JP2014093391A - 希土類磁石とその製造方法 - Google Patents
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 79
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 76
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 33
- 239000006247 magnetic powder Substances 0.000 claims abstract description 33
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 29
- 239000000956 alloy Substances 0.000 claims abstract description 29
- 230000005415 magnetization Effects 0.000 claims abstract description 27
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 23
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 16
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 15
- 238000012545 processing Methods 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 9
- 229910052742 iron Inorganic materials 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 description 28
- 239000013078 crystal Substances 0.000 description 10
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 10
- 229910000881 Cu alloy Inorganic materials 0.000 description 8
- 230000005496 eutectics Effects 0.000 description 7
- 229910001172 neodymium magnet Inorganic materials 0.000 description 7
- 229910000838 Al alloy Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 230000004907 flux Effects 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 5
- 238000000731 high angular annular dark-field scanning transmission electron microscopy Methods 0.000 description 5
- 230000007423 decrease Effects 0.000 description 4
- 229910052733 gallium Inorganic materials 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- 229910020598 Co Fe Inorganic materials 0.000 description 2
- 229910002519 Co-Fe Inorganic materials 0.000 description 2
- 229910000946 Y alloy Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 239000011796 hollow space material Substances 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
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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
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0576—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together pressed, e.g. hot working
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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
- B22F3/12—Both compacting and sintering
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- 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
- C22C1/04—Making non-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
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0266—Moulding; Pressing
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0273—Imparting anisotropy
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- Crystallography & Structural Chemistry (AREA)
- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
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Abstract
【解決手段】希土類磁石材料となる磁粉Bであって、RE-Fe-B系の主相MP(RE:NdおよびPr)と、主相MPの周りにあるRE-X合金(X:金属元素)の粒界相BPからなり、主相MPの平均粒径が10nm〜200nmの範囲にある磁粉Bを加圧成形して成形体Sを製造する第1のステップ、成形体Sに異方性を与える熱間塑性加工を施してナノ結晶磁石である希土類磁石Cを製造する第2のステップからなり、磁粉Bに含まれるNd、B、Co、Pr含有量がat%表示でNd:25〜35、B:0.5〜1.5、Co:2〜7と、さらにPrが0.2〜5at%とFeからなる。
【選択図】図5
Description
図1a、bはその順で本発明の希土類磁石の製造方法の第1のステップを説明した模式図であり、図2は第1のステップで製造された成形体のミクロ構造を説明した図である。また、図3は本発明の製造方法の第2のステップを説明した模式図である。
本発明者等は、希土類磁石の合金組成中のPr量の最適な範囲を特定するための実験をおこなった。この実験では、以下の方法で合金組成の異なる複数の磁粉を使用して希土類磁石の試験体を作成し、各試験体の磁気特性を測定した。
Nd-Fe-B系の粉末を溶湯温度1450℃、3000rpmで回転したCuロールにて急冷して作成した後(液体急冷法)、不活性雰囲気中で乳鉢ですり潰すように粉砕して磁石用の磁粉とした。この磁石用の磁粉の合金組成はat%表示で、Nd30-xCo4B1Prx(x:0、0.1、0.2、0.4、1、3.5、10、14.9、29.8)Ga0.5FeBal.であり、主相の平均粒径は10nm〜200nmである。
各試験片の磁気特性評価に関し、50℃での保磁力と残留磁化は、試料振動型磁力計(VSM)を用いて測定した。また、配高度は、パルス励磁型磁気特性測定装置(TPM)を用いて測定し、6Tにおける残留磁束密度/飽和磁化とした。測定結果を以下の表2と図5に示す。
本発明者等はさらに、Prの微量添加が保磁力を低下させずに高配向化(高い残留磁化)できる理由を考察するべく、製造された希土類磁石のHAADF-STEM像を観察するとともに、STEM-EDX(エネルギー分散型X線分析)を実施した。図6はHAADF-STEM像とSTEM-EDX(エネルギー分散型X線分析)結果を示した図であり、図7はHAADF-STEM像と主相のSTEM-EDX結果(上)と粒界相のSTEM-EDX結果(下)を示した図である。
Claims (3)
- 希土類磁石材料となる磁粉であって、RE-Fe-B系の主相(RE:NdおよびPr)と、該主相の周りにあるRE-X合金(X:金属元素)の粒界相からなり、主相の平均粒径が10nm〜200nmの範囲にある磁粉を加圧成形して成形体を製造する第1のステップ、
成形体に異方性を与える熱間塑性加工を施してナノ結晶磁石である希土類磁石を製造する第2のステップからなり、
前記磁粉に含まれるNd、B、Co、Pr含有量がat%表示でNd:25〜35、B:0.5〜1.5、Co:2〜7と、さらにPrが0.2〜5at%とFeからなる希土類磁石の製造方法。 - 前記第2のステップの熱間塑性加工は、熱処理が600〜850℃の温度範囲、歪速度が10-3〜10(/sec)の範囲、加工率50%以上でおこない、製造されるナノ結晶磁石の主相の平均粒径を50nm〜1000nmの範囲に成長させる請求項1に記載の希土類磁石の製造方法。
- RE-Fe-B系の主相(RE:NdおよびPr)と、該主相の周りにあるRE-X合金(X:金属元素)の粒界相からなり、
主相の平均粒径が50nm〜1000nmの範囲にあり、
前記磁粉に含まれるNd、B、Co、Pr含有量がat%表示でNd:25〜35、Pr:0.2〜5、B:0.5〜1.5、Co:2〜7、Fe:bal.であり、
150℃における保磁力が5.7kOe(453kA/m)以上であり、かつ、残留磁化が1.38T以上である、ナノ結晶磁石からなる希土類磁石。
Priority Applications (6)
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JP2012242528A JP5751237B2 (ja) | 2012-11-02 | 2012-11-02 | 希土類磁石とその製造方法 |
DE112013005248.2T DE112013005248T5 (de) | 2012-11-02 | 2013-10-08 | Seltenerdmagnet und Verfahren zur Herstellung desselben |
US14/437,898 US20150279529A1 (en) | 2012-11-02 | 2013-10-08 | Rare earth magnet and method for producing same |
CN201380057221.6A CN104798150B (zh) | 2012-11-02 | 2013-10-08 | 稀土类磁铁及其制造方法 |
KR1020157009792A KR101740165B1 (ko) | 2012-11-02 | 2013-10-08 | 희토류 자석과 그 제조 방법 |
PCT/JP2013/077310 WO2014069181A1 (ja) | 2012-11-02 | 2013-10-08 | 希土類磁石とその製造方法 |
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JP2012242528A JP5751237B2 (ja) | 2012-11-02 | 2012-11-02 | 希土類磁石とその製造方法 |
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JP2014093391A true JP2014093391A (ja) | 2014-05-19 |
JP5751237B2 JP5751237B2 (ja) | 2015-07-22 |
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US (1) | US20150279529A1 (ja) |
JP (1) | JP5751237B2 (ja) |
KR (1) | KR101740165B1 (ja) |
CN (1) | CN104798150B (ja) |
DE (1) | DE112013005248T5 (ja) |
WO (1) | WO2014069181A1 (ja) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2016034024A (ja) * | 2014-07-29 | 2016-03-10 | 日立金属株式会社 | R−t−b系焼結磁石の製造方法 |
CN107077935A (zh) * | 2014-12-08 | 2017-08-18 | Lg电子株式会社 | 包含非磁性合金的热压变形的磁体及其制造方法 |
Families Citing this family (8)
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JP5725200B2 (ja) | 2011-11-14 | 2015-05-27 | トヨタ自動車株式会社 | 希土類磁石 |
JP5790617B2 (ja) | 2012-10-18 | 2015-10-07 | トヨタ自動車株式会社 | 希土類磁石の製造方法 |
CN105518809B (zh) | 2013-06-05 | 2018-11-20 | 丰田自动车株式会社 | 稀土磁体及其制造方法 |
JP6003920B2 (ja) | 2014-02-12 | 2016-10-05 | トヨタ自動車株式会社 | 希土類磁石の製造方法 |
US10079084B1 (en) | 2014-11-06 | 2018-09-18 | Ford Global Technologies, Llc | Fine-grained Nd—Fe—B magnets having high coercivity and energy density |
CN104575906B (zh) * | 2014-12-11 | 2017-05-24 | 赣州市东磁稀土有限公司 | 一种高性能低成本稀土永磁材料及其制备方法 |
CN115244206B (zh) * | 2020-03-12 | 2024-08-09 | 株式会社村田制作所 | 铁基稀土类硼系各向同性磁铁合金 |
CN115430836B (zh) * | 2022-08-24 | 2023-11-17 | 广东省科学院资源利用与稀土开发研究所 | 一种高丰度稀土铈基各向异性纳米晶磁体的制备方法和装置 |
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- 2013-10-08 WO PCT/JP2013/077310 patent/WO2014069181A1/ja active Application Filing
- 2013-10-08 CN CN201380057221.6A patent/CN104798150B/zh not_active Expired - Fee Related
- 2013-10-08 US US14/437,898 patent/US20150279529A1/en not_active Abandoned
- 2013-10-08 DE DE112013005248.2T patent/DE112013005248T5/de active Pending
- 2013-10-08 KR KR1020157009792A patent/KR101740165B1/ko active IP Right Grant
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Cited By (3)
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JP2016034024A (ja) * | 2014-07-29 | 2016-03-10 | 日立金属株式会社 | R−t−b系焼結磁石の製造方法 |
CN107077935A (zh) * | 2014-12-08 | 2017-08-18 | Lg电子株式会社 | 包含非磁性合金的热压变形的磁体及其制造方法 |
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WO2014069181A1 (ja) | 2014-05-08 |
CN104798150A (zh) | 2015-07-22 |
DE112013005248T5 (de) | 2015-10-08 |
KR20150056832A (ko) | 2015-05-27 |
CN104798150B (zh) | 2017-03-22 |
JP5751237B2 (ja) | 2015-07-22 |
KR101740165B1 (ko) | 2017-05-25 |
US20150279529A1 (en) | 2015-10-01 |
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