JP5059929B2 - 磁石用粉末 - Google Patents
磁石用粉末 Download PDFInfo
- Publication number
- JP5059929B2 JP5059929B2 JP2010253753A JP2010253753A JP5059929B2 JP 5059929 B2 JP5059929 B2 JP 5059929B2 JP 2010253753 A JP2010253753 A JP 2010253753A JP 2010253753 A JP2010253753 A JP 2010253753A JP 5059929 B2 JP5059929 B2 JP 5059929B2
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- JP
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- Prior art keywords
- rare earth
- iron
- powder
- magnet
- alloy material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000843 powder Substances 0.000 title claims description 309
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 320
- 239000000956 alloy Substances 0.000 claims description 189
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 163
- 229910052742 iron Inorganic materials 0.000 claims description 140
- 239000000463 material Substances 0.000 claims description 85
- 229910052739 hydrogen Inorganic materials 0.000 claims description 78
- 239000001257 hydrogen Substances 0.000 claims description 78
- 239000006249 magnetic particle Substances 0.000 claims description 76
- 238000010438 heat treatment Methods 0.000 claims description 75
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 75
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 71
- 229910045601 alloy Inorganic materials 0.000 claims description 67
- 150000002910 rare earth metals Chemical class 0.000 claims description 66
- -1 hydrogen compound Chemical class 0.000 claims description 65
- 239000012298 atmosphere Substances 0.000 claims description 64
- 229910052757 nitrogen Inorganic materials 0.000 claims description 59
- 238000004519 manufacturing process Methods 0.000 claims description 44
- 239000002245 particle Substances 0.000 claims description 43
- 238000005121 nitriding Methods 0.000 claims description 36
- 239000001301 oxygen Substances 0.000 claims description 35
- 229910052760 oxygen Inorganic materials 0.000 claims description 35
- 239000002994 raw material Substances 0.000 claims description 35
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 34
- 229910001199 N alloy Inorganic materials 0.000 claims description 33
- 230000035699 permeability Effects 0.000 claims description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 22
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- 238000005984 hydrogenation reaction Methods 0.000 claims description 22
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 21
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- 150000001875 compounds Chemical class 0.000 claims description 12
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- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
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- 229910001172 neodymium magnet Inorganic materials 0.000 description 4
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- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 2
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
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- 238000004438 BET method Methods 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910017135 Fe—O Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
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- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910007991 Si-N Inorganic materials 0.000 description 1
- 229910006294 Si—N Inorganic materials 0.000 description 1
- 229910052768 actinide Inorganic materials 0.000 description 1
- 150000001255 actinides Chemical class 0.000 description 1
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- 238000004458 analytical method Methods 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
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- 230000001186 cumulative effect Effects 0.000 description 1
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- 238000011049 filling Methods 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 229910001337 iron nitride Inorganic materials 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
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- 239000004800 polyvinyl chloride Substances 0.000 description 1
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- 239000002244 precipitate Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1078—Alloys containing non-metals by internal oxidation of material in solid state
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
- C22C33/0228—Using a mixture of prealloyed powders or a master alloy comprising other non-metallic compounds or more than 5% of graphite
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
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- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
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- H01F1/047—Alloys characterised by their composition
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- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/0551—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0552—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 in the form of particles, e.g. rapid quenched powders or ribbon flakes with a protective layer
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- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
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- H01F1/0553—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 obtained by reduction or by hydrogen decrepitation or embrittlement
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
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- H01F1/053—Alloys characterised by their composition containing rare earth metals
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- H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
- H01F1/0556—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together pressed
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/059—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2
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- H—ELECTRICITY
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Description
準備工程:添加元素に希土類元素を含有する希土類-鉄系合金からなる合金粉末を準備する工程。
水素化工程:上記希土類-鉄系合金粉末を、水素元素を含む雰囲気中、上記希土類-鉄系合金の不均化温度以上の温度で熱処理して、以下の磁性粒子から構成される磁石用粉末を形成する工程。
上記各磁性粒子は、40体積%未満の希土類元素の水素化合物と残部がFeを含む鉄含有物とからなり、上記希土類元素の水素化合物の相と上記鉄含有物の相とが隣接して存在しており、かつ上記鉄含有物の相を介して隣り合う上記希土類元素の水素化合物の相間の間隔が3μm以下である。
[磁石用粉末]
本発明磁石用粉末を構成する各磁性粒子は、主成分を鉄含有物とし、その含有量を60体積%以上とする。鉄含有物の含有量が60体積%未満であると、硬質である希土類元素の水素化合物が相対的に多くなって、圧縮成形時、鉄含有物を十分に変形することが難しく、多過ぎると最終的に磁石特性の低下を招くことから90体積%以下が好ましい。
本発明粉末は、酸化し易い希土類元素を含有することから、例えば、大気雰囲気などの酸素を含む雰囲気で圧縮成形を行うと、圧縮により各磁性粒子に形成された新生面が酸化され、生成された酸化物の存在により、最終的に得られる磁石中の磁性相の割合の低下を招く恐れがある。これに対して、各磁性粒子の全周を覆うように上述した酸化防止層を具える形態とすると、各磁性粒子が雰囲気中の酸素と十分に遮断されて、上記磁性粒子の新生面の酸化を防止できる。この効果を得るためには、酸化防止層の酸素の透過係数(30℃)が小さいほど好ましく、1.0×10-11m3・m/(s・m2・Pa)未満、特に0.01×10-11m3・m/(s・m2・Pa)以下が好ましく、下限は設けない。
更に、上記本発明磁石用粉末は、各磁性粒子の外周に絶縁材料からなる絶縁被覆を具える形態とすることができる。絶縁被覆を具える粉末を用いることで、電気抵抗が高い希土類磁石が得られ、例えば、この磁石をモータに利用した場合、渦電流損を低減できる。絶縁被覆は、例えば、Si,Al,Tiなどの酸化物の結晶性被膜や非晶質のガラス被膜、Me-Fe-O(Me=Ba,Sr,Ni,Mnなどの金属元素)といったフェライトやマグネタイト(Fe3O4)、Dy2O3といった金属酸化物、シリコーン樹脂といった樹脂、シルセスキオキサン化合物などといった酸化物からなる被膜が挙げられる。また、熱伝導性を向上する目的で、Si-N、Si-C系のセラミックス被覆を施してもよい。上記結晶性被膜やガラス被膜、酸化物被膜、セラミックス被膜などは、酸化防止機能を有する場合があり、この場合、磁性粒子の酸化を防止できる。また、上述した酸化防止層に加えて上記酸化防止機能を有する被膜を具えることで、磁性粒子の酸化をより防止することができる。
≪準備工程≫
上記磁石用粉末の原料となる希土類-鉄系合金(例えば、Sm2Fe17,Sm1Fe11Ti1)からなる粉末は、例えば、所望の希土類-鉄系合金からなる溶解鋳造インゴットや急冷凝固法で得られる箔状体をジョークラッシャー、ジェットミルやボールミルなどの粉砕装置により粉砕したり、ガスアトマイズ法といったアトマイズ法を利用することで製造することができる。特に、ガスアトマイズ法を利用する場合、非酸化性雰囲気で粉末を形成することで、実質的に酸素が含有されない粉末(酸素濃度:500質量ppm以下)とすることができる。即ち、希土類-鉄系合金からなる粉末を構成する粒子中の酸素濃度が500質量ppm以下であることは、非酸化性雰囲気のガスアトマイズ法により製造された粉末であることを示す指標の一つとなり得る。上記希土類-鉄系合金からなる粉末の製造には、公知の製造方法を利用してもよいし、アトマイズ法により製造した粉末を更に粉砕してもよい。粉砕条件や製造条件を適宜変更することで、磁石用粉末の粒度分布や粒子の形状を調整することができる。例えば、アトマイズ法を利用すると、真球度が高く、成形時の充填性に優れた粉末を製造し易い。上記希土類-鉄系合金粉末を構成する各粒子は多結晶体でも単結晶体でもよい。多結晶体からなる粒子に適宜熱処理を加えて単結晶体からなる粒子とすることができる。
水素化工程において、上記水素元素を含む雰囲気は、水素(H2)のみの単一雰囲気、或いは水素(H2)とArやN2といった不活性ガスとの混合雰囲気が挙げられる。上記水素化工程の熱処理時の温度は、上記希土類-鉄系合金の不均化反応が進行する温度、即ち不均化温度以上とする。不均化反応とは、希土類元素の優先水素化により、希土類水素化合物と、Fe(或いはFe及び鉄化合物)とに分離する反応であり、この反応が生じる下限温度を不均化温度と呼ぶ。上記不均化温度は、上記希土類-鉄系合金の組成や希土類元素の種類により異なる。例えば、希土類-鉄系合金がSm2Fe17,Sm1Fe11Ti1の場合、600℃以上が挙げられる。水素化熱処理時の温度を不均化温度近傍とすると、上述した層状形態が得られ易く、当該温度を不均化温度+100℃以上に高めると、上述した粒状形態が得られ易い。上記水素化工程の熱処理時の温度を高めることで、Fe相のマトリックス化が進行するため、Feと同時に析出する硬質の希土類元素の水素化物が変形の阻害因子になり難くなり磁石用粉末の成形性を高められるが、高過ぎると粉末の溶融固着などの不具合が発生するため、この温度は1100℃以下が好ましい。特に、希土類-鉄系合金がSm2Fe17,Sm1Fe11Ti1の場合、上記水素化工程の熱処理時の温度を700℃以上900℃以下の比較的低めにすると、上記間隔が小さい微細な組織となり、このような粉末を利用することで保磁力が高い希土類磁石が得られ易い。保持時間は、0.5時間以上5時間以下が挙げられる。この熱処理は、上述したHDDR処理の不均化工程までの処理に相当し、公知の不均化条件を適用することができる。
上記各磁性粒子の表面に酸化防止層を具える形態とする場合、上記水素化工程により得られた各磁性粒子に酸化防止層を形成する。酸化防止層の形成には、乾式法及び湿式法のいずれもが利用できる。乾式法では、上記磁性粒子が雰囲気中の酸素に接触して表面が酸化することを防止するために、非酸化性雰囲気、例えば、ArやN2などの不活性雰囲気、減圧雰囲気などとすることが好ましい。湿式法では、上記磁性粒子の表面が雰囲気中の酸素に実質的に接触しないため、上述の不活性雰囲気などとする必要が無く、例えば、大気雰囲気で酸化防止層を形成できる。従って、湿式法は、酸化防止層の形成の作業性に優れる上に、上記磁性粒子の表面に酸化防止層を均一的な厚さに形成し易く好ましい。
上記本発明磁石用粉末を圧縮成形することで、本発明粉末成形体が得られる。上述のように本発明粉末は、成形性に優れることから相対密度(粉末成形体の真密度に対する実際の密度)が高い粉末成形体、例えば、相対密度が85%以上のものが得られる。相対密度が高いほど、最終的に磁性相の比率を高められる。但し、上記酸化防止層を具える形態において、当該酸化防止層の構成成分を窒化処理などの熱処理工程や、別途除去のための熱処理工程で焼失させる場合、相対密度が高過ぎると、上記酸化防止層の構成成分を十分に焼失させることが難しい。従って、酸化防止層を具える粉末を用いて粉末成形体を形成する場合、粉末成形体の相対密度は、90%〜95%程度が好ましいと考えられる。粉末成形体の相対密度を高める場合は、酸化防止層の厚さを薄めにしたり、別途熱処理(被覆除去)を行うと、酸化防止層を除去し易く好ましい。酸化防止層を有していない粉末を用いて粉末成形体を形成する場合、粉末成形体の相対密度の上限は特に設けない。
脱水素工程では、上記磁性粒子と反応せず、かつ水素を効率よく除去できるように非水素雰囲気にて熱処理を行う。非水素雰囲気には、不活性雰囲気や減圧雰囲気が挙げられる。不活性雰囲気は、例えば、ArやN2が挙げられる。減圧雰囲気は、標準の大気雰囲気よりも圧力を低下させた真空状態を言い、最終真空度は、10Pa以下が好ましい。減圧雰囲気で希土類元素の水素化合物から水素の除去を行うと、希土類元素の水素化合物が残存し難く、希土類-鉄系合金化を完全に起こさせることができる。従って、得られた希土類-鉄系合金材を素材とすることで、磁気特性に優れる希土類磁石が得られる。
窒化工程において窒素元素を含む雰囲気は、窒素(N2)のみの単一雰囲気、或いはアンモニア(NH3)雰囲気、或いは窒素(N2)やアンモニアとArといった不活性ガスとの混合ガスの雰囲気が挙げられる。上記窒化工程の熱処理時の温度は、上記希土類-鉄系合金が当該合金として窒素元素と反応する温度(窒化温度)以上、窒素不均化温度(鉄含有物と希土類元素とがそれぞれ分離・独立して、窒素元素と反応する温度)以下とする。上記窒化温度や窒素不均化温度は、上記希土類-鉄系合金の組成により異なる。例えば、希土類-鉄系合金がSm2Fe17,Sm1Fe11Ti1の場合、上記窒化処理時の温度は、200℃以上550℃以下(好ましくは300℃以上)が挙げられる。保持時間は、10分以上600分以下が挙げられる。特に、希土類-鉄系合金がSm1Fe11Ti1の場合、窒化処理を安定して、かつ希土類-鉄系合金材の全体に亘って均一的に窒化することができる。
上記本発明希土類-鉄-窒素系合金材を適宜着磁することで、希土類磁石を製造することができる。特に、上述した相対密度が高い粉末成形体を利用することで、磁性相の比率が80体積%以上、更に90体積%以上といった希土類磁石が得られる。
希土類元素と鉄元素とを含む粉末を種々作製し、得られた粉末を圧縮成形して、各粉末の成形性を調べた。
試験例1と同様にして希土類磁石を作製し、磁石特性を調べた。
希土類元素と鉄元素とを含む粉末を作製し、得られた粉末を圧縮成形して、粉末の成形性、酸化状態を調べた。この試験では、上記粉末を構成する磁性粒子の外周に酸化防止層を具えるものを作製した。
4 粉末成形体 5 希土類-鉄系合金材 6 希土類-鉄-窒素系合金材
7 希土類磁石
10 酸化防止層 11 酸素低透過層 12 湿気低透過層
Claims (21)
- 希土類磁石に用いられる磁石用粉末であって、
前記磁石用粉末を構成する各磁性粒子は、
40体積%未満の希土類元素の水素化合物と、残部がFeを含む鉄含有物とからなり、
前記希土類元素の水素化合物の相と前記鉄含有物の相とが隣接して存在しており、
前記鉄含有物の相を介して隣り合う前記希土類元素の水素化合物の相間の間隔が3μm以下であることを特徴とする磁石用粉末。 - 前記希土類元素は、Smであることを特徴とする請求項1に記載の磁石用粉末。
- 前記希土類元素の水素化合物の相は、粒状であり、
前記鉄含有物の相中に、前記粒状の希土類元素の水素化合物が分散して存在することを特徴とする請求項1又は2に記載の磁石用粉末。 - 前記希土類元素は、Smであり、
前記鉄含有物は、FeとFeTi化合物とを含有することを特徴とする請求項1〜3のいずれか1項に記載の磁石用粉末。 - 前記磁性粒子の外周に酸素の透過係数(30℃)が1.0×10-11m3・m/(s・m2・Pa)未満である酸化防止層を具えることを特徴とする請求項1〜4のいずれか1項に記載の磁石用粉末。
- 前記酸化防止層は、酸素の透過係数(30℃)が1.0×10-11m3・m/(s・m2・Pa)未満である材料から構成された酸素低透過層と、透湿率(30℃)が1000×10-13kg/(m・s・MPa)未満である材料から構成された湿気低透過層とを具えることを特徴とする請求項5に記載の磁石用粉末。
- 前記磁性粒子の平均粒径が10μm以上500μm以下であることを特徴とする請求項1〜6のいずれか1項に記載の磁石用粉末。
- 前記鉄含有物は、希土類元素とは独立的に存在することを特徴とする請求項1〜7のいずれか1項に記載の磁石用粉末。
- 希土類磁石の原料に用いられ、
請求項1〜8のいずれか1項に記載の磁石用粉末を圧縮成形して製造され、相対密度が85%以上であることを特徴とする粉末成形体。 - 希土類磁石の原料に用いられ、
請求項4に記載の磁石用粉末を圧縮成形して製造され、相対密度が90%以上であることを特徴とする粉末成形体。 - 希土類磁石の原料に用いられ、
請求項9又は10に記載の粉末成形体を不活性雰囲気中、又は減圧雰囲気中で熱処理して製造されたことを特徴とする希土類-鉄系合金材。 - 前記熱処理の前の粉末成形体と、前記熱処理の後の希土類-鉄系合金材との体積変化率が5%以下であることを特徴とする請求項11に記載の希土類-鉄系合金材。
- 希土類磁石の原料に用いられ、
請求項11又は12に記載の希土類-鉄系合金材を窒素元素を含む雰囲気中で熱処理して製造されたことを特徴とする希土類-鉄-窒素系合金材。 - 前記希土類-鉄-窒素系合金材を構成する希土類-鉄-窒素系合金は、Sm-Fe-Ti-N合金であることを特徴とする請求項13に記載の希土類-鉄-窒素系合金材。
- 前記熱処理の前の希土類-鉄系合金材と、前記熱処理の後の希土類-鉄-窒素系合金材との体積変化率が5%以下であることを特徴とする請求項13又は14に記載の希土類-鉄-窒素系合金材。
- 希土類磁石に用いられる磁石用粉末を製造する磁石用粉末の製造方法であって、
添加元素に希土類元素を含有する希土類-鉄系合金からなる合金粉末を準備する準備工程と、
前記希土類-鉄系合金粉末を、水素元素を含む雰囲気中、前記希土類-鉄系合金の不均化温度以上の温度で熱処理して、40体積%未満の希土類元素の水素化合物と残部がFeを含む鉄含有物とからなり、前記希土類元素の水素化合物の相と前記鉄含有物の相とが隣接して存在しており、かつ前記鉄含有物の相を介して隣り合う前記希土類元素の水素化合物の相間の間隔が3μm以下である磁性粒子から構成される磁石用粉末を形成する水素化工程とを具えることを特徴とする磁石用粉末の製造方法。 - 前記希土類-鉄系合金は、Sm-Fe-Ti合金であることを特徴とする請求項16に記載の磁石用粉末の製造方法。
- 前記鉄含有物は、希土類元素とは独立的に存在することを特徴とする請求項16又は17に記載の磁石用粉末の製造方法。
- 希土類磁石に用いられる希土類-鉄系合金材を製造する希土類-鉄系合金材の製造方法であって、
請求項16〜18のいずれか1項に記載の磁石用粉末の製造方法により得られた磁石用粉末を圧縮成形して、相対密度が85%以上である粉末成形体を成形する成形工程と、
前記粉末成形体を不活性雰囲気中、又は減圧雰囲気中で、当該粉末成形体の再結合温度以上の温度で熱処理して、前記希土類-鉄系合金材を形成する脱水素工程とを具えることを特徴とする希土類-鉄系合金材の製造方法。 - 希土類磁石に用いられる希土類-鉄-窒素系合金材を製造する希土類-鉄-窒素系合金材の製造方法であって、
請求項19に記載の希土類-鉄系合金材の製造方法により得られた希土類-鉄系合金材を窒素元素を含む雰囲気中、前記希土類-鉄系合金の窒化温度以上窒素不均化温度以下の温度で熱処理して、希土類-鉄-窒素系合金材を形成する窒化工程を具えることを特徴とする希土類-鉄-窒素系合金材の製造方法。 - 前記窒化工程は、100MPa以上の加圧下で行うことを特徴とする請求項20に記載の希土類-鉄-窒素系合金材の製造方法。
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