The present invention relates generally to the field of magnets and, more particularly, to anisotropic bonded magnets fabricated by surfactant-assisted ball milling and magnetic-field processing.
Improved permanent magnets are essential for emergent applications in electronic and electric devices [1-3]. While sintered permanent magnets are still the major type magnets for most applications, demand for bonded magnets is rapidly growing for the advantages of bonded magnets in part size and shape control which is particularly important for miniaturization of electronic devices [4]. However, there is a major disadvantage of bonded magnets: their energy density is substantially lower than sintered magnets, due to diluted magnetic components and the isotropic nature. Most rare-earth bonded magnets are isotropic because the magnetic powders used for producing bonded magnets are isotropic. Though attempts have been made to produce anisotropic bonded rare-earth magnets based on Nd—Fe—B and Sm—Fe—N micron-sized powder particles [5-8] production of nanoscale anisotropic rare-earth magnetic powder particles remains a significant challenge.
Surfactant-assisted ball-milling has been proven to be an effective technique to produce anisotropic hard magnetic nanoparticles including Sm—Co and Nd—Fe—B based rare-earth nanocrystalline materials [9-13]. The produced Sm—Co and Nd—Fe—B nanoparticles containing fine grains have high aspect ratio with their thickness of tens of nanometers and width and length of several hundred nanometers. The chip-like nanocrystals show strong magnetocrystalline anisotropy and can be aligned in a magnetic field.
The present invention provides a product and process from fabricating anisotropic bonded magnets by surfactant-assisted ball milling in a magnetic field and magnetic field alignment of the milled chip-like nanoparticles of the Sm—Co and Nd—Fe—B materials. The application of magnetic fields during the ball milling strengthens the anisotropy of the chips and therefore improves the alignment. This combined technique opens a new approach to fabrication of anisotropic bounded magnets for various applications.
More specifically, the present invention provides a method for fabricating an anisotropic bonded magnet by producing anisotropic chips by ball milling a rare-earth polycrystalline material with a surfactant in presence of a first magnetic field, mixing the anisotropic chips with one or more binding agents, and forming the anisotropic bonded magnet by compacting the mixture of anisotropic chips and binding agents in presence of a second magnetic field.
In addition, the present invention provides an anisotropic bonded magnet fabricated by producing anisotropic chips by ball milling a rare-earth polycrystalline material with a surfactant in presence of a first magnetic field, mixing the anisotropic chips with one or more binding agents, and forming the anisotropic bonded magnet by compacting the mixture of anisotropic chips and binding agents in presence of a second magnetic field.
Moreover, the present invention provides a method for fabricating an anisotropic bonded magnet by producing anisotropic chips by ball milling a SmCo5, Sm2Co7 or Nd2Fe14B material with oleic acid having a purity of at least 90% and heptane having a purity of at least 99% in presence of a first magnetic field having a first H-field value of at least 1 to 3 kOe, wherein the oleic acid is 50% by weight of the SmCo5, Sm2Co7 or Nd2Fe14B material. The anisotropic chips are then mixed with phenylene sulfide (PPS), and the anisotropic bonded magnet is formed by compacting the mixture of anisotropic chips and epoxy or polymer in presence of a second magnetic field having a second H-field value of at least 20 kOe.
Furthermore, the present invention provides an anisotropic bonded magnet fabricated by producing anisotropic chips by ball milling a SmCo5, Sm2Co7 or Nd2Fe14B material with oleic acid having a purity of at least 90% and heptane having a purity of at least 99% in presence of a first magnetic field having a first H-field value of at least 1 to 3 kOe, wherein the oleic acid is 50% by weight of the SmCo5, Sm2Co7 or Nd2Fe14B material, mixing the anisotropic chips with phenylene sulfide (PPS), and forming the anisotropic bonded magnet by compacting the mixture of anisotropic chips and epoxy or polymer in presence of a second magnetic field having a second H-field value of at least 20 kOe.
The present invention is described in detail below with reference to the accompanying drawings.
Further benefits and advantages of the present invention will become more apparent from the following description of various embodiments that are given by way of example with reference to the accompanying drawings:
While the making and using of various embodiments of the present invention are discussed in detail below, it should be appreciated that the present invention provides many applicable inventive concepts that can be embodied in a wide variety of specific contexts. The specific embodiments discussed herein are merely illustrative of specific ways to make and use the invention and do not delimit the scope of the invention.
To facilitate the understanding of this invention, a number of terms are defined below. Terms defined herein have meanings as commonly understood by a person of ordinary skill in the areas relevant to the present invention. Terms such as “a”, “an” and “the” are not intended to refer to only a singular entity, but include the general class of which a specific example may be used for illustration. The terminology herein is used to describe specific embodiments of the invention, but their usage does not delimit the invention, except as outlined in the claims.
To further enhance the magnetic anisotropy of the nanoparticles, the present invention provides a fabrication method in which a magnetic field is applied during surfactant-assisted ball-milling. The anisotropic nanoscale chips are then processed into bonded magnets by mixing binder materials with the powders and pressing the mixtures in a magnetic field. The description below demonstrates the anisotropic magnetic properties of the bonded magnets fabricated by methods of the present invention. Moreover, the effect of external magnetic fields during ball milling on the magnetic properties will be discussed in detail.
Now referring to
The oleic acid can have a purity of at least 90%. Moreover, the oleic acid can be 50% by weight of the rare-earth polycrystalline material. A phenylene sulfide (PPS) can be used as the binding agent. The first magnetic field can have a first H-field value of at least 1 to 3 kOe and the second magnetic field can have a second H-field value of at least 20 kOe. The first magnetic field and the second magnetic field can have a B-field value of at least 15 to 20 kG. The ball milling process can take between 10 minutes to 20 hours. The first magnetic field and the second magnetic field are produced by two diametrically oriented arc-segment permanent magnets fixed around a non-metallic vessel (e.g., stainless steel, etc.). As will be appreciated by those skilled in the art, the rare-earth polycrystalline materials, binding agents, magnetic field values, processing times and other components and variables described herein are merely representative examples and can be changed and/or modified depending on the characteristics and properties that are desired in the resulting magnet.
In addition, a solvent (e.g., heptane, xylene, etc.) can be used with the rare-earth polycrystalline material in addition to the surfactant. The method can also include the steps of curing the compacted mixture of anisotropic chips and binding agents, or removing one or more fine particles from the anisotropic chips. For example, the fine particles can be removed by subjecting the anisotropic chips to an ultrasonic vibration, washing the anisotropic chips, and centrifuging the anisotropic chips. The anisotropic chips can be washed with a solution comprising heptane. Moreover, the step of mixing the anisotropic chips with the one or more binding agents is performed within the first magnetic field or the second magnetic field or a third magnetic field. Note that the magnetic fields can be the same throughout the process.
In some embodiments of the present invention, the anisotropic chips have an energy product greater than or equal to 24 MGOe and a remanence of greater than equal to 0.92 Tesla. The anisotropic bonded magnet can have an energy product greater than 13 MGOe with a density of greater than 6.5 g/cm3.
As a result, the present invention provides an anisotropic bonded magnet fabricated by producing anisotropic chips by ball milling a rare-earth polycrystalline material with a surfactant in presence of a first magnetic field, mixing the anisotropic chips with one or more binding agents, and forming the anisotropic bonded magnet by compacting the mixture of anisotropic chips and binding agents in presence of a second magnetic field.
Referring now to
As a result, the present invention provides an anisotropic bonded magnet fabricated by producing anisotropic chips by ball milling a SmCo5, Sm2Co7 or Nd2Fe14B material with oleic acid having a purity of at least 90% and heptane having a purity of at least 99% in presence of a first magnetic field having a first H-field value of at least 1 to 3 kOe, wherein the oleic acid is 50% by weight of the SmCo5, Sm2Co7 or Nd2Fe14B material, mixing the anisotropic chips with phenylene sulfide (PPS), and forming the anisotropic bonded magnet by compacting the mixture of anisotropic chips and epoxy or polymer in presence of a second magnetic field having a second H-field value of at least 20 kOe.
In one example of the present invention, the starting commercial SmCo5, Sm2Co7 and Nd2Fe14B powders of particle size ˜45 μm were mixed with organic solvent heptane of 99.8% purity and surfactant oleic acid of 90% purity. In a typical milling load, powder to ball weight ratio of 1:10 was used in a nonmagnetic stainless steel vial. The amount of surfactant used was 50% by weight of the starting powders. Two diametrically oriented arc-segment permanent magnets were fixed around a nonmagnetic stainless steel vial to create a quasi-homogeneous magnetic field of about 1-3 kOe. The mixtures were then milled using a high-energy ball milling machine from 10 minutes to 20 hours. For comparison, the starting powders were also milled without magnetic field while keeping other milling parameters unchanged. A size selection process was employed after the milling process to remove fine particles by ultrasonic vibration and washing final products several times with heptane followed by centrifugal process [10-12]. To characterize the anisotropic magnetic properties, nanoscale chips were mixed with epoxy and aligned in a magnetic field of 20 kOe. Bonded magnets were made by mixing as-milled nanoparticles with organic binders and pressing the mixture under a magnetic field of about 16 kG. Magnetic properties were measured by a superconducting interference device magnetometer with a maximum applied field of 70 kOe. Structural and morphological characterizations were performed using x-ray diffraction (XRD) (Rigaku Ultima IV diffractometer operating with CuKα radiation) and scanning electron microscope (SEM). Measurement of (002) pole figures were carried out by the Schulz's reflection method. The tilt angle (α) was varied from 0° to 70° in steps of 2.5°. The angle of rotation, azimuth angle (β) was varied from 0° to 360° in steps of 5°.
Now referring to
To further enhance the magnetic anisotropy, an external magnetic field was applied during the ball milling process. Previous investigations [14, 15] revealed that external magnetic fields enhance magnetic anisotropy in polycrystalline particles prepared by ball milling. The magnetic fields, however, reduced the milling efficiency simultaneously, as seen from the grain size reduction for samples milled for same time. Therefore, it is more reasonable to compare the anisotropy of samples with same grain size (instead of same milling time).
Degree of alignment of chips can also be calculated by the average misalignment angle ψ=arctan [2Mr (⊥)/Mr (//)], where Mr (⊥) and Mr (//) are the remanences perpendicular and parallel to the direction of the easy axis [16].
Referring now to
Morphology of SmCo and NdFeB chips obtained by surfactant-assisted ball milling in a magnetic field and in absence of magnetic field for different milling time was monitored by SEM.
As a result of the enhanced magnetic anisotropy, remarkably higher energy product values are obtained for SmCo5 nanoscale chips milled under magnetic field compared to those without magnetic field in same milling conditions. For example, higher energy products up to 26.0 MGOe has been obtained for SmCo5 nanoparticles prepared in magnetic field, compared to 23.5 MGOe of that without magnetic field (with the remanence of 0.96 and 0.91, respectively). The higher energy product in a field milled chips samples results from enhanced remanence and better squareness of the demagnetization curves compared to the nanoparticles milled without field. The difference of magnetic properties is also an evidence for enhanced anisotropy. Based on the anisotropic chips, it is possible to fabricate anisotropic bulk magnets by compaction of the chips in the presence of a magnetic field. The magnetic field aligns the chips during which the compaction consolidates the aligned flakes. The energy product above 13 MGOe with real density 6.5 g/cm3 has been obtained for the bonded magnets prepared by SmCo5 chips milled in presence of a magnetic field and compacted under the magnetic field using PPS as binder.
Based on the experimental results including SEM images, XRD patterns (including pole figures) and magnetic properties, mechanisms for better alignment of the SmCo5, Sm2Co7 and Nd2Fe14B nanoscale chips milled in the magnetic field will now be described. When the milling process is carried out in a magnetic field, the chips are magnetized and formed chains with their surfaces perpendicular to magnetic field direction as seen in
In summary, anisotropic bonded magnets have been successfully fabricated by using the surfactant-assisted ball milling and magnetic field processing during the milling and aligning procedures. The structural and magnetic characterizations revealed that the hard magnetic SmCo and NdFeB chips obtained by surfactant-assisted milling in a magnetic field exhibit enhanced magnetic anisotropy compared to those milled without a magnetic field. A higher energy product up to 26 MGOe has been obtained for SmCo5 chips prepared in magnetic field compared to 23 MGOe without magnetic field with remanence of 0.96 and 0.91. The energy product above 13 MGOe has been obtained for anisotropic bonded magnets with density of 6.5 g/cm3 compacted in presence of a magnetic field. This combined technique shows promise for producing novel nanostructured anisotropic bulk magnets with enhanced magnetic properties.
Although the present invention and its advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims. Moreover, the scope of the present application is not intended to be limited to the particular embodiments of the process, machine, manufacture, composition of matter, means, methods and steps described in the specification, but only by the claims.
This invention was made with government support under Grant No. W911NF-08-1-0249 awarded by the U.S. Department of Defense/Defense Advanced Research Projects Agency/Army Research Office. The U.S. government has certain rights in the invention.
Filing Document | Filing Date | Country | Kind |
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PCT/US2013/053529 | 8/3/2013 | WO | 00 |
Number | Date | Country | |
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61679409 | Aug 2012 | US |