JP5983598B2 - 希土類磁石の製造方法 - Google Patents
希土類磁石の製造方法 Download PDFInfo
- Publication number
- JP5983598B2 JP5983598B2 JP2013271985A JP2013271985A JP5983598B2 JP 5983598 B2 JP5983598 B2 JP 5983598B2 JP 2013271985 A JP2013271985 A JP 2013271985A JP 2013271985 A JP2013271985 A JP 2013271985A JP 5983598 B2 JP5983598 B2 JP 5983598B2
- Authority
- JP
- Japan
- Prior art keywords
- rare earth
- sintered body
- earth magnet
- powder
- ppm
- 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.)
- Expired - Fee Related
Links
- 229910052761 rare earth metal Inorganic materials 0.000 title claims description 64
- 150000002910 rare earth metals Chemical class 0.000 title claims description 60
- 238000004519 manufacturing process Methods 0.000 title claims description 39
- 239000000843 powder Substances 0.000 claims description 50
- 238000005121 nitriding Methods 0.000 claims description 34
- 239000013078 crystal Substances 0.000 claims description 31
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 19
- 229910045601 alloy Inorganic materials 0.000 claims description 16
- 239000000956 alloy Substances 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 13
- 229910052779 Neodymium Inorganic materials 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 238000010791 quenching Methods 0.000 claims description 6
- 230000000171 quenching effect Effects 0.000 claims description 6
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 2
- 239000012071 phase Substances 0.000 description 28
- 238000012545 processing Methods 0.000 description 28
- 238000001125 extrusion Methods 0.000 description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 24
- 239000007791 liquid phase Substances 0.000 description 23
- 230000005415 magnetization Effects 0.000 description 18
- 238000000034 method Methods 0.000 description 14
- 238000009825 accumulation Methods 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 12
- 238000012360 testing method Methods 0.000 description 11
- 239000012298 atmosphere Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 230000001965 increasing effect Effects 0.000 description 7
- 239000002159 nanocrystal Substances 0.000 description 7
- 238000005242 forging Methods 0.000 description 6
- 230000006872 improvement Effects 0.000 description 5
- 239000000696 magnetic material Substances 0.000 description 5
- 229910001172 neodymium magnet Inorganic materials 0.000 description 5
- 238000003672 processing method Methods 0.000 description 5
- 229910000838 Al alloy Inorganic materials 0.000 description 4
- 229910000881 Cu alloy Inorganic materials 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000005496 eutectics Effects 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910020598 Co Fe Inorganic materials 0.000 description 1
- 229910002519 Co-Fe Inorganic materials 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000010304 firing Methods 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
- 239000000314 lubricant Substances 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
-
- 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
- H01F1/0577—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 sintered
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Description
図1aは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1bは第2のステップを説明した模式図であり、図2は図1bで示す焼結体のミクロ構造を説明した図である。また、図3は図1bに続いて第3のステップを説明した図であり、図4は製造された希土類磁石のミクロ構造を説明した図である。
本発明者等は、磁石材料粉末の窒化量を変化させて希土類磁石を製作し、各希土類磁石の残留磁化を測定するとともに、粉末における窒化量なしの希土類磁石の残留磁化を基準として他の希土類磁石の残留磁化の増加量を求め、窒化量と残留磁化の増加量の関係を特定する実験をおこなった。
試験体となる希土類磁石の製作方法は次の通りである。まず、磁石原料(合金組成は、質量%で、Fe-30Nd-0.93B-4Co-0.4Ga)を所定量配合し、Ar雰囲気中で溶解した後、その溶湯をφ0.8mmのオリフィスからCrめっきを施したCu製の回転ロールに射出して急冷し、急冷薄帯を製作した。この急冷薄帯をAr雰囲気中でカッターミルで粉砕篩し、0.3mm以下の磁石材料となる粉末を得た。
図5に実験結果を示す。同図より、窒化量1000ppmで変曲点を迎え、1000ppm未満で残留磁化の増加量が急激に少なくなる一方、1000ppm以上の範囲では残留磁化増加量が0.1T程度でサチュレートし、3000pmでは試験体の液相硬化に伴う変形能低下により、後方押出加工時に多数の割れが発生し、磁気特性の確認ができなかった。
また、この実験では、窒素雰囲気保持時間と磁石材料粉末の窒化量の関係も特定している。具体的には、窒素雰囲気の際の窒素濃度97kPaの下で、保持時間を0、1、2、3、5、10分保持した際の窒化量を測定した。その結果を図6に示す。
さらに、この実験では、磁石材料粉末の窒化量が2000ppmの試験体の組織と200ppmの試験体の組織をSEM観察した。ここで、図7a、図7bはともに磁石材料粉末の窒化量が2000ppmの試験体の組織を観察したSEM写真図であり、図7aは10000倍の写真図であり、図7bは50000倍の写真図である。また、図8a、図8bはともに磁石材料粉末の窒化量が200ppmの試験体の組織を観察したSEM写真図であり、図8aは10000倍の写真図であり、図8bは50000倍の写真図である。
本発明者等はさらに、既に述べた実験にて製作した試験体の前駆体である焼結体のうち、粉末の窒化量が2000ppmの焼結体と200ppmの焼結体を選定し、以下3種の熱間塑性加工をそれぞれの焼結体に実施して希土類磁石を製造し、各希土類磁石の残留磁化を測定し、窒化量200ppmの試験体の残留磁化に対する窒化量2000ppmの試験体の残留磁化の増加量を特定する実験をおこなった。
Claims (2)
- 液体急冷にて微細な結晶粒である急冷薄帯を製作し、これを粉砕して、希土類磁石材料となる粉末であって、RE-Fe-B系の主相(RE:Nd、Prの少なくとも一種)と、該主相の周りにあるRE-X合金(X:金属元素)の粒界相からなる希土類磁石用の粉末を製作する第1のステップ、
前記希土類磁石用の粉末を加圧成形して焼結体を製造する第2のステップ、
前記焼結体に異方性を与える熱間塑性加工を施して希土類磁石を製造する第3のステップからなり、
第1のステップもしくは第2のステップの少なくともいずれか一方のステップを窒素雰囲気下でおこない、前記粉末の窒化量を1000ppm以上で3000ppm未満の範囲に調整する希土類磁石の製造方法。 - 第1のステップにおいて粉砕後の粉末の粒径は75μm〜300μmの範囲にあり、第2のステップにおいて焼結体を構成する主相の平均粒径は300nm以下である請求項1に記載の希土類磁石の製造方法。
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2013271985A JP5983598B2 (ja) | 2013-12-27 | 2013-12-27 | 希土類磁石の製造方法 |
PCT/IB2014/002839 WO2015097524A1 (en) | 2013-12-27 | 2014-12-19 | Method of manufacturing rare earth magnet |
US15/107,631 US10192679B2 (en) | 2013-12-27 | 2014-12-19 | Method of manufacturing rare earth magnet |
DE112014006035.6T DE112014006035T5 (de) | 2013-12-27 | 2014-12-19 | Verfahren zur Herstellung eines Seltene-Erden-Magneten |
CN201480070837.1A CN105849829B (zh) | 2013-12-27 | 2014-12-19 | 制造稀土磁体的方法 |
KR1020167016870A KR101813427B1 (ko) | 2013-12-27 | 2014-12-19 | 희토류 자석의 제조 방법 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2013271985A JP5983598B2 (ja) | 2013-12-27 | 2013-12-27 | 希土類磁石の製造方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2015126213A JP2015126213A (ja) | 2015-07-06 |
JP5983598B2 true JP5983598B2 (ja) | 2016-08-31 |
Family
ID=52462949
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2013271985A Expired - Fee Related JP5983598B2 (ja) | 2013-12-27 | 2013-12-27 | 希土類磁石の製造方法 |
Country Status (6)
Country | Link |
---|---|
US (1) | US10192679B2 (ja) |
JP (1) | JP5983598B2 (ja) |
KR (1) | KR101813427B1 (ja) |
CN (1) | CN105849829B (ja) |
DE (1) | DE112014006035T5 (ja) |
WO (1) | WO2015097524A1 (ja) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP6451529B2 (ja) * | 2015-07-07 | 2019-01-16 | トヨタ自動車株式会社 | 高周波誘導加熱方法 |
CN106887294B (zh) * | 2017-03-10 | 2020-05-22 | 钢铁研究总院 | 多硬磁主相辐向取向无缝稀土永磁环及低温成型方法 |
WO2022039552A1 (ko) * | 2020-08-20 | 2022-02-24 | 한국재료연구원 | 다상 구조 자석의 제조방법 및 그로부터 제조된 다상 구조 자석 |
JP2022098987A (ja) | 2020-12-22 | 2022-07-04 | Tdk株式会社 | R‐t‐b系永久磁石 |
Family Cites Families (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2001267163A (ja) * | 2000-03-21 | 2001-09-28 | Sumitomo Special Metals Co Ltd | 希土類磁石の製造方法および焼結用台板 |
JP3294841B2 (ja) * | 2000-09-19 | 2002-06-24 | 住友特殊金属株式会社 | 希土類磁石およびその製造方法 |
JP2004250781A (ja) * | 2002-10-08 | 2004-09-09 | Neomax Co Ltd | 焼結型永久磁石およびその製造方法 |
JP3683260B2 (ja) * | 2003-06-27 | 2005-08-17 | Tdk株式会社 | 希土類永久磁石 |
JP5328161B2 (ja) * | 2008-01-11 | 2013-10-30 | インターメタリックス株式会社 | NdFeB焼結磁石の製造方法及びNdFeB焼結磁石 |
JP5413383B2 (ja) * | 2011-02-23 | 2014-02-12 | トヨタ自動車株式会社 | 希土類磁石の製造方法 |
JP5640946B2 (ja) * | 2011-10-11 | 2014-12-17 | トヨタ自動車株式会社 | 希土類磁石前駆体である焼結体の製造方法 |
JP5969750B2 (ja) | 2011-10-14 | 2016-08-17 | 日東電工株式会社 | 希土類永久磁石の製造方法 |
JP5640954B2 (ja) * | 2011-11-14 | 2014-12-17 | トヨタ自動車株式会社 | 希土類磁石の製造方法 |
-
2013
- 2013-12-27 JP JP2013271985A patent/JP5983598B2/ja not_active Expired - Fee Related
-
2014
- 2014-12-19 DE DE112014006035.6T patent/DE112014006035T5/de not_active Withdrawn
- 2014-12-19 KR KR1020167016870A patent/KR101813427B1/ko active IP Right Grant
- 2014-12-19 CN CN201480070837.1A patent/CN105849829B/zh not_active Expired - Fee Related
- 2014-12-19 WO PCT/IB2014/002839 patent/WO2015097524A1/en active Application Filing
- 2014-12-19 US US15/107,631 patent/US10192679B2/en active Active
Also Published As
Publication number | Publication date |
---|---|
KR101813427B1 (ko) | 2017-12-28 |
KR20160089485A (ko) | 2016-07-27 |
JP2015126213A (ja) | 2015-07-06 |
WO2015097524A1 (en) | 2015-07-02 |
US20160336112A1 (en) | 2016-11-17 |
CN105849829A (zh) | 2016-08-10 |
DE112014006035T5 (de) | 2016-09-15 |
CN105849829B (zh) | 2018-06-22 |
US10192679B2 (en) | 2019-01-29 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
KR101661416B1 (ko) | 희토류 자석의 제조 방법 | |
CA2887984C (en) | Rare-earth magnet production method | |
JP5790617B2 (ja) | 希土類磁石の製造方法 | |
JP5413383B2 (ja) | 希土類磁石の製造方法 | |
US10347418B2 (en) | Method of manufacturing rare earth magnet | |
JP2013149862A (ja) | 希土類磁石の製造方法 | |
JP5708242B2 (ja) | 希土類磁石の製造方法 | |
JP6471669B2 (ja) | R−t−b系磁石の製造方法 | |
JP5983598B2 (ja) | 希土類磁石の製造方法 | |
JP6274068B2 (ja) | 希土類磁石の製造方法 | |
KR101664726B1 (ko) | 희토류 자석의 제조 방법 | |
JP5757234B2 (ja) | 希土類磁石用の急冷リボンの製造方法 | |
JP6691666B2 (ja) | R−t−b系磁石の製造方法 | |
JP6691667B2 (ja) | R−t−b系磁石の製造方法 | |
JP6313202B2 (ja) | 希土類磁石の製造方法 | |
EP3007192A1 (en) | Method for manufacturing rare-earth magnets | |
US20190311851A1 (en) | Method of producing nd-fe-b magnet | |
JP2015123463A (ja) | 前方押出し鍛造装置と前方押出し鍛造方法 | |
JP2013138111A (ja) | 希土類磁石の製造方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20150925 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20151104 |
|
TRDD | Decision of grant or rejection written | ||
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20160705 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20160718 |
|
R151 | Written notification of patent or utility model registration |
Ref document number: 5983598 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R151 |
|
LAPS | Cancellation because of no payment of annual fees |