Method Of Producing Soft Magnetic Material, Soft Magnetic Powder, And Dust Core

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a schematic view of a cross section of a dust core produced by a method of producing a soft magnetic material according to an embodiment of the present invention.

FIG. 2 is a schematic view showing a state of a soft magnetic particle obtained in an atomization process of producing the dust core as shown in FIG. 1.

FIG. 3 is a picture of a SEM-EBSP image (scanning electron microscope-electron back scattering pattern) of the soft magnetic particle schematically shown in FIG. 2.

FIG. 4 is an enlarged view of the soft magnetic particle showing the area defined by a chain line with two dots IV shown in FIG. 3.

FIG. 5 is a schematic view showing a state of the soft magnetic particle obtained in an etching step of producing the dust core shown in FIG. 1.

FIG. 6 is a schematic view showing a state of the soft magnetic particle obtained in a first heat treatment step of producing the dust core shown in FIG. 1.

FIG. 7 is a schematic view showing a state of the soft magnetic particle obtained in a pressure-forming step of producing the dust core shown in FIG. 1.

FIG. 8 is a schematic view showing a state of the soft magnetic particle obtained in a second heat treatment step of producing the dust core shown in FIG. 1.

FIG. 9 is a graph showing a relationship between a heat treatment temperature and coercivity of soft magnetic powder in a second embodiment of the present invention.

DESCRIPTION OF THE REFERENCE CHARACTERS

10 soft magnetic particle, 10a surface, 20 insulating film, 30 composite magnetic particle, 40 organic matter.

BEST MODES FOR CARRYING OUT THE INVENTION

Embodiments of the present invention will be described with reference to the drawings.

Referring to FIG. 1, a dust core includes a plurality of composite magnetic particles 30 each formed of a soft magnetic particle 10 and an insulating film 20 surrounding a surface of soft magnetic particle 10. Organic matter 40 is disposed between the plurality of composite magnetic particles 30. Each of the plurality of composite magnetic particles 30 is bonded to each other through organic matter 40, or bonded to each other through engagement of protrusions and recesses of composite magnetic particles 30. Organic matter 40 firmly bonds composite magnetic particles 30 together to improve the strength of the dust core.

Soft magnetic particle 10 can be made of, for example, iron (Fe), an iron (Fe)-silicon (Si) alloy, an iron (Fe)-nitrogen (N) alloy, an iron (Fe)-nickel (Ni) alloy, an iron (Fe)-carbon (C) alloy, an iron (Fe)-boron (B) alloy, an iron (Fe)-cobalt (Co) alloy, an iron (Fe)-phosphorus (P) alloy, an iron (Fe)-nickel (Ni)-cobalt (Co) alloy, an iron (Fe)-aluminum (Al)-silicon (Si) alloy and the like. Soft magnetic particle 10 may be of a simple substance of metal or an alloy.

Insulating film 20 is formed, for example, by treating soft magnetic particle 10 with phosphoric acid. Further, insulating film 20 preferably contains an oxide. As insulating film 20 containing the oxide, an oxide insulator can be used, such as, in addition to iron phosphate containing phosphorus and iron, manganese phosphate, zinc phosphate, calcium phosphate, aluminum phosphate, silicon oxide, titanium oxide, aluminum oxide, or zirconium oxide. Insulating film 20 may be formed in a single layer as shown in the drawing, or may be formed in multiple layers.

Insulating film 20 serves as an insulating layer between soft magnetic particles 10. By covering soft magnetic particle 10 with insulating film 20, electric resistivity ρ of the dust core can be increased. Thus, eddy current can be prevented from flowing between soft magnetic particles 10, to thereby reduce iron loss of the dust core resulting from the eddy current.

As organic matter 40, thermoplastic resin such as thermoplastic polyimide, thermoplastic polyamide, thermoplastic polyamidimide, polyphenylene sulfide, polyamidimide, polyethersulfone, polyether imide or polyetheretherketone; non-thermoplastic resin such as wholly aromatic polyester or wholly aromatic polyimide; and higher fatty acid such as high-molecular-weight polyethylene, zinc stearate, lithium stearate, calcium stearate, lithium palmitate, calcium palmitate, lithium oleate and calcium oleate can be employed. These can also be employed in combination with each other. A high-molecular-weight polyethylene refers to a polyethylene having a molecular weight of not less than 100,000.

A method of producing a soft magnetic material according to the embodiment will then be described using FIGS. 2 to 8.

Referring to FIG. 2, first, an atomization method is used to produce soft magnetic powder made of plurality of soft magnetic particles 10. More specifically, dissolved source metal is pulverized by using high-pressure water to spray and rapidly quench the metal, and thus, the plurality of soft magnetic particles 10 are produced. Soft magnetic particle 10 obtained by this rapid quenching step includes, in addition to a grain boundary 51 extending between grains, a surface layer microgram 57 formed along a surface 10a with a predetermined depth, a surface layer micrograin boundary 53 extending between surface layer micrograins 57, a subgrain 56 formed within soft magnetic particle 10, and a subgrain boundary 52 extending between subgrains 56. It is to be noted that the method of producing the soft magnetic powder is not limited to a water atomization method and may be a gas atomization method.

FIGS. 3 and 4 show atomized iron powder with a purity of not less than 99.8% produced by the water atomization method. Referring to FIGS. 3 and 4, in the case of using the water atomization method, soft magnetic particle 10 with a diameter of about 100 μm has surface layer micrograin 57 formed at a depth of about 100 nm to 250 nm from the surface. On the other hand, in the case where the gas atomization method is used to produce the soft magnetic powder, the formed depth of the surface layer micrograin is relatively shallow, which is in the vicinity of 10 nm relative to the diameter of about 100 μm. However, the formed depth of the surface layer micrograin described herein is an example, and varies with the quality and the particle size of the soft magnetic particle, the conditions of producing the soft magnetic powder, and the like.

Referring to FIG. 5, the soft magnetic powder is then subjected to an etching process by introducing the soft magnetic powder into hydrogen chloride (HCl) aqueous solution (hydrochloric acid) and performing a stirring process for a predetermined time. In this case, in addition to hydrochloric acid, phosphoric acid (H₃PO₄), nitric acid (HNO₃), sulfuric acid (H₂SO₄) and a mixed solution thereof can be used. In addition to the acid treatment using these aqueous solutions, for example, an argon ion milling method performed using an ion milling device and a reactive ion etching method using active species of reactive gas in plasma can also be used.

The above-described etching process removes the surface of soft magnetic particle 10 along a predetermined depth from surface 10a, to thereby remove surface layer micrograin 57 formed in soft magnetic particle 10 from soft magnetic particle 10. In this case, the etching process is preferably performed such that the average particle size of the soft magnetic powder after the etching process takes a value of not less than 90% of the average particle size of the soft magnetic powder before the etching process. The average particle size described herein refers to a particle size obtained when the sum of masses of particles added in ascending order of particle size in a histogram of particle sizes measured by a laser scatter diffraction method and the like reaches 50% of the total mass, that is, 50% particle size D.

It is also preferable that, after the etching process, the particle size of soft magnetic particle 10 is substantially distributed only in the range of not less than 10 μm and not more than 400 μm. In this case, any particle with a size of less than 10 μm and any particle with a size of greater than 400 μm may be forcefully removed from the soft magnetic powder after the etching process, by using a sieve with appropriate mesh size. It is further preferable that the particle size of soft magnetic particle 10 is substantially distributed only in the range of not less than 75 μm and not more than 355 μm.

The soft magnetic powder subjected to the etching process is then washed, and the soft magnetic powder is subsequently dried by replacing moisture with acetone.

Referring to FIG. 6, the soft magnetic powder is then subjected to a heat treatment at a temperature of not less than 400° C. and not more than 900° C., for example, for one hour. The heat treatment is further preferably performed at a temperature of not less than 700° C. and not more than 900° C. If this heat treatment leaves subgrain boundary 52 formed within soft magnetic particle 10 and the surface layer micrograin on a new surface 10b of soft magnetic particle 10, the grain boundary by the surface layer micrograin is caused to be eliminated. In this case, since the etching process performed in the previous step causes all or most of the surface layer micrograins to be previously removed, the grain discontinuities existing within soft magnetic particle 10 can be effectively eliminated.

Referring to FIG. 7, insulating film 20 is formed on surface 10b of soft magnetic particle 10 to produce composite magnetic particles 30. Mixed powder is then obtained by adding organic matter 40 to resulting composite magnetic particles 30 and mixing together. There is no specific limitation on the mixing technique, and any technique such as mechanical alloying, vibratory ball milling, planetary ball milling, mechanofusion, coprecipitation, chemical vapor deposition (CVD), physical vapor deposition (PVD), plating, sputtering, vapor deposition, or sol-gel process may be used.

The obtained mixed powder is then introduced into a mold and pressure-formed under a pressure of 700 MPa to 1500 MPa, for example. This results in compression of the mixed powder to create a compact. The mixed powder is preferably pressure-formed in an inert gas atmosphere or a decompressed atmosphere. In this case, the mixed powder can be prevented from oxidation by oxygen in the atmosphere. This pressure-forming causes strain 61 to be newly created in soft magnetic particle 10.

In this case, most of surface layer micrograin boundary 53 and subgrain boundary 52 originally existing within soft magnetic particle 10 are eliminated by the etching process as described using FIG. 5 and the heat treatment as described using FIG. 6. Thus, composite magnetic particle 30 is in a state which is easily deformed in the pressure-forming. Therefore, the compact can be formed in such a manner that the plurality of composite magnetic particles 30 are engaged with each other without gaps, as shown in FIG. 1. This allows an increase in the density of the compact, to thereby achieve high magnetic permeability. Organic matter 40 is located between adjacent composite magnetic particles 30 to serve as a lubricant and prevent breakage of insulating film 20 due to rubbing of composite magnetic particles 30 against each other.

Referring to FIG. 8, the compact obtained by the pressure-forming is then heat-treated at a temperature of not less than 30° C. and less than the thermal decomposition temperature of insulating film 20. Insulating film 20 has a thermal decomposition temperature of, for example, 500° C. in the case of a phosphate insulating film.

In this case, since most of surface layer micrograin boundary 53 and subgrain boundary 52 originally existing within soft magnetic particle 10 are eliminated, the amount of the grain discontinuities within the compact is relatively small even after the pressure-forming. Furthermore, since there are few grain discontinuities within soft magnetic particle 10 in the pressure-forming, new strain 61 is created without complexly intertwining with these grain discontinuities. For these reasons, the grain discontinuities existing within the compact can be easily reduced despite that the heat treatment is carried out at a relatively low temperature of less than the thermal decomposition temperature of insulating film 20.

Since the heat treatment on the compact is performed at a temperature of less than the thermal decomposition temperature of insulating film 20, the heat treatment does not lead to deterioration of insulating film 20. This keeps insulating film 20 covering soft magnetic particle 10 even after the heat treatment, and allows insulating film 20 to reliably prevent an eddy current from flowing between soft magnetic particles 10. More preferably, the compact obtained by the pressure-forming is heat-treated at a temperature of not less than 30° C. and not more than 300° C. In this case, insulating film 20 can be further prevented from deterioration.

The resulting compact is thereafter subjected to an appropriate treatment such as extrusion or cutting to provide a finished dust core as shown in FIG. 1.

The method of producing the soft magnetic material according to the embodiment of the present invention includes the steps of preparing the soft magnetic powder containing the plurality of soft magnetic particles 10, etching the soft magnetic powder to remove surfaces 10a of soft magnetic particles 10, and, after the etching step, performing the heat treatment of the soft magnetic powder in a finely divided state at a temperature of not less than 400° C. and not more than 900° C.

According to the method of producing the soft magnetic material configured as above, soft magnetic particle 10 before the pressure-forming is subjected to the etching process and also to the heat treatment at a predetermined range of the temperature, to allow production of the dust core with the grain discontinuities well eliminated. This allows hysteresis loss of the dust core to be reduced. Since the heat treatment to the soft magnetic powder is carried out before insulating film 20 is formed on soft magnetic particle 10, the heat treatment does not lead to deterioration of insulating film 20. Furthermore, since the heat treatment to the compact is carried out at a temperature of less than the thermal decomposition temperature of insulating film 20, deterioration of insulating film 20 by the heat treatment is also suppressed. This allows insulating film 20 to serve well as an insulating layer between soft magnetic particles 10 and eddy current loss of the dust core to be reduced. As a result, iron loss of the dust core can be significantly reduced through reduction in hysteresis loss and eddy current loss.

EXAMPLE

The method of producing the soft magnetic material according to the present invention was evaluated by the examples described below.

Example 1

According to the producing method described in the embodiment, the soft magnetic powder was first subjected to the etching process. In this case, as soft magnetic particle 10, water-atomized iron powder with a purity of not less than 99.8% (product name “ABC100.30” manufactured by Hoganas AB) was used. The etching process was carried out by preparing hydrogen chloride aqueous solution with a concentration of 3% by mass (600 cm³), introducing 200 grams of the soft magnetic powder into the solution and stirring the solution. In this case, different stirring times in a range of 10 minutes to 300 minutes were employed to produce the plurality of soft magnetic powders which were subjected to the etching process under different conditions. The soft magnetic powder which was not subjected to the etching process was also prepared for comparison purposes.

The average particle size and coercivity of the soft magnetic powder produced as above were measured. When the coercivity was measured, a resin binder was first used to solidify the soft magnetic powder and produce a pellet (20 mm in diameter, 5 mm in thickness). A magnetic field was applied to the pellet in the sequence of 1 (T: tesla), −1 T, 1 T and −1 T, and a vibrating sample magnetometer (VSM) was used to specify the shape of a B (magnetic flux) H (magnetic field) loop at the time. From the shape of this BH loop was calculated the coercivity of the pellet whose value was assumed to be the coercivity of the soft magnetic powder.

The soft magnetic powder was then subjected to the heat treatment under conditions at a temperature of 850° C. in a hydrogen gas stream for one hour. The coercivity of the soft magnetic powder after the heat treatment was measured by the similar method as above.

The soft magnetic powder was then covered with a film to form a phosphate iron film as insulating film 20 on the surface of soft magnetic particle 10. Polyphenylene sulfide (PPS resin) was added to the soft magnetic powder covered with the film in a proportion of 1% by mass relative to the soft magnetic powder, and mixed together. The resulting mixed powder was press-formed at a surface pressure of 13 ton/cm²to produce the compact in a ring shape (34 mm in outer diameter, 20 mm in inner diameter, 5 mm in thickness). By winding a coil around the obtained compact (300 turns for the primary and 20 turns for the secondary) and applying a magnetic field to the compact, the coercivity and the magnetic permeability of the compact were measured.

The compact was then subjected to the heat treatment under conditions at a temperature of 550° C. in a nitrogen gas stream for one hour. The coercivity and the magnetic permeability of the compact after the heat treatment was measured by the similar method as above. Values of the coercivity and the magnetic permeability of the soft magnetic powder and the compact obtained by the above-described measurement are shown in Table 1.

TABLE 1

Soft Magnetic Powder

Average

Compact

Particle
Coercivity

Coercivity
Magnetic

Size after
after
Coercivity
after
Permeability
Coercivity
Magnetic

Stirring
Etching
Etching
after Heat
Pressure
after
after Heat
Permeability

Time
Process
Process
Treatment
Forming
Pressure
Treatment
after Heat

(min.)
(μm)
(Oe)
(Oe)
(Oe)
Forming
(Oe)
Treatment

0
83
2.86
2.20
4.28
573
1.52
954

10
82
2.84
2.16
4.22
582
1.46
1008

20
80
2.77
2.11
4.13
596
1.42
1066

30
80
2.54
1.95
3.74
635
1.26
1164

40
76
2.61
2.03
3.96
615
1.30
1122

60
76
2.74
2.10
4.01
566
1.36
1040

90
74
2.96
2.23
4.19
530
1.55
922

120
70
3.11
2.29
4.25
508
1.62
901

150
68
3.14
2.27
4.26
482
1.69
888

180
67
3.13
2.31
4.29
468
1.80
842

240
63
3.25
2.36
4.30
452
1.83
831

300
59
3.37
2.42
4.38
429
1.86
779

As can be seen from Table 1, the soft magnetic powder with the stirring time of not more than 60 minutes achieved the average particle size which was kept to a value of not less than 90% relative to the average particle size before the etching process. In this case, the coercivity after the heat treatment could be reduced as compared to the soft magnetic powder which was not subjected to the etching process. In particular, the coercivity could be effectively reduced with the stirring time in the range of 30 to 40 minutes. It is thought that the reason why the coercivity was increased with increasing stirring time in the range of not less than 60 minutes was that soft magnetic particle 10 with the particle size reduced too much caused the effects of the shape diamagnetic field and stress strain by surface energy to exceed the effect of eliminating the surface layer micrograin boundary by the etching process.

More specifically, if no processing was performed, the original coercivity of the soft magnetic powder was 2.86 (Oe: oersted). If the heat treatment was performed, a coercivity of 2.20 (Oe) was achieved, which was about 77% of the original coercivity. On the other hand, when stirring was performed for 30 minutes in the etching process, the coercivity after the heat treatment was 1.95 (Oe), which was a value of about 68% relative to 2.86 (Oe). Thus, it was possible to confirm that the coercivity of the soft magnetic powder could be reduced to a value of not more than 70% according to the present invention.

In accordance with the reduced coercivity of the soft magnetic powder as described above, each coercivity of the compact obtained by the pressure forming and the compact further subjected to the heat treatment could be reduced and each magnetic permeability thereof could be increased. Particularly in the case of the processing time in the range of 30 minutes to 40 minutes, the coercivity of the compact after the heat treatment could be reduced to a value of not more than 1.30 (Oe) (=1.0×10²A/m).

Example 2

In the present example, the soft magnetic powder which was used in Example 1 and was not subjected to the etching process and the soft magnetic powder which was stirred for 30 minutes in the etching process were subjected to the heat treatment under conditions at different heat treatment temperatures in the hydrogen gas stream for one hour. Each coercivity of the soft magnetic powder treated at respective heat treatment temperatures was measured by a method similar to that of Example 1. Values of each coercivity obtained by the measurement are shown in Table 2 and plotted values are shown in FIG. 9.

TABLE 2

Stirring Time
Stirring Time

0 (min.)
30 (min.)

Coercivity of
Coercivity of

Soft Magnetic
Soft Magnetic

Temperature of First Heat
Powder after
Powder after

Treatment on Soft
Heat Treatment
Heat Treatment

Magnetic Powder (° C.)
(Oe)
(Oe)

25
2.86
2.54

250
2.82
2.52

300
2.78
2.49

350
2.74
2.46

400
2.68
2.41

450
2.62
2.36

500
2.55
2.29

550
2.48
2.2

600
2.4
2.13

650
2.33
2.08

700
2.28
2

750
2.23
1.98

800
2.21
1.94

850
2.2
1.95

900
2.26
2.52

(Pulverization
(Pulverization

Needed)
Needed)

950
2.66
Measurement Not

(Pulverization
Available

Needed)
(Pulverization

Not Available)

1000
Measurement
Measurement

Not Available
Not Available

(Pulverization
(Pulverization

Not Available)
Not Available)

Referring to Table 2 and FIG. 9, in the case of the heat treatment temperature of 900° C., the heat treatment caused the soft magnetic powder to be slightly solidified to create a need for slight pulverization. As a result, the measured coercivity had an increased value. In the case of the heat treatment temperature of greater than 900° C., the soft magnetic powder was solidified rigidly such that it could not be pulverized in some cases. Also in the case where the solidified soft magnetic powder could be pulverized, the measured coercivity had a significantly increased value. Thus, it was possible to confirm that the coercivity of the soft magnetic powder could be reduced by setting the temperature in the heat treatment on the soft magnetic powder to a temperature of not more than 900° C., for example, 850° C., as performed in Example 1.

It should be understood that the embodiments and examples disclosed herein are illustrative and non-restrictive in every respect. The scope of the present invention is defined by the terms of the claims, rather than the description above, and is intended to include any modifications within the scope and meaning equivalent to the terms of the claims.

INDUSTRIAL APPLICABILITY

The present invention is applicable in manufacturing motor cores, electromagnetic valves, reactors or other electromagnetic components fabricated from pressure-formed soft magnetic powder, for example.

Method Of Producing Soft Magnetic Material, Soft Magnetic Powder, And Dust Core

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