







Example 25







Reference




1.1




1,910




0.87




220







Example 26







Reference




1.1




1,906




0.88




218







Example 27







Reference




1.0




1,897




0.88




213







Example 28







Reference




1.1




1,907




0.88




217







Example 29


















Comparative




Properties of magnetic recording medium
















Examples






Linear







and




Surface





absorption







Reference




roughness Ra




Young's modulus




coefficient







Examples




(nm)




(relative value)




(μm


−1


)











Comparative




24.3




113




1.04







Example 32







Comparative




38.5




96




1.09







Example 33







Comparative




19.8




112




1.16







Example 34







Comparative




12.6




113




1.14







Example 35







Comparative




21.9




110




1.06







Example 36







Comparative




12.5




113




1.09







Example 37







Comparative




10.7




116




1.15







Example 38







Comparative




11.0




119




1.17







Example 39







Comparative




13.1




119




1.13







Example 40







Reference




6.6




122




1.22







Example 21







Reference




7.0




124




1.24







Example 22







Reference




7.3




126




1.23







Example 23







Reference




7.6




133




1.27







Example 24







Reference




6.4




124




1.27







Example 25







Reference




6.1




123




1.25







Example 26







Reference




6.0




126




1.23







Example 27







Reference




6.4




125




1.25







Example 28







Reference




6.1




124




1.24







Example 29



















Comparative









Examples




Properties of magnetic recording medium







and




Durability















Reference




Running time








Examples




(min)




Scratch resistance











Comparative




8.3




D







Example 32







Comparative




1.6




D







Example 33







Comparative




9.2




D







Example 34







Comparative




14.5




C







Example 35







Comparative




12.6




C







Example 36







Comparative




13.6




C







Example 37







Comparative




11.8




D







Example 38







Comparative




12.3




C







Example 39







Comparative




13.6




C







Example 40







Reference




22.9




B







Example 21







Reference




24.8




A







Example 22







Reference




24.2




B







Example 23







Reference




23.6




B







Example 24







Reference




25.2




A







Example 25







Reference




18.2




B







Example 26







Reference




20.1




B







Example 27







Reference




18.9




B







Example 28







Reference




20.6




B







Example 29



















Comparative









Examples




Properties of magnetic recording medium







and




Corrosion resistance















Reference




Percentage of change




Percentage of change







Examples




in coercive force (%)




in B


m


(%)











Comparative




38.2




32.6







Example 32







Comparative




41.2




28.1







Example 33







Comparative




36.5




29.2







Example 34







Comparative




31.3




26.5







Example 35







Comparative




32.1




21.3







Example 36







Comparative




36.5




16.8







Example 37







Comparative




17.9




17.8







Example 38







Comparative




16.5




21.6







Example 39







Comparative




19.8




17.3







Example 40







Reference




13.6




12.6







Example 21







Reference




17.8




16.5







Example 22







Reference




13.2




17.1







Example 23







Reference




12.6




15.6







Example 24







Reference




10.9




11.6







Example 25







Reference




13.1




12.8







Example 26







Reference




12.2




12.4







Example 27







Reference




13.6




13.1







Example 28







Reference




10.8




10.4







Example 29


























TABLE 19














Properties of acicular







Production of




goethite particles















acicular goethite





Geometrical







particles




Average




standard

















Kind of




major




deviation of








aluminum




axial




major axial






Kind of




Production




compound




diameter




diameter






Precursor




method




added




(μm)




(−)









Precursor




(B)




Aluminum




0.185




1.31






7





sulfate






Precursor




(C)




Aluminum




0.233




1.33






8





acetate






Precursor




(D)




Aluminum




0.246




1.26






9





sulfate






Precursor




(A)




Sodium




0.218




1.31






10





aluminate






Precursor




(E)




Aluminum




0.150




1.34






11





sulfate






Precursor




(F)




Aluminum




0.268




1.31






12





sulfate






Precursor




(A)









0.333




1.42






13
















Properties of acicular goethite particles


















Geometrical










Average




standard





BET







minor




deviation of





specific







axial




minor axial




Aspect




surface




Content






Kind of




diameter




diameter




ratio




area




of Al






Precursor




(μm)




(−)




(−)




(m


2


/g)




(wt %)









Precursor




0.0235




1.38




7.9:1




141.1




1.68






7






Precursor




0.0281




1.37




8.3:1




96.1




0.82






8






Precursor




0.0289




1.41




8.5:1




85.8




3.58






9






Precursor




0.0228




1.38




9.6:1




73.8




1.65






10






Precursor




0.0205




1.38




7.3:1




171.6




2.13






11






Precursor




0.0331




1.37




8.1:1




60.6




0.46






12






Precursor




0.0370




1.39




9.0:1




55.8











13
















Properties of acicular goethite particles

















Soluble




Soluble









sodium salt




sulfate








(calculated




(calculated







Kind of




as Na)




as SO


4


)




pH value







Precursor




(ppm)




(ppm)




(−)











Precursor




1,378




902




6.3







7







Precursor




889




774




6.5







8







Precursor




726




1,251




6.2







9







Precursor




583




645




7.9







10







Precursor




1,020




1,009




6.0







11







Precursor




1,406




503




5.3







12







Precursor




552




618




7.2







13

























TABLE 20











Examples




Kind of




Anti-sintering treatment















and




acicular




Kind of








Comparative




goethite




sintering




Calcu-




Amount






Examples




particles




preventive




lated as




(w %)









Example 93




Particles




Water glass #3




SiO


2






0.5







used in







Example 5






Example 94




Precursor




Water glass #3




SiO


2






1.0







7




Phosphoric acid




P




1.0






Example 95




Precursor




Phosphoric acid




P




1.5







8






Example 96




Precursor




Sodium hexa-




P




2.0







9




metaphosphate






Example 97




Precursor




Water glass #3




SiO


2






3.0







10






Example 98




Precursor




Sodium hexa-




P




1.5







11




metaphosphate






Example 99




Precursor




Water glass #3




SiO


2






2.0







12




Phosphoric acid




P




1.0






Comparative




Particles





















Example 41




used in







Example 5






Comparative




Particles





















Example 42




used in







Example 5






Comparative




Particles




Water glass #3




SiO


2






1.5






Example 43




used in







Example 5






Comparative




Particles




Phosphoric acid




P




1.5






Example 44




used in







Example 5






Comparative




Particles




Phosphoric acid




P




1.0






Example 45




used in







Example 5






Comparative




Precursor




Water glass #3




SiO


2






1.0






Example 46




13


















Examples and









Comparative




Heat-dehydration















Examples




Temperature (° C.)




Time (min)











Example 93




340




30







Example 94




350




60







Example 95




330




60







Example 96




330




60







Example 97




340




45







Example 98




300




120 







Example 99




360




30







Comparative




320




60







Example 41







Comparative




330




45







Example 42







Comparative




340




30







Example 43







Comparative

















Example 44







Comparative




340




30







Example 45







Comparative




320




60







Example 46

























TABLE 21













Properties of low-density acicular hematite particles

















Geometrical





Geometrical







Average




standard




Average




standard






Examples




major




deviation of




minor




deviation of






and




axial




major axial




axial




minor axial






Comparative




diameter




diameter




diameter




diameter






Examples




(μm)




(−)




(μm)




(−)









Example 93




0.144




1.35




0.0194




1.38






Example 94




0.150




1.36




0.0191




1.38






Example 95




0.195




1.29




0.0240




1.37






Example 96




0.215




1.33




0.0250




1.41






Example 97




0.171




1.33




0.0193




1.38






Example 98




0.120




1.36




0.0168




1.38






Example 99




0.234




1.33




0.0285




1.37






Comparative




0.142




1.36




0.0193




1.38






Example 41






Comparative




0.137




1.37




0.0198




1.38






Example 42






Comparative




0.140




1.36




0.0193




1.38






Example 43






Comparative


























Example 44






Comparative




0.143




1.37




0.0190




1.38






Example 45






Comparative




0.256




1.42




0.0331




1.39






Example 46















Examples




Properties of low-density acicular hematite particles
















and




Aspect




Content






S


BET


/S


TEM








Comparative




ratio




of Al




S


BET






S


TEM






value






Examples




(−)




(wt %)




(m


2


/g)




(m


2


/g)




(−)









Example 93




7.4:1




1.23




153.8




42.3




3.63






Example 94




7.9:1




1.82




149.0




42.8




3.48






Example 95




8.1:1




0.90




115.3




34.0




3.39






Example 96




8.6:1




3.90




111.5




32.6




3.42






Example 97




8.9:1




1.83




95.9




42.1




2.28






Example 98




7.1:1




2.35




180.6




49.0




3.69






Example 99




8.2:1




0.51




81.2




28.6




2.84






Comparative




7.4:1




1.23




148.3




42.6




3.48






Example 41






Comparative




6.9:1




1.24




136.8




41.7




3.28






Example 42






Comparative




7.3:1




1.23




151.2




42.6




3.55






Example 43






Comparative































Example 44






Comparative




7.5:1




1.22




158.6




43.2




3.67






Example 45






Comparative




7.7:1









78.8




24.7




3.18






Example 46
















Properties of low-density acicular hematite particles


















Soluble










Amount of




sodium




Soluble







sintering




salt




sulfate







preventive




(calcu-




(calcu-





Resin


















Calcu-





lated




lated




pH




adsorp-






Ex. and




lated




Content




as Na)




as SO


4


)




value




tion






Com. Ex.




as




(wt %)




(ppm)




(ppm)




(−)




(%)









Ex. 93




SiO


2






0.55




1,705




964




6.3











Ex. 94




SiO


2






1.07




2,108




1,332




6.2












P




1.07






Ex. 95




P




1.68




1,811




1,290




6.4











Ex. 96




P




2.27




1,493




1,688




6.1











Ex. 97




SiO


2






3.27




1,276




919




7.3











Ex. 98




P




1.67




1,929




1,456




5.9











Ex. 99




SiO


2






2.21




2,352




827




5.8












P




1.11






Com. Ex.














1,695




953




6.3




46.8






41






Com. Ex.














1,714




987




6.4











42






Com. Ex.




SiO


2






1.65




1,742




1,001




6.2




40.6






43






Com. Ex.




P




1.50




  987




685




6.5











44






Com. Ex.




P




1.09




1,671




972




6.3











45






Com. Ex.




SiO


2






1.10




1,198




1,045




6.9











46



























TABLE 22














Kind of low-









Examples




density




Heat-treatment for high







and




acicular




densification
















Comparative




hematite




Temperature




Time







Examples




particles




(° C.)




(min)











Example 100




Example 93




630




60







Example 101




Example 94




650




60







Example 102




Example 95




680




30







Example 103




Example 96




640




75







Example 104




Example 97




680




30







Example 105




Example 98




660




30







Example 106




Example 99




710




20







Comparative




Comparative




680




30







Example 47




Example 42







Comparative




Comparative




680




30







Example 48




Example 44







Comparative




Comparative




450




30







Example 49




Example 45







Comparative




Comparative




850




30







Example 50




Example 46







Comparative




Comparative




670




30







Example 51




Example 46

























TABLE 23













Properties of high-density acicular hematite particles

















Geometrical





Geometrical







Average




standard




Average




standard






Examples




major




deviation of




minor




deviation of






and




axial




major axial




axial




minor axial






Comparative




diameter




diameter




diameter




diameter






Examples




(μm)




(−)




(μm)




(−)









Example 100




0.138




1.35




0.0193




1.38






Example 101




0.151




1.36




0.0198




1.39






Example 102




0.195




1.31




0.0245




1.37






Example 103




0.213




1.34




0.0253




1.42






Example 104




0.168




1.34




0.0196




1.38






Example 105




0.120




1.35




0.0170




1.38






Example 106




0.230




1.34




0.0287




1.38






Comparative




0.068




1.86




0.0333




1.65






Example 47






Comparative




0.128




1.65




0.0226




1.38






Example 48






Comparative




0.142




1.37




0.0193




1.38






Example 49






Comparative




0.110




1.68




0.0260




1.39






Example 50






Comparative




0.234




1.44




0.0295




1.39






Example 51















Examples




Properties of high-density acicular hematite particles
















and




Aspect




Content






S


BET


/S


TEM








Comparative




ratio




of Al




S


BET






S


TEM






value






Examples




(−)




(wt %)




(m


2


/g)




(m


2


/g)




(−)









Example 100




7.2:1




1.23




51.4




42.6




1.21






Example 101




7.6:1




1.82




52.6




41.4




1.27






Example 102




8.0:1




0.90




43.1




33.4




1.29






Example 103




8.4:1




3.91




41.2




32.2




1.28






Example 104




8.6:1




1.83




55.2




41.5




1.33






Example 105




7.1:1




2.35




56.1




48.5




1.16






Example 106




8.0:1




0.51




41.0




28.5




1.44






Comparative




2.0:1




1.24




13.8




28.8




0.48






Example 47






Comparative




5.7:1




1.23




25.6




37.0




0.69






Example 48






Comparative




7.4:1




1.23




100.8




42.6




2.37






Example 49






Comparative




4.2:1









26.8




33.1




0.81






Example 50






Comparative




7.9:1









42.5




27.7




1.53






Example 51
















Properties of high-density acicular hematite particles


















Soluble










Amount of




sodium




Soluble







sintering




salt




sulfate







preventive




(calcu-




(calcu-





Resin

















Ex.




Calcu-





lated




lated




pH




adsorp-






and




lated




Content




as Na)




as SO


4


)




value




tion






Com. Ex.




as




(wt %)




(ppm)




(ppm)




(−)




(%)









Ex. 100




SiO


2






0.55




2,516




2,788




5.3











Ex. 101




SiO


2






1.07




3,009




3,072




5.2












P




1.06






Ex. 102




P




1.66




2,641




2,904




5.3











Ex. 103




P




2.25




2,038




3,456




5.0











Ex. 104




SiO


2






3.29




1,515




2,622




6.2











Ex. 105




P




1.68




2,463




3,291




4.9











Ex. 106




SiO


2






2.23




3,652




2,543




4.8












P




1.10






Com. Ex.














2,588




2,862




5.3




21.8






47






Com. Ex.




P




1.66




2,832




2,904




5.3




36.8






48






Com. Ex.




P




1.09




2,613




3,008




5.4




51.3






49






Com. Ex.




SiO


2






1.10




1,582




2,936




5.3




36.8






50






Com. Ex.




SiO


2






1.10




1,654




2,890




5.8




37.8






51



























TABLE 24














Kind of high-










density







Examples and




acicular




Wet-pulverization
















Comparative




hematite




Use or




Residue on







Examples




particles




non-use




sieve (wt %)











Example 107




Example 100




used




0







Example 108




Example 101




used




0







Example 109




Example 102




used




0







Example 110




Example 103




used




0







Example 111




Example 104




used




0







Example 112




Example 105




used




0







Example 113




Example 106




used




0







Comparative




Particles used




used




0







Example 52




in Example 5







Comparative




Comparative




used




0







Example 53




Example 51
















Examples




Acid-dissolving treatment
















and





Concen-




Tempera-





pH






Comparative




Kind of




tration




ture




Time




value






Examples




acid




(N)




(° C.)




(Hr)




(−)









Example 107




Sulfuric




1.5




85




5.0




0.55







acid






Example 108




Sulfuric




1.4




90




6.0




0.61







acid






Example 109




Sulfuric




1.8




85




7.0




0.48







acid






Example 110




Sulfuric




1.6




75




5.0




0.50







acid






Example 111




Sulfuric




1.3




75




2.5




0.71







acid






Example 112




Sulfuric




1.5




80




2.0




0.68







acid






Example 113




Sulfuric




2.0




90




7.0




0.36







acid






Comparative




Sulfuric




3.0E−05




80




5.5




4.7






Example 52




acid






Comparative




Sulfuric




4.0E−04




80




8.0




3.4






Example 53




acid
























TABLE 25













Properties of acicular hematite particles







washed with water after acid-dissolving treatment

















Geometrical





Geometrical







Average




standard




Average




standard






Examples




major




deviation of




minor




deviation of






and




axial




major axial




axial




minor axial






Comparative




diameter




diameter




diameter




diameter






Examples




(μm)




(−)




(μm)




(−)









Example 107




0.132




1.34




0.0187




1.33






Example 108




0.142




1.35




0.0179




1.34






Example 109




0.173




1.31




0.0218




1.33






Example 110




0.195




1.33




0.0231




1.34






Example 111




0.163




1.33




0.0195




1.32






Example 112




0.121




1.35




0.0165




1.32






Example 113




0.195




1.33




0.0227




1.33






Comparative




0.138




1.35




0.0194




1.38






Example 52






Comparative




0.234




1.44




0.0296




1.39






Example 53


















Properties of acicular hematite particles







Examples




washed with water after acid-dissolving treatment
















and





Amount








Comparative




Aspect ratio




dissolved




Content of Al







Examples




(−)




(wt %)




(wt %)











Example 107




7.1:1




25.8




1.22







Example 108




7.9:1




31.2




1.83







Example 109




7.9:1




39.8




0.91







Example 110




8.4:1




21.3




3.92







Example 111




8.4:1




11.6




1.85







Example 112




7.3:1




18.2




2.36







Example 113




8.6:1




42.8




0.52







Comparative




7.1:1




0.3




1.23







Example 52







Comparative




7.9:1




1.0












Example 53

















Properties of acicular hematite particles






Examples




washed with water after acid-dissolving treatment














and






S


BET


/S


TEM








Comparative




S


BET






S


TEM






value






Examples




(m


2


/g)




(m


2


/g)




(−)









Example 107




56.1




44.0




1.27






Example 108




57.6




45.7




1.26






Example 109




48.2




37.5




1.29






Example 110




45.6




35.3




1.29






Example 111




58.1




41.8




1.39






Example 112




61.2




49.8




1.23






Example 113




47.1




35.9




1.31






Comparative




50.8




42.4




1.20






Example 52






Comparative




40.6




27.6




1.47






Example 53
















Properties of acicular hematite particles washed







with water after acid-dissolving treatment


















Soluble










Amount of




sodium




Soluble







sintering




salt




sulfate







preventive




(calcu-




(calcu-





Resin


















Calcu-





lated




lated as




pH




adsorp-






Ex. and




lated




Content




as Na)




SO


4


)




value




tion






Com. Ex.




as




(wt %)




(ppm)




(ppm)




(−)




(%)









Ex. 107




SiO


2






0.54




118




343




5.0




68.6






Ex. 108




SiO


2






1.07




141




410




5.2




68.3







P




1.05






Ex. 109




P




1.67




124




368




5.1




66.8






Ex. 110




P




2.26




89




532




4.9




67.1






Ex. 111




SiO


2






3.30




72




295




5.3




71.2






Ex. 112




P




1.68




103




491




5.1




70.6






Ex. 113




SiO


2






2.24




152




206




5.0




66.9







P




1.11






Com. Ex.




SiO


2






0.58




107




314




5.3




61.2






52






Com. Ex.




SiO


2






1.11




96




357




5.2




54.3






53
























TABLE 26












Kind of high-







Examples




density




Heat-treatment in aqueous






and




acicular




alkali solution















Reference




hematite




pH value




Temperature




Time






Examples




particles




(−)




(° C.)




(min)









Example




Example 107




13.6




90




180






114






Example




Example 108




13.5




95




180






115






Example




Example 109




13.2




85




240






116






Example




Example 110




13.4




85




180






117






Example




Example 111




13.5




80




300






118






Example




Example 112




13.3




95




120






119






Example




Example 113




13.2




90




240






120






Reference




Example 107




 9.3




90




180






Example 30






Reference




Example 107




13.1




43




180






Example 31
























TABLE 27













Properties of acicular hematite particles







washed with water after heat-treatment in







aqueous alkali solution

















Geometrical





Geometrical







Average




standard




Average




standard






Examples




major




deviation of




minor




deviation of






and




axial




major axial




axial




minor axial






Reference




diameter




diameter




diameter




diameter






Examples




(μm)




(−)




(μm)




(−)









Example 114




0.132




1.34




0.0188




1.33






Example 115




0.142




1.33




0.0179




1.34






Example 116




0.173




1.31




0.0217




1.32






Example 117




0.195




1.31




0.0231




1.34






Example 118




0.163




1.38




0.0195




1.31






Example 119




0.121




1.35




0.0166




1.32






Example 120




0.195




1.32




0.0227




1.33






Reference




0.132




1.34




0.0188




1.38






Example 30






Reference




0.132




1.34




0.0188




1.39






Example 31
















Properties of acicular hematite particles







washed with water after heat-treatment in







aqueous alkali solution
















Examples











and




Aspect




Content






S


BET


/S


TEM








Reference




ratio




of Al




S


BET






S


TEM






value






Examples




(−)




(wt %)




(m


2


/g)




(m


2


/g)




(−)









Example 114




7.0:1




1.22




57.0




43.8




1.30






Example 115




7.9:1




1.83




57.3




45.7




1.25






Example 116




8.0:1




0.91




49.6




37.7




1.32






Example 117




8.4:1




3.92




46.3




35.3




1.31






Example 118




8.4:1




1.85




59.6




41.8




1.43






Example 119




7.3:1




2.36




62.0




49.5




1.25






Example 120




8.6:1




0.52




47.1




35.9




1.31






Reference




7.0:1




1.22




57.1




43.8




1.30






Example 30






Reference




7.0:1




1.22




57.3




43.8




1.31






Example 31
















Properties of acicular hematite particles washed







with water after heat-treatment in aqueous alkali







solution


















Soluble










Amount of




sodium




Soluble









sintering




salt




sulfate









preventive




(calcu-




(calcula





Resin


















Calcu-





lated




ted as




pH




adsorp-






Ex. and




lated




Content




as Na)




SO


4


)




value




tion






Com. Ex.




as




(wt %)




(ppm)




(ppm)




(−)




(%)









Ex. 114




SiO


2






0.44




96




7




9.2




70.8






Ex. 115




SiO


2






0.77




101




10




9.1




71.6







P




0.32






Ex. 116




P




0.48




72




6




9.1




72.1






Ex. 117




P




0.61




56




21




8.9




73.2






Ex. 118




SiO


2






2.25




52




6




8.9




74.1






Ex. 119




P




0.50




92




16




9.3




74.2






Ex. 120




SiO


2






1.68




110




3




9.6




70.6







P




0.34






Ref. Ex.




SiO


2






0.43




136




293




7.3




66.4






30






Ref. Ex.




SiO


2






0.44




156




216




7.7




65.8






31

























TABLE 28













Kind of acicular




Surface treatment















hematite





Amount







particles




Kind of




added







treated in




surface




(calculated







aqueous alkaline




treatment




as Al or






Examples




solution




material




SiO


2


) (wt %)









Example 121




Example 114




Sodium aluminate




1.0






Example 122




Example 115




Water glass #3




1.0






Example 123




Example 116




Aluminum sulfate




1.5








Water glass #3




0.5






Example 124




Example 117




Aluminum acetate




4.0






Example 125




Example 118




Sodium aluminate




2.0








Colloidal silica




0.5






Example 126




Example 119




Colloidal silica




2.0






Example 127




Example 120




Sodium aluminate




15.0
















Coating material



















Coating amount










(calculated as Al







Examples




Kind*


1






Calculated as




or SiO


2


) (wt %)











Example 121




A




Al




0.99







Example 122




S




SiO


2






0.98







Example 123




A




Al




1.47








S




SiO


2






0.49







Example 124




A




Al




3.85







Example 125




A




Al




1.96








S




SiO


2






0.49







Example 126




S




SiO


2






1.96







Example 127




A




Al




13.00













Note *


1


: “A” represents a hydroxide of aluminum.











“S” represents an oxide of silicon.























TABLE 29













Properties of acicular hematite particles







washed with water after surface-treatment

















Geometrical





Geometrical







Average




standard




Average




standard







major




deviation of




minor




deviation of







axial




major axial




axial




minor axial







diameter




diameter




diameter




diameter






Examples




(μm)




(−)




(μm)




(−)









Example 121




0.131




1.34




0.0188




1.33






Example 122




0.142




1.35




0.0179




1.34






Example 123




0.173




1.31




0.0217




1.32






Example 124




0.195




1.33




0.0232




1.34






Example 125




0.163




1.33




0.0195




1.31






Example 126




0.121




1.35




0.0166




1.32






Example 127




0.195




1.33




0.0227




1.33
















Properties of acicular hematite particles







washed with water after surface-treatment

















Aspect




Content






S


BET


/S


TEM









ratio




of Al*


2






S


BET






S


TEM






value






Examples




(−)




(wt %)




(m


2


/g)




(m


2


/g)




(−)









Example 121




7.0:1




1.22




57.3




43.9




1.31






Example 122




7.9:1




1.83




58.1




45.7




1.27






Example 123




8.0:1




0.91




48.9




37.7




1.30






Example 124




8.4:1




3.92




46.9




35.1




1.34






Example 125




8.4:1




1.85




61.2




41.8




1.46






Example 126




7.3:1




2.36




63.6




49.5




1.28






Example 127




8.6:1




0.52




47.4




35.9




1.32
















Properties of acicular hematite particles washed







with water after surface-treatment


















Soluble










Amount of




sodium




Soluble









sintering




salt




sulfate









preventive




(calcu-




(Calcula





Resin


















Calcu-





lated




ted as




pH




adsorp







lated




Content




as Na)




SO


4


)




value




-tion






Examples




as




(wt %)




(ppm)




(ppm)




(−)




(%)









Example




SiO


2






0.44




91




1




9.4




78.2






121






Example




SiO


2






0.77




78




5




9.2




81.2






122




P




0.32






Example




P




0.48




63




6




9.1




83.6






123






Example




P




0.61




71




2




9.0




84.1






124






Example




SiO


2






2.25




58




8




8.9




80.6






125






Example




P




0.50




62




3




9.0




79.8






126






Example




SiO


2






1.68




65




1




9.2




81.6






127




P




0.34











Note*


2


: Al content excluding amount of Al in surface-coating layer.
























TABLE 30













Production of non-magnetic








coating composition




Non-magnetic















Kind of




Weight ratio




coating







acicular




of particles




composition







hematite




to resin




Viscosity






Examples




particles




(−)




(cP)









Example 128




Example 114




5.0




333






Example 129




Example 115




5.0




358






Example 130




Example 116




5.0




333






Example 131




Example 117




5.0




284






Example 132




Example 118




5.0




230






Example 133




Example 119




5.0




410






Example 134




Example 120




5.0




384






Example 135




Example 121




5.0




333






Example 136




Example 122




5.0




284






Example 137




Example 123




5.0




333






Example 138




Example 124




5.0




207






Example 139




Example 125




5.0




230






Example 140




Example 126




5.0




284






Example 141




Example 127




5.0




207

















Properties of non-magnetic undercoat layer



















Surface




Young's









roughness




modulus







Thickness




Gloss




Ra




(relative






Examples




(μm)




(%)




(nm)




value)









Example 128




3.5




212




6.2




123






Example 129




3.4




201




6.4




123






Example 130




3.4




205




6.4




128






Example 131




3.5




203




6.4




130






Example 132




3.4




218




5.4




128






Example 133




3.3




220




5.8




125






Example 134




3.4




216




5.7




134






Example 135




3.5




213




5.8




127






Example 136




3.5




210




6.0




127






Example 137




3.5




213




6.1




130






Example 138




3.5




216




5.8




136






Example 139




3.4




223




5.0




129






Example 140




3.3




221




5.6




125






Example 141




3.5




220




5.0




136


























TABLE 31














Production of non-magnetic








Comparative




coating composition




Non-magnetic
















Examples




Kind of




Weight ratio




coating







and




acicular




of particles




composition







Reference




hematite




to resin




Viscosity







Examples




particles




(−)




(cP)











Comparative




Comparative




5.0




7,680







Example 54




Example 41







Comparative




Comparative




5.0




10,240







Example 55




Example 43







Comparative




Comparative




5.0




384







Example 56




Example 47







Comparative




Comparative




5.0




640







Example 57




Example 48







Comparative




Comparative




5.0




5,632







Example 58




Example 49







Comparative




Comparative




5.0




230







Example 59




Example 50







Comparative




Comparative




5.0




410







Example 60




Example 51







Comparative




Comparative




5.0




384







Example 61




Example 52







Comparative




Comparative




5.0




435







Example 62




Example 53







Reference




Example 107




5.0




384







Example 32







Reference




Example 108




5.0




410







Example 33







Reference




Example 109




5.0




410







Example 34







Reference




Example 110




5.0




281







Example 35







Reference




Example 111




5.0




281







Example 36







Reference




Example 112




5.0




410







Example 37







Reference




Example 113




5.0




384







Example 38







Reference




Reference




5.0




384







Example 39




Example 30







Reference




Reference




5.0




320







Example 40




Example 31



















Comparative




Properties of nonmagnetic undercoat layer


















Examples






Surface




Young's







and






roughness




modulus







Reference




Thickness




Gloss




Ra




(relative







Examples




(μm)




(%)




(nm)




value)











Comparative




3.5




126




20.6




106







Example 54







Comparative




3.7




88




38.9




99







Example 55







Comparative




3.5




142




20.2




110







Example 56







Comparative




3.5




173




12.3




111







Example 57







Comparative




3.6




126




26.5




106







Example 58







Comparative




3.5




160




18.2




106







Example 59







Comparative




3.5




183




9.9




114







Example 60







Comparative




3.5




189




9.2




116







Example 61







Comparative




3.5




175




13.6




116







Example 62







Reference




3.5




200




7.2




123







Example 32







Reference




3.4




195




7.6




121







Example 33







Reference




3.5




198




6.8




120







Example 34







Reference




3.4




196




7.4




132







Example 35







Reference




3.5




211




6.4




126







Example 36







Reference




3.5




211




6.0




124







Example 37







Reference




3.4




211




6.3




131







Example 38







Reference




3.5




210




6.8




121







Example 39







Reference




3.4




206




6.8




124







Example 40

























TABLE 32













Production of magnetic recording medium



















Weight










ratio of








Kind of non-





particles








magnetic




Kind of magnetic




to resin







Examples




substrate




particles




(−)











Example 142




Example 128




Particles used in




5.0









Example 7







Example 143




Example 129




Magnetic metal




5.0









particles (a)







Example 144




Example 130




Magnetic metal




5.0









particles (a)







Example 145




Example 131




Magnetic metal




5.0









particles (b)







Example 146




Example 132




Magnetic metal




5.0









particles (b)







Example 147




Example 133




Magnetic metal




5.0









particles (c)







Example 148




Example 134




Magnetic metal




5.0









particles (c)







Example 149




Example 135




Particles used in




5.0









Example 7







Example 150




Example 136




Magnetic metal




5.0









particles (a)







Example 151




Example 137




Magnetic metal




5.0









particles (a)







Example 152




Example 138




Magnetic metal




5.0









particles (b)







Example 153




Example 139




Magnetic metal




5.0









particles (b)







Example 154




Example 140




Magnetic metal




5.0









particles (c)







Example 155




Example 141




Magnetic metal




5.0









particles (c)


















Properties of magnetic recording medium

















Thickness










of










magnetic




Coercive




Br/Bm








layer




force (Hc)




value




Gloss






Examples




(μm)




(Oe)




(−)




(%)









Example 142




1.0




1,979




0.87




230






Example 143




1.0




1,984




0.87




226






Example 144




1.0




1,990




0.88




226






Example 145




1.0




2,005




0.87




220






Example 146




1.0




1,994




0.87




243






Example 147




1.1




2,141




0.88




245






Example 148




1.1




2,146




0.88




238






Example 149




1.1




1,981




0.88




231






Example 150




1.0




1,994




0.88




236






Example 151




1.0




1,980




0.89




230






Example 152




1.1




2,001




0.90




237






Example 153




1.0




2,010




0.89




245






Example 154




1.0




2,141




0.90




241






Example 155




1.0




2,138




0.90




243
















Properties of magnetic recording medium


















Linear










absorp-








Surface




Young's




tion




Durability

















rough-




modulus




coeffi-




Running








ness Ra




(relative




cient




time




Scratch






Examples




(nm)




value)




(μm


−1


)




(min)




resistance









Example 142




5.8




127




1.22




29.6




A






Example 143




6.4




129




1.24




24.8




B






Example 144




6.2




128




1.26




24.8




B






Example 145




6.4




131




1.28




27.7




A






Example 146




6.0




132




1.27




28.9




A






Example 147




5.8




131




1.24




≧30




A






Example 148




6.1




132




1.25




≧30




A






Example 149




5.8




128




1.25




≧30




A






Example 150




5.5




132




1.25




≧30




A






Example 151




6.1




133




1.26




≧30




A






Example 152




6.0




136




1.28




≧30




A






Example 153




5.3




137




1.26




≧30




A






Example 154




5.8




135




1.25




≧30




A






Example 155




5.9




133




1.25




≧30




A

















Properties of magnetic recording medium








Corrosion resistance















Percentage of change




Percentage of change






Examples




in coercive force (%)




in B


m


(%)









Example 142




3.1




2.8






Example 143




4.2




4.6






Example 144




4.6




3.1






Example 145




2.6




2.1






Example 146




3.5




1.8






Example 147




3.2




3.4






Example 148




3.4




3.8






Example 149




3.4




2.6






Example 150




4.1




1.6






Example 151




4.6




4.1






Example 152




1.8




3.8






Example 153




0.8




0.6






Example 154




2.6




2.8






Example 155




2.6




1.6

























TABLE 33













Production of magnetic recording medium

















Comparative






Weight







Examples






ratio of







and




Kind of non-





particles







Reference




magnetic




Kind of magnetic




to resin







Examples




substrate




particles




(−)











Comparative




Comparative




Magnetic metal




5.0







Example 63




Example 54




particles (a)







Comparative




Comparative




Magnetic metal




5.0







Example 64




Example 55




particles (a)







Comparative




Comparative




Magnetic metal




5.0







Example 65




Example 56




particles (a)







Comparative




Comparative




Magnetic metal




5.0







Example 66




Example 57




particles (a)







Comparative




Comparative




Magnetic metal




5.0







Example 67




Example 58




particles (a)







Comparative




Comparative




Magnetic metal




5.0







Example 68




Example 59




particles (d)







Comparative




Comparative




Magnetic metal




5.0







Example 69




Example 60




particles (d)







Comparative




Comparative




Magnetic metal




5.0







Example 70




Example 61




particles (d)







Comparative




Comparative




Magnetic metal




5.0







Example 71




Example 62




particles (d)







Reference




Reference




Magnetic metal




5.0







Example 41




Example 32




particles (a)







Reference




Reference




Magnetic metal




5.0







Example 42




Example 33




particles (a)







Reference




Reference




Magnetic metal




5.0







Example 43




Example 34




particles (a)







Reference




Reference




Magnetic metal




5.0







Example 44




Example 35




particles (a)







Reference




Reference




Magnetic metal




5.0







Example 45




Example 36




particles (a)







Reference




Reference




Magnetic metal




5.0







Example 46




Example 37




particles (d)







Reference




Reference




Magnetic metal




5.0







Example 47




Example 38




particles (d)







Reference




Reference




Magnetic metal




5.0







Example 48




Example 39




particles (d)







Reference




Reference




Magnetic metal




5.0







Example 49




Example 40




particles (d)














Properties of magnetic recording medium


















Comparative




Thickness










Examples




of










and




magnetic




Coercive




Br/Bm








Reference




layer




force (Hc)




value




Gloss







Examples




(μm)




(Oe)




(−)




(%)











Comparative




1.2




1,957




0.78




135







Example 63







Comparative




1.3




1,961




0.76




118







Example 64







Comparative




1.1




1,968




0.82




173







Example 65







Comparative




1.1




1,963




0.84




182







Example 66







Comparative




1.2




1,954




0.78




161







Example 67







Comparative




1.1




1,863




0.84




178







Example 68







Comparative




1.0




1,871




0.85




190







Example 69







Comparative




1.1




1,878




0.85




189







Example 70







Comparative




1.0




1,876




0.83




182







Example 71







Reference




1.1




1,986




0.87




217







Example 41







Reference




1.1




1,991




0.87




214







Example 42







Reference




1.1




1,984




0.87




212







Example 43







Reference




1.1




1,989




0.87




210







Example 44







Reference




1.1




1,986




0.87




213







Example 45







Reference




1.2




1,909




0.88




218







Example 46







Reference




1.1




1,910




0.88




220







Example 47







Reference




1.1




1,891




0.88




216







Example 48







Reference




1.1




1,900




0.88




220







Example 49

















Properties of magnetic recording medium


















Linear







Comparative






absorp-







Examples




Surface




Young's




tion




Durability
















and




rough-




modulus




coeffi-




Running







Reference




ness Ra




(relative




cient




time




Scratch






Examples




(nm)




value)




(μm


−1


)




(min)




resistance









Comparative




24.3




113




1.04




8.3




D






Example 63






Comparative




38.5




96




1.09




1.6




D






Example 64






Comparative




19.8




112




1.16




9.2




D






Example 65






Comparative




12.6




113




1.14




14.5




C






Example 66






Comparative




21.9




110




1.06




12.6




C






Example 67






Comparative




12.5




113




1.09




13.6




C






Example 68






Comparative




10.7




116




1.15




11.8




D






Example 69






Comparative




11.0




119




1.17




12.3




C






Example 70






Comparative




13.1




119




1.13




13.6




C






Example 71






Reference




6.8




123




1.21




23.8




B






Example 41






Reference




6.8




123




1.22




24.2




B






Example 42






Reference




7.2




128




1.22




24.4




B






Example 43






Reference




7.2




130




1.24




23.4




B






Example 44






Reference




6.8




126




1.25




25.6




A






Example 45






Reference




6.2




125




1.24




22.3




B






Example 46






Reference




6.0




125




1.24




23.9




B






Example 47






Reference




6.2




125




1.25




24.2




B






Example 48






Reference




6.0




125




1.25




24.8




B






Example 49


















Comparative









Examples




Properties of magnetic recording medium








and




Corrosion resistance
















Reference




Percentage of change




Percentage of change







Examples




in coercive force (%)




in B


m


(%)











Comparative




38.2




32.6







Example 63







Comparative




41.2




28.1







Example 64







Comparative




36.5




29.2







Example 65







Comparative




31.3




26.5







Example 66







Comparative




32.1




21.3







Example 67







Comparative




36.5




16.8







Example 68







Comparative




17.9




17.8







Example 69







Comparative




16.5




21.6







Example 70







Comparative




19.8




17.3







Example 71







Reference




11.8




11.6







Example 41







Reference




15.8




16.8







Example 42







Reference




11.6




18.6







Example 43







Reference




10.8




13.2







Example 44







Reference




10.1




10.9







Example 45







Reference




13.2




14.1







Example 46







Reference




11.8




13.1







Example 47







Reference




14.1




12.8







Example 48







Reference




12.0




10.9







Example 49


























TABLE 34













Properties of acicular goethite particles




















Geometrical










standard









Average major




deviation of







Kind of





axial diameter




major axial







Precursor




Shape




(μm)




diameter (−)











Goethite




Spindle-




0.0593




1.56







particles 1




shaped







Goethite




Acicular




0.0932




1.53







particles 2

















Properties of acicular goethite particles


















Geometrical










standard









Average minor




deviation of








Kind of




axial diameter




minor axial




Aspect ratio







Precursor




(μm)




diameter (−)




(−)











Goethite




0.0096




1.37




6.2:1







particles 1







Goethite




0.0126




1.39




7.4:1







particles 2


















Properties of acicular goethite particles


















Soluble




Soluble









sodium salt




sulfate








BET specific




(calculated




(calculated




pH






Kind of




surface area




as Na)




as SO


4


)




value






Precursor




(m


2


/g)




(ppm)




(ppm)




(−)









Goethite




231.3




563




412




5.8






particles 1






Goethite




186.8




1,126




368




7.8






particles 2

























TABLE 35













Properties of acicular goethite








particles subjected to anti-








sintering treatment


















Geometrical








Average major




standard deviation







Kind of




axial




of major axial






Precursor




Precursor




diameter (μm)




diameter (−)









Goethite




Particles




0.0813




1.53






particles 3




obtained in







Example 8






Goethite




Goethite




0.0593




1.56






particles 4




particles 1






Goethite




Goethite




0.0931




1.53






particles 5




particles 2
















Properties of acicular goethite particles







subjected to anti-sintering treatment

















Average




Geometrical









minor axial




standard deviation




Aspect








diameter




of minor axial




ratio







Precursor




(μm)




diameter (−)




(−)











Goethite




0.0110




1.37




7.4:1







particles 3







Goethite




0.0096




1.37




6.2:1







particles 4







Goethite




0.0128




1.39




7.3:1







particles 5

















Properties of acicular goethite particles







subjected to anti-sintering treatment















BET specific









surface area




Sintering preventive

















Precursor




(m


2


/g)




Calculated as




Amount (wt %)











Goethite




190.8




P




1.08







particles 3







Goethite




228.6




P




1.64







particles 4







Goethite




185.2




SiO


2






1.09







particles 5

















Properties of acicular goethite particles







subjected to anti-sintering treatment

















Soluble




Soluble









sodium salt




sulfate









(calculated




(Calculated as









as Na)




SO


4


)




pH value







Precursor




(ppm)




(ppm)




(−)











Goethite




813




412




7.6







particles 3







Goethite




612




515




6.1







particles 4







Goethite




1,326




412




8.0







particles 5

























TABLE 36













Conditions of heat-treatment















Goethite




Kind of





Temperature




Time






particles




Precursor




Atmosphere




(° C.)




(min)









Goethite




Goethite




Air




150




30






particles 6




particles 3






Goethite




Goethite




Air




180




30






particles 7




particles 4






Goethite




Goethite




Air




120




20






particles 8




particles 5






Goethite




Goethite




Air




80




30






particles 9




particles 4
























TABLE 37













Properties of acicular goethite particles







heat-treated

















Geometrical





Geometrical







Average




standard




Average




standard







major




deviation of




minor




deviation of






Kind of




axial




major axial




axial




minor axial






goethite




diameter




diameter




diameter




diameter






particles




(μm)




(−)




(μm)




(−)









Goethite




0.0812




1.38




0.0109




1.16






particles 6






Goethite




0.0591




1.43




0.0098




1.21






particles 7






Goethite




0.0930




1.36




0.0128




1.25






particles 8






Goethite




0.0590




1.53




0.0099




1.37






particles 9

















Properties of acicular goethite particles








heat-treated




















BET











specific




Sintering








Kind of




Aspect




surface




preventive


















goethite




ratio




area




Calculated




Amount







particles




(−)




(m


2


/g)




as




(wt %)











Goethite




7.4:1




191.2




P




1.18







particles 6







Goethite




6.0:1




227.6




P




1.82







particles 7







Goethite




7.3:1




184.8




SiO


2






1.20







particles 8







Goethite




6.0:1




225.1




P




1.80







particles 9

















Properties of acicular goethite particles







heat-treated

















Soluble




Soluble









sodium salt




sulfate








Kind of




(calculated as




(calculated as








goethite




Na)




SO


4


)




pH value







particles




(ppm)




(ppm)




(−)











Goethite




883




446




7.5







particles 6







Goethite




710




532




6.0







particles 7







Goethite




1,410




483




7.9







particles 8







Goethite




681




518




6.1







particles 9

























TABLE 38











Kind of





Conditions of heat-dehydration






particles




Kind of




treatment















to be




goethite





Temperature




Time






treated




particles




Atmosphere




(° C.)




(min)









Hematite




Goethite




Air




320




20






particles 1




particles 6






Hematite




Goethite




Air




340




30






particles 2




particles 7






Hematite




Goethite




Air




350




20






particles 3




particles 8






Hematite




Goethite




Air




340




20






particles 4




particles 4
























TABLE 39













Properties of low-density acicular hematite







particles

















Geometrical





Geometrical







Average




standard




Average




standard






Kind of




major




deviation of




minor




deviation of






particles




axial




major axial




axial




minor axial






to be




diameter




diameter




diameter




diameter






treated




(μm)




(−)




(μm)




(−)









Hematite




0.0731




1.37




0.0113




1.16






particles 1






Hematite




0.0533




1.43




0.0103




1.20






particles 2






Hematite




0.0841




1.36




0.0131




1.25






particles 3






Hematite




0.0531




1.56




0.0104




1.37






particles 4

















Properties of low-density acicular hematite








particles


















Kind of




Aspect






S


BET


/S


TEM









particles




ratio




S


BET






S


TEM






value







to be treated




(−)




(m


2


/g)




(m


2


/g)




(−)











Hematite




6.5:1




226.5




73.3




3.09







particles 1







Hematite




5.2:1




263.8




81.9




3.22







particles 2







Hematite




6.4:1




216.8




63.3




3.43







particles 3







Hematite




5.1:1




226.6




81.2




2.79







particles 4

















Properties of low-density acicular hematite







particles

















Soluble










sodium




Soluble









salt




sulfate







Kind of




Sintering




(calcu-




(calcu-







particles




preventive




lated as




lated as




pH
















to be




Calcu-




Amount




Na)




SO


4


)




value






treated




lated as




(wt %)




(ppm)




(ppm)




(−)









Hematite




P




1.18




1,625




913




7.4






particles 1






Hematite




P




1.81




1,321




615




6.0






particles 2






Hematite




SiO


2






1.20




1,821




516




7.6






particles 3






Hematite




P




1.79




1,326




712




6.3






particles 4
























TABLE 40











Kind of




Kind of




Conditions of high-temperature






particles




particles




heat-treatment















to be




to be





Temperature




Time






treated




treated




Atmosphere




(° C.)




(min)









Hematite




Hematite




Air




680




30






particles 5




particles 1






Hematite




Hematite




Air




630




40






particles 6




particles 2






Hematite




Hematite




Air




600




40






particles 7




particles 3






Hematite




Goethite




Air




650




20






particles 8




particles 7






Hematite




Goethite




Air




700




30






particles 9




particles 1






Hematite




Goethite




Air




630




30






particles 10




particles 9






Hematite




Hematite




Air




680




30






particles 11




particles 4






Hematite




Hematite




Air




450




30






particles 12




particles 3






Hematite




Hematite




Air




900




30






particles 13




particles 3
























TABLE 41













Properties of high-density acicular hematite







particles

















Geometrical





Geometrical







Average




standard




Average




standard






Kind of




major




deviation of




minor




deviation of






particles




axial




major axial




axial




minor axial






to be




diameter




diameter




diameter




diameter






treated




(μm)




(−)




(μm)




(−)









Hematite




0.0730




1.37




0.0114




1.16






particles 5






Hematite




0.0531




1.43




0.0103




1.20






particles 6






Hematite




0.0840




1.36




0.0130




1.25






particles 7






Hematite




0.0583




1.40




0.0108




1.27






particles 8






Hematite




0.0432




1.61




0.0156




1.39






particles 9






Hematite




0.0456




1.59




0.0152




1.39






particles 10






Hematite




0.0528




1.56




0.0107




1.37






particles 11






Hematite




0.0841




1.35




0.0132




1.28






particles 12






Hematite




0.0613




1.59




0.0232




1.38






particles 13



















Properties of high-density acicular hematite








Kind of




particles


















particles




Aspect






S


BET


/S


TEM









to be




ratio




S


BET






S


TEM






value







treated




(−)




(m


2


/g)




(m


2


/g)




(−)











Hematite




6.4:1




81.2




72.7




1.12







particles 5







Hematite




5.2:1




91.6




81.9




1.12







particles 6







Hematite




6.5:1




71.6




63.8




1.12







particles 7







Hematite




5.4:1




84.6




77.8




1.09







particles 8







Hematite




2.8:1




58.2




58.2




1.00







particles 9







Hematite




3.0:1




72.3




59.0




1.22







particles 10







Hematite




4.9:1




65.6




79.2




0.83







particles 11







Hematite




6.4:1




186.2




62.8




2.96







particles 12







Hematite




2.6:1




36.8




39.4




0.93







particles 13

















Properties of high-density acicular hematite







particles

















Soluble










sodium




Soluble









salt




sulfate







Kind of




Sintering




(calcu-




(calcu-







particles




preventive




lated as




lated




pH
















to be




Calcu-




Amount




Na)




as SO


4


)




value






treated




lated as




(wt %)




(ppm)




(ppm)




(−)









Hematite




P




1.18




2,863




2,162




6.9






particles 5






Hematite




P




1.81




2,068




1,865




5.9






particles 6






Hematite




SiO


2






1.20




2,365




3,100




6.0






particles 7






Hematite




P




1.82




1,563




2,016




5.6






particles 8






Hematite




P




1.79




2,880




2,266




6.8






particles 9






Hematite




P




1.81




1,865




1,265




5.8






particles 10






Hematite




P




1.79




2,653




2,565




5.9






particles 11






Hematite




SiO


2






1.20




1,865




2,O11




5.6






particles 12






Hematite




SiO


2






1.21




1,780




2,025




5.6






particles 13
























TABLE 42











Examples





Heat-treatment in aqueous






and




Kind of




alkali solution















Reference




particles to




pH value




Temperature




Time






Examples




be treated




(−)




(° C.)




(min)









Example




Hematite




13.7




85




210






156




particles 5






Example




Hematite




13.4




95




120






157




particles 6






Example




Hematite




13.8




90




240






158




particles 7






Example




Hematite




13.1




98




180






159




particles 8






Reference




Hematite




8.9




80




180






Example 50




particles 5






Reference




Hematite




13.5




40




180






Example 51




particles 5
























TABLE 43













Properties of high-density acicular hematite







particles washed with water after heat-treatment







in aqueous alkali solution
















Average




Geometrical




Average




Geometrical







major




standard




minor




standard






Examples and




axial




deviation of




axial




deviation of






Reference




diameter




major axial




diameter




minor axial






Examples




(μm)




diameter (−)




(μm)




diameter (−)









Example 156




0.0731




1.36




0.0114




1.16






Example 157




0.0532




1.42




0.0102




1.21






Example 158




0.0840




1.36




0.0129




1.26






Example 159




0.0583




1.39




0.0108




1.27






Reference




0.0730




1.37




0.0114




1.17






Example 50






Reference




0.0730




1.37




0.0114




1.17






Example 51
















Properties of high-density acicular hematite







particles washed with water after heat-treatment







in aqueous alkali solution

















Examples and




Aspect






S


BET


/S


TEM









Reference




ratio




S


BET






S


TEM






value







Examples




(−)




(m


2


/g)




(m


2


/g)




(−)











Example 156




6.4:1




81.2




72.7




1.13







Example 157




5.2:1




92.6




82.6




1.12







Example 158




6.5:1




72.1




64.2




1.12







Example 159




5.4:1




84.8




77.8




1.09







Reference




6.4:1




82.6




72.7




1.14







Example 50







Reference




6.4:1




81.9




72.7




1.13







Example 51

















Properties of high-density acicular hematite







particles washed with water after heat-







treatment in aqueous alkali solution

















Soluble










sodium




Soluble









salt




sulfate








Sintering




(calcu-




(calcula







Examples and




preventive




lated as




ted as




pH
















Reference




Calcu-




Amount




Na)




SO


4


)




value






Examples




lated as




(wt %)




(ppm)




(ppm)




(−)









Example 156




P




0.56




86




12




9.1






Example 157




P




0.93




73




6




9.2






Example 158




SiO


2






1.16




125




38




9.3






Example 159




P




0.91




113




21




9.3






Reference




P




1.18




436




216




7.6






Example 50






Reference




P




1.18




365




182




7.7






Example 51
























TABLE 44












Kind of








particles to be




Concentration of water






Examples




treated




suspension (g/liter)









Example




Example




45






160




156






Example




Example




45






161




157






Example




Example




45






162




158






Example




Example




45






163




159
















Coating treatment with aluminum compound or







silicon compound














Aluminum compound or silicon








compound



















Amount added








pH value





(calculated




Final







before





as Al or




pH







addition




Kind of




SiO


2


)




value






Examples




(−)




additives




(wt %)




(−)









Example




4.0




Aluminum acetate




3.0




7.1






160






Example




10.0




Water glass #3




1.0




6.9






161






Example




10.3




Sodium aluminate




5.0




7.5






162






Example




10.2




Sodium aluminate




2.0




7.0






163





Water glass #3




0.5
























TABLE 45













Properties of acicular hematite particles after







surface-coating treatment

















Geometrical





Geometrical







Average




standard




Average




standard







major




deviation of




minor




deviation of







axial




major axial




axial




minor axial







diameter




diameter




diameter




diameter






Examples




(μm)




(−)




(μm)




(−)









Example




0.0731




1.36




0.0114




1.17






160






Example




0.0531




1.42




0.0102




1.20






161






Example




0.0840




1.36




0.0129




1.26






162






Example




0.0582




1.39




0.0108




1.27






163
















Properties of acicular hematite particles







after surface-coating treatment
















Aspect






S


BET


/S


TEM









ratio




S


BET






S


TEM






value






Examples




(−)




(m


2


/g)




(m


2


/g)




(−)









Example




6.4:1




83.1




72.7




1.14






160






Example




5.2:1




92.8




82.7




1.12






161






Example




6.5:1




74.1




64.2




1.15






162






Example




5.4:1




86.0




77.8




1.10






163
















Properties of acicular hematite particles after







surface-coating treatment

















Surface-









coating








Surface-coating




amount of








amount of




oxide of







Sintering




hydroxide of




silicon







preventive




aluminum




(calculated
















Calcu-




Amount




(calculated as




as






Examples




lated as




(wt %)




Al) (wt %)




SiO


2


) (wt %)









Example




P




0.54




2.93











160






Example




P




0.92









0.99






161






Example




SiO


2






1.08




4.72











162






Example




P




0.89




1.95




0.50






163
















Properties of acicular hematite particles







after surface-coating treatment

















Soluble sodium










salt




Soluble sulfate









(calculated as




(calculated as









Na)




SO


4


)




pH value







Examples




(ppm)




(ppm)




(−)











Example




52




8




9.2







160







Example




61




16




9.1







161







Example




78




23




9.1







162







Example




96




18




9.3







163



























TABLE 46














Production of non-magnetic








Examples,




coating








Comparative




composition




Non-magnetic
















Examples





Weight ratio




coating







and




Kind of non-




of particles




composition







Reference




magnetic




to resin




Viscosity







Examples




particles




(−)




(cP)











Example 164




Example 155




5.0




512







Example 165




Example 156




5.0




435







Example 166




Example 157




5.0




410







Example 167




Example 158




5.0




384







Example 168




Example 159




5.0




307







Example 169




Example 160




5.0




358







Example 170




Example 161




5.0




461







Example 171




Example 162




5.0




384







Comparative




Hematite




5.0




717







Example 72




particles 9







Comparative




Hematite




5.0




614







Example 73




particles 10







Comparative




Hematite




5.0




563







Example 74




particles 11







Comparative




Hematite




5.0




14,410







Example 75




particles 12







Comparative




Hematite




5.0




307







Example 76




particles 13







Reference




Reference




5.0




563







Example 52




Example 50







Reference




Reference




5.0




589







Example 53




Example 51



















Examples,









Comparative




Properties of non-magnetic undercoat layer


















Examples






Surface




Young's







and






roughness




modulus







Reference




Thickness




Gloss




Ra




(relative







Examples




(μm)




(%)




(nm)




value)











Example 164




0.35




215




6.0




136







Example 165




0.35




221




5.6




133







Example 166




0.35




213




6.2




138







Example 167




0.34




206




6.8




133







Example 168




0.35




216




6.1




138







Example 169




0.35




228




5.8




135







Example 170




0.34




215




6.3




139







Example 171




0.36




210




6.5




135







Comparative




0.35




153




21.6




108







Example 72







Comparative




0.36




158




18.9




113







Example 73







Comparative




0.35




168




16.8




119







Example 74







Comparative




0.37




102




32.1




90







Example 75







Comparative




0.34




173




16.2




81







Example 76







Reference




0.35




194




8.6




128







Example 52







Reference




0.35




191




8.8




128







Example 53


























TABLE 47













Production of magnetic recording medium

















Examples,






Weight







Comparative






ratio of







Examples and




Kind of non-





particles







Reference




magnetic




Kind of magnetic




to resin







Examples




substrate




particles




(−)











Example 172




Example 164




Magnetic metal




5.0









particles (d)







Example 173




Example 165




Magnetic metal




5.0









particles (d)







Example 174




Example 168




Magnetic metal




5.0









particles (d)







Example 175




Example 169




Magnetic metal




5.0









particles (d)







Example 176




Example 164




Magnetic metal




5.0









particles (a)







Example 177




Example 165




Magnetic metal




5.0









particles (b)







Example 178




Example 166




Magnetic metal




5.0









particles (c)







Example 179




Example 167




Magnetic metal




5.0









particles (c)







Example 180




Example 168




Magnetic metal




5.0









particles (a)







Example 181




Example 169




Magnetic metal




5.0









particles (b)







Example 182




Example 170




Magnetic metal




5.0









particles (c)







Example 183




Example 171




Magnetic metal




5.0









particles (c)







Comparative




Comparative




Magnetic metal




5.0







Example 77




Example 72




particles (d)







Comparative




Comparative




Magnetic metal




5.0







Example 78




Example 73




particles (d)







Comparative




Comparative




Magnetic metal




5.0







Example 79




Example 74




particles (d)







Comparative




Comparative




Magnetic metal




5.0







Example 80




Example 75




particles (d)







Comparative




Comparative




Magnetic metal




5.0







Example 81




Example 76




particles (d)







Reference




Reference




Magnetic metal




5.0







Example 54




Example 52




particles (d)







Reference




Reference




Magnetic metal




5.0







Example 55




Example 53




particles (d)



















Examples,









Comparative




Properties of magnetic recording medium

















Examples




Thickness










and




of coating




Coercive




Br/Bm







Reference




film




force (Hc)




value




Gloss







Examples




(μm)




(Oe)




(−)




(%)











Example 172




1.0




1,963




0.87




219







Example 173




1.1




1,958




0.87




218







Example 174




1.0




1,968




0.88




223







Example 175




1.0




1,960




0.87




225







Example 176




1.0




1,972




0.88




228







Example 177




1.1




1,996




0.88




224







Example 178




1.0




2,136




0.89




226







Example 179




1.1




2,134




0.89




221







Example 180




1.0




1,986




0.89




233







Example 181




1.0




2,001




0.89




235







Example 182




1.0




2,127




0.90




238







Example 183




1.1




2,130




0.89




221







Comparative




1.2




1,956




0.78




163







Example 77







Comparative




1.2




1,958




0.76




173







Example 78







Comparative




1.1




1,965




0.82




178







Example 79







Comparative




1.1




1,959




0.80




168







Example 80







Comparative




1.1




1,961




0.78




156







Example 81







Reference




1.1




1,976




0.86




213







Example 54







Reference




1.0




1,980




0.86




210







Example 55

















Properties of magnetic recording medium















Examples,






Linear







Comparative






absorp-






Examples




Surface




Young's




tion




Durability
















and




rough-




modulus




coeffi-




Running







Reference




ness Ra




(relative




cient




time




Scratch






Examples




(nm)




value)




(μm


−1


)




(min)




resistance









Example 172




6.2




136




1.28




21.3




B






Example 173




6.2




136




1.27




21.6




B






Example 174




5.9




138




1.30




22.5




A






Example 175




5.8




137




1.31




22.4




A






Example 176




6.1




137




1.28




29.6




A






Example 177




5.7




135




1.27




28.9




A






Example 178




5.7




138




1.31




≧30




A






Example 179




6.2




135




1.29




27.1




B






Example 180




5.7




139




1.29




≧30




A






Example 181




5.6




136




1.32




≧30




A






Example 182




5.5




140




1.27




≧30




A






Example 183




6.1




138




1.26




≧30




A






Comparative




19.8




118




1.01




11.6




D






Example 77






Comparative




14.6




116




1.03




12.6




D






Example 78






Comparative




13.2




115




1.09




14.5




D






Example 79






Comparative




15.1




116




1.11




11.6




D






Example 80






Comparative




18.6




118




1.12




9.6




D






Example 81






Reference




7.4




129




1.18




18.6




C






Example 54






Reference




7.8




129




1.16




19.3




C






Example 55


















Examples,









Comparative







Examples




Properties of magnetic recording medium







and




Corrosion resistance















Reference




Percentage of change




Percentage of change







Examples




in coercive force (%)




in B


m


(%)











Example 172




4.5




4.3







Example 173




3.8




3.6







Example 174




4.0




2.8







Example 175




4.2




3.8







Example 176




4.1




1.6







Example 177




3.6




0.8







Example 178




2.1




0.6







Example 179




1.8




0.9







Example 180




2.6




2.1







Example 181




4.6




1.8







Example 182




1.6




2.1







Example 183




3.1




4.2







Comparative




38.6




26.8







Example 77







Comparative




43.0




26.5







Example 78







Comparative




28.3




32.5







Example 79







Comparative




31.6




28.2







Example 80







Comparative




21.3




19.6







Example 81







Reference




17.8




18.2







Example 54







Reference




16.5




16.8







Example 55


























TABLE 48













Properties of acicular goethite particles




















Geometrical










standard










deviation of









Average major




major axial







Kind of





axial diameter




diameter







Precursor




Shape




(μm)




(−)











Goethite




Spindle-




0.0586




1.53







particles 10




shaped







Goethite




Acicular




0.0893




1.52







particles 11

















Properties of acicular goethite particles


















Geometrical










standard










deviation of









Average minor




minor axial




Aspect







Kind of




axial diameter




diameter




ratio







Precursor




(μm)




(−)




(−)











Goethite




0.0084




1.41




7.0:1







particles 10







Goethite




0.0118




1.42




7.6:1







particles 11

















Properties of acicular goethite particles



















Soluble











sodium




Soluble










salt




sulfate








BET





(calcu-




(calcu-








specific




Content




lated




lated




pH






Kind of




surface




of Al




as Na)




as SO


4


)




value






Precursor




area (m


2


/g)




(wt %)




(ppm)




(ppm)




(−)









Goethite




242.6




2.86




412




381




5.9






particles 10






Goethite




190.6




1.32




832




265




7.6






particles 11

























TABLE 49













Properties of acicular








goethite particles subjected








to anti-sintering treatment




















Geometrical









Average




standard









major axial




deviation of







Kind of




Kind of




diameter




major axial







Precursor




Precursor




(μm)




diameter (−)











Goethite




Goethite




0.0808




1.52







particles 12




particles








used in








Example 12







Goethite




Goethite




0.0586




1.53







particles 13




particles 10







Goethite




Goethite




0.0893




1.52







particles 14




particles 11

















Properties of acicular goethite particles







subjected to anti-sintering treatment


















Geometrical










standard










deviation of









Average minor




minor axial




Aspect







Kind of




axial diameter




diameter




ratio







Precursor




(μm)




(−)




(−)











Goethite




0.0113




1.41




7.2:1







particles 12







Goethite




0.0084




1.41




7.0:1







particles 13







Goethite




0.0118




1.42




7.6:1







particles 14

















Properties of acicular goethite particles







subjected to anti-sintering treatment
















Sintering








BET specific




preventive

















Kind of




surface area




Calculated




Amount







Precursor




(m


2


/g)




as




(wt %)











Goethite




200.6




P




1.16







particles 12







Goethite




240.6




P




1.59







particles 13







Goethite




189.8




SiO


2






1.11







particles 14

















Properties of acicular goethite particles







subjected to anti-sintering treatment

















Soluble




Soluble









sodium salt




sulfate








Content




(calculated




(calculated







Starting




of Al




as Na)




as SO


4


)




pH value






particles




(wt %)




(ppm)




(ppm)




(−)









Goethite




3.36




765




362




7.6






particles 12






Goethite




2.85




532




412




5.8






particles 13






Goethite




1.31




963




282




7.6






particles 14
























TABLE 50











Kind of





Conditions of heat treatment















goethite




Kind of





Temperature




Time






particies




precursor




Atmosphere




(° C.)




(min)









Goethite




Goethite




Air




130




40






particles 15




particles 12






Goethite




Goethite




Air




150




30






particles 16




particles 13






Goethite




Goethite




Air




180




20






particles 17




particles 14






Goethite




Goethite




Air




80




30






particles 18




particles 13
























TABLE 51













Properties of acicular goethite particles







heat-treated

















Geometrical





Geometrical







Average




standard




Average




standard







major




deviation of




minor




deviation of






Kind of




axial




major axial




axial




minor axial






goethite




diameter




diameter




diameter




diameter






particles




(μm)




(−)




(μm)




(−)









Goethite




0.0808




0.37




0.0112




1.26






particles 15






Goethite




0.0586




1.38




0.0084




1.27






particles 16






Goethite




0.0893




1.36




0.0117




1.29






particles 17






Goethite




0.0586




1.52




0.0084




1.41






particles 18

















Properties of acicular goethite particles








heat-treated




















BET











specific




Sintering








Kind of




Aspect




surface




preventive


















goethite




ratio




area




Calculated




Content







particles




(−)




(m


2


/g)




as




(wt %)











Goethite




7.2:1




201.8




P




1.17







particles 15







Goethite




7.0:1




239.4




P




1.59







particles 16







Goethite




7.6:1




190.1




SiO


2






1.12







particles 17







Goethite




7.0:1




239.8




P




1.59







particles 18

















Properties of acicular goethite particles







heat-treated

















Soluble




Soluble









sodium salt




sulfate







Kind of




Content




(calculated




(calculated







goethite




of Al




as Na)




as SO


4


)




pH value






particles




(wt %)




(ppm)




(ppm)




(−)









Goethite




3.36




681




293




7.1






particles 15






Goethite




2.86




543




421




5.9






particles 16






Goethite




1.31




1,128




462




7.6






particles 17






Goethite




2.85




652




413




5.9






particles 18
























TABLE 52











Kind of





Conditions of heat-dehydration






particles




Kind of




treatment















to be




goethite





Temperature




Time






treated




particles




Atmosphere




(° C.)




(min)









Hematite




Goethite




Air




330




30






particles 14




particles 15






Hematite




Goethite




Air




350




30






particles 15




particles 16






Hematite




Goethite




Air




370




25






particles 16




particles 17






Hematite




Goethite




Air




340




30






particles 17




particles 18
























TABLE 53













Properties of low-density acicular hematite







particles

















Geometrical





Geometrical







Average




standard




Average




standard






Kind of




major




deviation of




minor




deviation of






particles




axial




major axial




axial




minor axial






to be




diameter




diameter




diameter




diameter






treated




(μm)




(−)




(μm)




(−)









Hematite




0.0727




1.37




0.0110




1.27






particles 14






Hematite




0.0533




1.38




0.0085




1.27






particles 15






Hematite




0.0822




1.36




0.0116




1.29






particles 16






Hematite




0.0539




1.52




0.0086




1.42






particles 17

















Properties of low-density acicular hematite








particles


















Kind of




Aspect






S


BET


/S


TEM









particles




ratio




S


BET






S


TEM






value







to be treated




(−)




(m


2


/g)




(m


2


/g)




(−)











Hematite




6.6:1




218.6




75.2




2.91







particles 14







Hematite




6.3:1




251.2




97.7




2.57







particles 15







Hematite




7.1:1




209.6




71.0




2.95







particles 16







Hematite




6.3:1




246.8




96.6




2.56







particles 17

















Properties of low-density acicular hematite







particles















Kind of




Sintering








particles




preventive

















to be




Calculated




Amount




Content of Al







treated




as




(wt %)




(wt %)











Hematite




P




1.30




3.73







particles 14







Hematite




P




1.74




3.18







particles 15







Hematite




SiO


2






1.24




1.45







particles 16







Hematite




P




1.75




3.17







particles 17

















Properties of low-density acicular hematite







particles

















Soluble sodium









Kind of




salt




Soluble sulfate








particles




(calculated as




(calculated as








to be




Na)




SO


4


)




pH value







treated




(ppm)




(ppm)




(−)











Hematite




1,321




721




7.2







particles 14







Hematite




1,165




583




5.5







particles 15







Hematite




1,811




412




7.8







particles 16







Hematite




1,011




562




6.1







particles 17

























TABLE 54












Kind of







Kind of




particles




Conditions of heat-treatment















hematite




to be





Temperature




Time






particles




treated




Atmosphere




(° C.)




(min)









Hematite




Hematite




Air




670




20






particles




particles 14






18






Hematite




Hematite




Air




630




30






particles




particles 15






19






Hematite




Hematite




Air




610




40






particles




particles 16






20






Hematite




Goethite




Air




640




30






particles




particles 16






21






Hematite




Goethite




Air




650




30






particles




particles 17






22






Hematite




Goethite




Air




650




30






particles




particles 18






23






Hematite




Hematite




Air




650




30






particles




particles 17






24






Hematite




Hematite




Air




440




30






particles




particles 16






25






Hematite




Hematite




Air




910




30






particles




particles 16






26
























TABLE 55













Properties of high-density acicular hematite particles
















Average




Geometrical




Average




Geometrical







major




standard




minor




standard






Kind of




axial




deviation of




axial




deviation of






hematite




diameter




major axial




diameter




minor axial






particles




(μm)




diameter (−)




(μm)




diameter (−)









Hematite




0.0726




1.37




0.0111




1.28






particles 18






Hematite




0.0532




1.39




0.0086




1.27






particles 19






Hematite




0.0821




1.36




0.0117




1.29






particles 20






Hematite




0.0521




1.38




0.0087




1.29






particles 21






Hematite




0.0412




1.63




0.0150




1.44






particles 22






Hematite




0.0521




1.61




0.0091




1.41






particles 23






Hematite




0.0538




1.53




0.0087




1.42






particles 24






Hematite




0.0822




1.36




0.0116




1.29






particles 25






Hematite




0.0642




1.58




0.0213




1.43






particles 26
















Properties of high-density acicular hematite particles















Kind of




Aspect






S


BET


/S


TEM








hematite




ratio




S


BET






S


TEM






value






particles




(−)




(m


2


/g)




(m


2


/g)




(−)









Hematite




6.5:1




84.6




74.6




1.13






particles 18






Hematite




6.2:1




95.6




96.7




0.99






particles 19






Hematite




7.0:1




73.2




70.4




1.04






particles 20






Hematite




6.0:1




91.8




95.8




0.96






particles 21






Hematite




2.7:1




38.3




60.6




0.63






particles 22






Hematite




5.7:1




63.6




91.9




0.69






particles 23






Hematite




6.2:1




73.8




95.6




0.77






particles 24






Hematite




7.1:1




189.9




71.0




2.67






particles 25






Hematite




3.0:1




39.6




42.1




0.94






particles 26
















Properties of high-density acicular hematite particles













Kind of




Sintering







hematite




preventive




Content of Al














particles




Calculated as




Amount (wt %)




(wt %)









Hematite




P




1.30




3.73






particles 18






Hematite




P




1.75




3.18






particles 19






Hematite




SiO


2






1.24




1.45






particles 20






Hematite




P




1.76




3.18






particles 21






Hematite














3.19






particles 22






Hematite




P




1.76




3.18






particles 23






Hematite




P




1.75




3.17






particles 24






Hematite




SiO


2






1.24




1.45






particles 25






Hematite




SiO


2






1.24




1.46






particles 26
















Properties of high-density acicular hematite particles

















Soluble




Soluble









sodium salt




sulfate






Kind of




Resin




(calculated




(calculated






hematite




adsorp-




as Na)




as SO


4


)




pH value






particles




tion (%)




(ppm)




(ppm)




(−)









Hematite




74.6




2,221




1,652




6.9






particles 18






Hematite




73.2




2,102




1,632




6.3






particles 19






Hematite




71.3




1,821




2,236




5.6






particles 20






Hematite




72.6




1,321




1,821




5.3






particles 21






Hematite




61.6




2,016




1,621




6.3






particles 22






Hematite




67.1




1,211




821




5.9






particles 23






Hematite




68.3




2,182




2,265




5.5






particles 24






Hematite




67.2




1,683




1,821




5.3






particles 25






Hematite




62.1




1,321




1,865




5.7






particles 26
























TABLE 56











Examples





Heat treatment in aqueous






and




Kind of




alkali solution















Reference




particles to




pH value




Temperature




Time






Examples




be treated




(−)




(° C.)




(min)









Example




Hematite




13.1




90




180






184




particles 18






Example




Hematite




13.5




95




120






185




particles 19






Example




Hematite




13.6




98




150






186




particles 20






Example




Hematite




13.8




85




240






187




particles 21






Reference




Hematite




8.2




85




180






Example 56




particles 18






Reference




Hematite




13.4




40




180






Example 57




particles 18
























TABLE 57













Properties of high-density acicular hematite







particles heat-treated in aqueous alkali solution

















Geometrical





Geometrical







Average




standard




Average




standard







major




deviation of




minor




deviation of






Examples and




axial




major axial




axial




minor axial






Reference




diameter




diameter




diameter




diameter






Examples




(μm)




(−)




(μm)




(−)









Example 184




0.0725




1.36




0.0110




1.28






Example 185




0.0531




1.38




0.0086




1.27






Example 186




0.0821




1.35




0.0117




1.29






Example 187




0.0520




1.37




0.0088




1.29






Reference




0.0726




1.37




0.0111




1.28






Example 56






Reference




0.0726




1.37




0.0111




1.28






Example 57

















Properties of high-density acicular hematite








particles heat-treated in aqueous alkali








solution


















Examples and




Aspect






S


BET


/S


TEM









Reference




ratio




S


BET






S


TEM






value







Examples




(−)




(m


2


/g)




(m


2


/g)




(−)











Example 184




6.6:1




85.1




75.2




1.13







Example 185




6.2:1




96.1




96.7




0.99







Example 186




7.0:1




74.1




70.4




1.05







Example 187




5.9:1




90.6




94.8




0.96







Reference




6.5:1




83.2




74.6




1.12







Example 56







Reference




6.5:1




84.6




74.6




1.13







Example 57

















Properties of high-density acicular hematite







particles heat-treated in aqueous alkali







solution
















Sintering








Examples and




preventive

















Reference




Calculated




Amount




Content of Al







Examples




as




(wt %)




(wt %)











Example 184




P




0.64




3.72







Example 185




P




0.83




3.16







Example 186




SiO


2






1.01




1.44







Example 187




P




0.80




3.16







Reference




P




1.30




3.73







Example 56







Reference




P




1.31




3.76







Example 57

















Properties of high-density acicular hematite







particles heat-treated in aqueous alkali







solution

















Soluble




Soluble









sodium salt




sulfate







Examples and




Resin




(calculated




(calculated







Reference




adsorp-




as Na)




as SO


4


)




pH value






Examples




tion (%)




(ppm)




(ppm)




(−)









Example 184




75.3




72




18




9.3






Example 185




76.8




112




10




9.1






Example 186




78.2




56




23




9.2






Example 187




77.8




81




29




8.9






Reference




61.8




396




192




7.3






Example 56






Reference




64.1




410




190




7.4






Example 57
























TABLE 58












Kind of








particles to be




Concentration of water






Examples




treated




suspension (g/liter)









Example




Example




45






188




184






Example




Example




45






189




185






Example




Example




45






190




186






Example




Example




45






191




187
















Coating treatment with aluminum compound or







silicon compound














Aluminum compound or silicon








compound



















Amount added








pH value





(calculated




Final







before





as Al or




pH







addition




Kind of




SiO


2


)




value






Examples




(−)




additives




(wt %)




(−)









Example




4.0




Aluminum acetate




3.0




7.0






188






Example




10.0




Water glass #3




1.0




6.9






189






Example




10.3




Sodium aluminate




5.0




7.2






190






Example




10.1




Sodium aluminate




2.0




7.0






191





Water glass #3




0.5
























TABLE 59













Properties of acicular hematite particles after







surface-coating treatment

















Geometrical





Geometrical







Average




standard




Average




standard







major




deviation of




minor




deviation of







axial




major axial




axial




minor axial







diameter




diameter




diameter




diameter






Examples




(μm)




(−)




(μm)




(−)









Example




0.0725




1.36




0.0111




1.28






188






Example




0.0531




1.38




0.0086




1.26






189






Example




0.0820




1.36




0.0117




1.28






190






Example




0.0523




1.38




0.0087




1.29






191

















Properties of acicular hematite particles after








surface-coating treatment

















Aspect






S


BET


/S


TEM









ratio




S


BET






S


TEM






value






Examples




(−)




(m


2


/g)




(m


2


/g)




(−)









Example




6.5:1




85.6




74.6




1.15






188






Example




6.2:1




97.1




96.7




1.00






189






Example




7.0:1




75.1




70.4




1.07






190






Example




6.0:1




92.9




95.8




0.97






191
















Properties of acicular hematite particles after







surface-coating treatment














Sintering








preventive


















Calculated




Amount




Content of Al







Examples




as




(wt %)




(wt %)











Example




P




0.62




3.71







188







Example




P




0.80




3.15







189







Example




SiO


2






1.00




1.41







190







Example




P




0.78




3.14







191

















Properties of acicular hematite particles after







surface-coating treatment















Surface-coating




Surface-coating








amount of




amount of oxide of








hydroxide of




silicon








aluminum




(calculated as




Resin







(calculated as Al)




SiO


2


)




adsorption






Examples




(wt %)




(wt %)




(%)









Example




2.93









81.6






188






Example









0.99




83.2






189






Example




4.71









84.1






190






Example




1.96




0.49




81.8






191
















Properties of acicular hematite particles after







surface-coating treatment

















Soluble sodium




Soluble sulfate









salt (calculated




(calculated as









as Na)




SO


4


)




pH value







Examples




(ppm)




(ppm)




(−)











Example




78




13




9.1







188







Example




56




8




9.0







189







Example




82




12




9.0







190







Example




52




26




9.2







191



























TABLE 60













Examples,




Production of non-magnetic








Comparative




coating composition




Non-magnetic
















Examples




Kind of




Weight ratio




coating







and




acicular




of particles




composition







Reference




hematite




to resin




Viscosity







Examples




particles




(−)




(cP)











Example 192




Example 184




5.0




384







Example 193




Example 185




5.0




358







Example 194




Example 186




5.0




364







Example 195




Example 187




5.0




435







Example 196




Example 188




5.0




512







Example 197




Example 189




5.0




461







Example 198




Example 190




5.0




307







Example 199




Example 191




5.0




410







Comparative




Hematite




5.0




870







Example 82




particles 22







Comparative




Hematite




5.0




794







Example 83




particles 23







Comparative




Hematite




5.0




717







Example 84




particles 24







Comparative




Hematite




5.0




11,240







Example 85




particles 25







Comparative




Hematite




5.0




307







Example 86




particles 26







Reference




Reference




5.0




461







Example 58




Example 56







Reference




Reference




5.0




502







Example 59




Example 57



















Examples,




Properties of non-magnetic undercoat








Comparative




layer


















Examples






Surface




Young's







and






roughness




modulus







Reference




Thickness




Gloss




Ra




(relative







Examples




(μm)




(%)




(nm)




value)











Example 192




0.35




218




6.1




136







Example 193




0.35




225




5.7




133







Example 194




0.35




218




6.0




138







Example 195




0.35




211




6.4




134







Example 196




0.35




218




6.0




137







Example 197




0.35




225




5.6




136







Example 198




0.35




216




6.1




137







Example 199




0.35




214




6.3




135







Comparative




0.35




154




20.1




110







Example 82







Comparative




0.35




161




17.8




111







Example 83







Comparative




0.35




164




17.2




116







Example 84







Comparative




0.37




113




28.3




98







Example 85







Comparative




0.35




176




15.4




79







Example 86







Reference




0.35




198




8.2




128







Example 58







Reference




0.36




196




8.5




128







Example 59


























TABLE 61













Examples,




Production of magnetic recording medium













Weight
















Comparative






ratio of







Examples and




Kind of non-





particles







Reference




magnetic




Kind of magnetic




to resin







Examples




substrate,




particles




(−)











Example 200




Example 192




Magnetic metal




5.0









particles (d)







Example 201




Example 195




Magnetic metal




5.0









particles (d)







Example 202




Example 196




Magnetic metal




5.0









particles (d)







Example 203




Example 191




Magnetic metal




5.0









particles (d)







Example 204




Example 192




Magnetic metal




5.0









particles (a)







Example 205




Example 193




Magnetic metal




5.0









particles (b)







Example 206




Example 194




Magnetic metal




5.0









particles (c)







Example 207




Example 195




Magnetic metal




5.0









particles (c)







Example 208




Example 196




Magnetic metal




5.0









particles (a)







Example 209




Example 197




Magnetic metal




5.0









particles (b)







Example 210




Example 198




Magnetic metal




5.0









particles (c)







Example 211




Example 199




Magnetic metal




5.0









particles (c)







Comparative




Comparative




Magnetic metal




5.0







Example 87




Example 82




particles (d)







Comparative




Comparative




Magnetic metal




5.0







Example 88




Example 83




particles (d)







Comparative




Comparative




Magnetic metal




5.0







Example 89




Example 84




particles (d)







Comparative




Comparative




Magnetic metal




5.0







Example 90




Example 85




particles (d)







Comparative




Comparative




Magnetic metal




5.0







Example 91




Example 86




particles (d)







Reference




Reference




Magnetic metal




5.0







Example 60




Example 58




particles (d)







Reference




Reference




Magnetic metal




5.0







Example 61




Example 59




particles (d)


















Examples,




Properties of magnetic recording medium

















Comparative




Thickness










Examples




of







and




magnetic




Coercive




Br/Bm







Reference




layer




force (Hc)




value




Gloss







Examples




(μm)




(Oe)




(−)




(%)











Example 200




1.0




1,968




0.87




223







Example 201




1.0




1,971




0.87




221







Example 202




1.0




1,965




0.88




226







Example 203




1.1




1,962




0.89




228







Example 204




1.0




1,981




0.89




235







Example 205




1.0




1,999




0.87




230







Example 206




1.0




2,130




0.87




226







Example 207




1.1




2,133




0.88




233







Example 208




1.0




1,983




0.88




241







Example 209




1.1




2,001




0.89




238







Example 210




1.0




2,129




0.89




248







Example 211




1.0




2,125




0.90




229







Comparative




1.1




1,960




0.76




168







Example 87







Comparative




1.0




1,963




0.75




175







Example 88







Comparative




1.1




1,968




0.81




176







Example 89







Comparative




1.1




1,963




0.79




171







Example 90







Comparative




1.0




1,965




0.78




152







Example 91







Reference




1.1




1,978




0.86




214







Example 60







Reference




1.1




1,983




0.86




211







Example 61

















Properties of magnetic recording medium
















Examples,






Linear








Comparative






absorp-






Examples




Surface




Young's




tion




Durability






and




rough-




modulus




coeffi-




Running







Reference




ness Ra




(relative




cient




time




Scratch






Examples




(nm)




value)




(μm


−1


)




(min)




resistance









Example 200




6.4




137




1.26




27.1




A






Example 201




6.3




136




1.27




27.3




B






Example 202




6.0




138




1.28




28.1




A






Example 203




5.8




137




1.28




28.5




A






Example 204




6.0




137




1.29




≧30




A






Example 205




6.2




135




1.29




29.6




B






Example 206




6.3




138




1.31




≧30




A






Example 207




6.0




135




1.28




28.6




B






Example 208




5.8




139




1.27




≧30




A






Example 209




5.6




136




1.31




≧30




A






Example 210




5.2




141




1.27




≧30




A






Example 211




5.9




136




1.28




≧30




A






Comparative




18.4 




110




1.03




12.6




D






Example 87






Comparative




13.6 




115




1.05




13.1




D






Example 88






Comparative




12.9 




119




1.10




13.6




D






Example 89






Comparative




15.0 




 93




1.10




12.3




D






Example 90






Comparative




18.4 




 83




1.03




10.6




D






Example 91






Reference




7.8




129




1.17




19.2




C






Example 60






Reference




7.6




129




1.17




18.6




C






Example 61
















Examples,







Comparative















Examples




Properties of magnetic recording medium








and




Corrosion resistance
















Reference




Percentage of change




Percentage of change







Examples




in coercive force (%)




in B


m


(%)











Example 200




4.1




3.9







Example 201




3.8




4.4







Example 202




4.0




2.6







Example 203




3.6




3.1







Example 204




3.1




2.1







Example 205




2.6




1.6







Example 206




1.6




1.8







Example 207




2.1




1.8







Example 208




2.6




2.3







Example 209




1.8




3.6







Example 210




0.6




0.4







Example 211




3.2




0.9







Comparative




31.2




28.1







Example 87







Comparative




26.5




26.5







Example 88







Comparative




31.2




23.1







Example 89







Comparative




41.3




32.6







Example 90







Comparative




26.5




31.2







Example 91







Reference




16.1




17.0







Example 60







Reference




15.6




16.0







Example 61














Claims
  • 1. Acicular hematite particles comprising an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35 and a pH value of not less than 8, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO4.
  • 2. Acicular hematite particles according to claim 1, which further comprise a coat formed on at least a part of the surface of said acicular hematite particle, comprising at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon in amount of 0.05 to 50% by weight, calculated as Al or SiO2, based on the weight of said acicular hematite particles.
  • 3. Acicular hematite particles according to claim 1, which further comprise aluminum existing in the particle in an amount of 0.05 to 50% by weight, calculated as Al, based on the weight of said acicular hematite particles.
  • 4. Acicular hematite particles according to claim 3, which further comprise a resin adsorptivity of not less than 65%.
  • 5. Acicular hematite particles according to claim 3, which further comprise a coat formed on at least a part of the surface of said acicular hematite particle, comprising at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon in amount of 0.05 to 50% by weight, calculated as Al or SiO2, based on the weight of said acicular hematite particles.
  • 6. Acicular hematite particles according to claim 1, which further comprise a geometrical standard deviation of major axis diameter of not more than 1.50 and a BET specific surface area of 35.9 to 180 m2/g.
  • 7. Acicular hematite particles according to claim 1, which further comprise an aspect ratio (average major axis diameter/average minor axis diameter) of 2:1 to 20:1, and a ratio value of a BET specific surface area SBET to a specific surface area STEM of 0.5 to 2.5 (the specific surface area STEM being calculated from the major axis diameter and the minor axis diameter which were measured from the particles in an electron micrograph of the acicular hematite particles).
  • 8. Acicular hematite particles according to claim 1, which further comprise a geometrical standard deviation of major axis diameter of not more than 1.50, a geometrical standard deviation of minor axis diameter of not more than 1.30, a BET specific surface area of 40 to 150 m2/g and an average major axis diameter of 0.01 to 0.2 μm.
  • 9. A magnetic recording medium comprising:a non-magnetic base film; a non-magnetic undercoat layer formed on said non-magnetic base film, comprising a binder resin and acicular hematite particles having an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35 and a pH value of not less than 8, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO4; and a magnetic coating film comprising a binder resin and magnetic acicular metal particles containing iron as a main component.
  • 10. A magnetic recording medium according to claim 9, wherein said acicular hematite particles have a coat formed on at least a part of the surface of said acicular hematite particle and comprising at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon in an amount of 5 to 50% by weight based on the total weight of the acicular hematite particles.
  • 11. A magnetic recording medium according to claim 9, wherein said acicular hematite particles contain aluminum existing in the particle in an amount of 0.05 to 50% by weight, calculated as Al, based on the weight of said acicular hematite particles.
  • 12. Magnetic recording medium according to claim 11, wherein said acicular hematite particles have a resin adsorptivity of not less than 65%.
  • 13. A magnetic recording medium according to claim 11, wherein said acicular hematite particles have a coat formed on at least a part of the surface of said acicular hematite particle and comprising at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon in an amount of 5 to 50% by weight based on the total weight of the acicular hematite particles.
  • 14. A magnetic recording medium according to claim 11, which further comprises a gloss of coating film of 194 to 300%, a surface roughness Ra of coating film of not more than 9.6 nm, a linear absorption of coating film of 1.10 to 2.00 μm—1, and a running durability of not less than 22 minutes.
  • 15. A magnetic recording medium according to claim 9, wherein said acicular hematite particles have a geometrical standard deviation of major axis diameter of not more than 1.50 and a BET specific surface area of 35.9 to 180 m2/g.
  • 16. A magnetic recording medium according to claim 9, wherein said acicular hematite particles have a geometrical standard deviation of major axis diameter of not more than 1.50, a geometrical standard deviation of minor axis diameter of not more than 1.30, a BET specific surface area of 40 to 150 m2/g and an average major axis diameter of 0.01 to 0.2 μm.
  • 17. A magnetic recording medium according to claim 16, which further comprises a gloss of coating film of 196 to 300%, a surface roughness Ra of coating film of not more than 9.4 nm, and a linear absorption of coating film of 1.10 to 2.00 μm−1.
  • 18. A magnetic recording medium according to claim 9, wherein said magnetic acicular metal particles containing iron as a main component contain aluminum in an amount of 0.05 to 10% by weight, calculated as Al, based on the weight of said magnetic acicular metal particles containing iron as a main component.
  • 19. A magnetic recording medium according to claim 18, which further comprises a gloss of coating film of 194 to 300%, a surface roughness Ra of coating film of not more than 9.6 nm, a linear absorption of coating film of 1.10 to 2.00 μm−1, and a running durability of not less than 24 minutes.
  • 20. A magnetic recording medium according to claim 9, which further comprises a gloss of coating film of 192 to 300%, a surface roughness Ra of coating film of not more than 9.8 nm, and a linear absorption of coating film of 1.10 to 2.00 μm−1.
  • 21. A magnetic recording medium according to claim 9, which further comprises the change in the coercive force of not more than 10.0% and the change in the saturation magnetic flux density of not more than 10.0%.
  • 22. A non-magnetic substrate comprising:a non-magnetic base film; and a non-magnetic undercoat layer formed on said non-magnetic base film, comprising a binder resin and acicular hematite particles having an average major axis diameter of 0.004 to 0.295 μm, a geometrical standard deviation of minor axis diameter of not more than 1.35 and a pH value of not less than 8, and containing not more than 300 ppm of soluble sodium salt, calculated as Na and not more than 150 ppm of soluble sulfate, calculated as SO4.
  • 23. A non-magnetic substrate according to claim 22, wherein said acicular hematite particles have a coat formed on at least a part of the surface of said acicular hematite particle and comprising at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon in an amount of 5 to 50% by weight based on the total weight of the acicular hematite particles.
  • 24. A non-magnetic substrate according to claim 22, wherein said acicular hematite particles contain aluminum existing within the particle in an amount of 0.05 to 50% by weight, calculated as Al, based on the weight of said acicular hematite particles.
  • 25. A non-magnetic substrate according to claim 24, wherein said acicular hematite particles have a coat formed on at least a part of the surface of said acicular hematite particle and comprising at least one compound selected from the group consisting of hydroxides of aluminum, oxides of aluminum, hydroxides of silicon and oxides of silicon in an amount of 5 to 50% by weight based on the total weight of the acicular hematite particles.
  • 26. A non-magnetic substrate according to claim 24, which further comprises a gloss of coating film of 191 to 300% and a surface roughness Ra of coating film of 0.5 to 9.3 nm.
  • 27. A non-magnetic substrate according to claim 22, wherein said acicular hematite particles further have a geometrical standard deviation of major axis diameter of not more than 1.50 and a BET specific surface area of 35.9 to 180 m2/g.
  • 28. A non-magnetic substrate according to claim 22, wherein said acicular hematite particles have a geometrical standard deviation of major axis diameter of not more than 1.50, a geometrical standard deviation of minor axis diameter of not more than 1.30, a BET specific surface area of 40 to 150 m2/g and an average major axis diameter of 0.01 to 0.2 μm.
  • 29. A non-magnetic substrate according to claim 28, which further comprises a gloss of coating film of 193 to 300% and a surface roughness Ra of coating film of 0.5 to 9.0 nm.
  • 30. A non-magnetic substrate according to claim 22, which further comprises a gloss of coating film of 189 to 300% and a surface roughness Ra of coating film of 0.5 to 9.6 nm.
Priority Claims (3)
Number Date Country Kind
9-369364 Dec 1997 JP
10-018143 Jan 1998 JP
10-116046 Apr 1998 JP
US Referenced Citations (11)
Number Name Date Kind
3843773 Pingaud Oct 1974
4033891 Matsui et al. Jul 1977
5133805 Kurata et al. Jul 1992
5137783 Tanihara et al. Aug 1992
5156922 Mishima et al. Oct 1992
5411801 Honmyo May 1995
5443666 Kiatamura et al. Aug 1995
5512194 Ogasawara et al. Apr 1996
5660927 Arase et al. Aug 1997
5750250 Hayashi et al. May 1998
5922464 Hayashi et al. Jul 1999
Foreign Referenced Citations (3)
Number Date Country
0 597 694 A1 May 1994 EP
0 769 775 A1 Apr 1997 EP
63-153201 Jun 1988 JP