JP6852351B2 - 希土類永久磁石の製造方法 - Google Patents
希土類永久磁石の製造方法 Download PDFInfo
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Description
本開示の希土類永久磁石の製造方法は、本開示の作用効果を得られる限り、特に制限されない。希土類永久磁石の製造方法に関する本開示の一形態は、炭素低減工程と、脱脂工程とを含む。炭素低減工程を設けることにより、主相に侵入する炭素量を低減できる。その結果、主相中の所定の原子を元素Lの原子で置換させやすくなる。
微粒子化工程の前段階として、原料合金を準備する。原料合金は、Ndを含む一種以上の希土類元素Rと、CoとBeとLiとAlとSiとCuとNbとZrとTiとGaとからなる群から一種以上選択される元素と、Feと、Bとをそれぞれ含有する原料金属を、上記の各元素が所定の化学量論比になるように仕込み、溶解させることで得られる。
磁場中成形工程では、得られた原料合金微粒子を配向磁場下で圧縮成型する。本工程は、磁場強度は0.8MA/m以上4.0MA/m以下、圧力1MPa以上200MPa以下で行うことが好ましい。バインダーとしては、本開示の作用効果を発揮する限り特に限定されないが、脂肪酸エステルを溶剤で希釈したものを例示できる。脂肪酸エステルとしては、カプロン酸メチル、カプリル酸メチル、ラウリン酸メチル、ラウリル酸メチルなどを例示できる。溶剤としては、イソパラフィンに代表される石油系溶剤やナフテン系溶剤などを例示できる。脂肪酸エステルと溶剤との混合例としては、1:20〜1:1の重量比での混合物が挙げられる。その他、脂肪酸として、アラキジン酸が1.0wt%以下で含まれていてもよい。また、液体潤滑剤に代え、あるいは液体潤滑剤と共にステアリン酸亜鉛のような固体潤滑剤も使用してもよい。
本開示は脱脂工程前に焼結炉外で脱気工程や乾燥工程を行うことにより、焼結工程前に脱脂工程だけを行う場合と比較して、圧粉体中の炭素量を低減できる。炭素量の低減は、脱気工程と乾燥工程とはいずれか一つを行っても実現できるが、両工程を行ってもよい。両工程を行う場合は、脱気工程後に乾燥工程を行うことが好ましい。炭素低減工程を行うことにより、希土類永久磁石中の炭素量が超微量になり、炭素量が希土類永久磁石の主相に侵入しやすい場合の炭素量よりも少なくなる。別言すれば、本開示は、炭素低減工程を行うことによりC原子が侵入し難くなるため、所定のB原子が元素Lの原子と置換しやすくなる。
乾燥工程では、密閉性の処理容器に圧粉体を載置し、処理容器内を低湿度環境にして圧粉体を保持する。脱気工程後に乾燥工程を行う場合は、脱気工程を実施した処理容器内で引き続き乾燥工程を実施してもよい。本開示において低湿度環境とは、露点-60℃以下、好ましくは-80℃以下、より好ましくは-110℃以下の雰囲気を意味する。保持時間は、6時間以上96時間以下が好ましく、24時間以上96時間以下がより好ましい。これにより、炭素量が低減され、かつ酸化し難い圧粉体を作製できる。保持時間が24時間未満の場合、酸化により特性が悪化することになる。また96時間を超えると、酸化により磁気特性が悪化することになる。
炭素低減工程の後、圧粉体を焼結炉に移し、脱脂工程を開始する。脱脂工程では、圧粉体全体を均一に脱脂するため、一段階または複数段階の温度管理を行い、焼結炉内の真空度を10Pa以下で、好ましくは10-2Pa以下で維持することが好ましい。これにより、炭素低減工程後に圧粉体に残存する炭素を一層低減でき、希土類永久磁石の主相を所望の元素分布を備える結晶構造にすることができる。
焼結工程は、脱脂工程後、焼結炉内に圧粉体を保持したまま、炉内温度を昇温して行う。焼結工程を行うことにより、本開示所定の希土類永久磁石の主相を形成できる。本開示は、圧粉体を焼結炉内に載置する前に上記の炭素低減工程を行う。これにより焼結炉内の真空度の推移にスパイク波形が発生し難い。すなわち焼結炉の炉内環境の安定性を維持して希土類永久磁石を製造できる。焼結工程および熱処理工程での焼結炉内の温度管理は、圧粉体の含有成分の融点に基づいて決定される。
熱処理工程は、焼結工程後、炉内温度を所定の熱処理温度に設定し行う。熱処理工程を行うことにより、本開示所定の希土類永久磁石の主相の周囲に粒界相や副相を析出させることができる。
実施例1ないし実施例4と比較例1ないし比較例3とを作製し、磁気性能を測定した。実施例1ないし実施例3と比較例1ないし比較例3とは、実施例1と比較例1とからなるセット1と、実施例2と比較例2からなるセット2と、実施例3と比較例3とからなるセット3とを構成する。実施例1と、比較例1と、実施例4とについては3DAPによる主相の元素分析と、Rietveld methodによる主相の結晶構造解析とを行った。
機器名 : LEAP3000XSi (AMETEK社製)
測定条件: レーザパルスモード(レーザ波長=532nm)
レーザパワー=0.5nJ、試料温度=50K
分析条件:
ターゲット:Cu
単色化:入射側に対称Johansson 型Ge 結晶を使用(CuKα1)
ターゲット出力:45kV-200mA
検出器:1次元検出器(HyPix3000)
(通常測定):θ/2θ走査
スリット入射系:発散1/2°
スリット受光系:20mm
走査速度:1°/min
サンプリング幅:0.01°
測定角度(2θ):10°〜110°
比較例4-1と比較例4-2とを作製した。比較例4-1と比較例4-2とは、実施例4と同じ仕込組成の原料合金を用いた。比較例4-1は、熱処理工程を行わなかった。しかし脱気工程と乾燥工程とを含む他の工程は、全て実施例4と同じ条件で行って作製した。比較例4-2は、脱気工程と乾燥工程と熱処理工程とを行わなかった。しかし、これらの工程以外は全ての工程を実施例4と同じ条件で行って作製した。
101 R-Fe-B層
102 Fe層
200 Co原子の第一の周期
201 Co原子の第一の周期の第一の変曲点
202 Co原子の第一の周期の第二の変曲点
203 Co原子の第一の周期の第三の変曲点(Co原子の第二の周期の第一の変曲点)
210 Co原子の第二の周期
211 Co原子の第二の周期の第一の変曲点
212 Co原子の第二の周期の第二の変曲点
213 Co原子の第二の周期の第三の変曲点
300 Nd原子の第一の周期
301 Nd原子の第一の周期の第一の変曲点
302 Nd原子の第一の周期の第二の変曲点
303 Nd原子の第一の周期の第三の変曲点(Nd原子の第二の周期の第一の変曲点)
310 Nd原子の第二の周期
311 Nd原子の第二の周期の第一の変曲点
312 Nd原子の第二の周期の第二の変曲点
313 Nd原子の第二の周期の第三の変曲点
Claims (4)
- Ndを含む一種以上の希土類元素Rと、CoとBeとLiとAlとSiとCuとNbとZrとTiとGaとからなる群から一種以上選択される元素と、BとFeと、を含有する原料合金の圧粉体を真空中で保持する脱脂工程と、前記脱脂工程前に前記圧粉体中の炭素量を低減する炭素低減工程とを含み、
前記炭素低減工程が、前記脱脂工程前に前記圧粉体を露点-60℃以下の雰囲気中で保持する乾燥工程を含み、
脱気工程の後に前記乾燥工程を行う、希土類永久磁石の製造方法。 - 前記脱気工程が、前記脱脂工程前に前記圧粉体を100℃以下で1時間以上保持する、請求項1に記載される希土類永久磁石の製造方法。
- 前記脱脂工程の後に前記圧粉体を焼結する焼結工程と、前記焼結工程で作製された焼結体を、焼結温度より低い温度で熱処理する熱処理工程とを含む、請求項1に記載される希土類永久磁石の製造方法。
- 前記希土類永久磁石が、主相を形成する結晶がP42/mnmに属し、前記結晶の4fサイトを占有するB原子の一部が元素Lの原子と置換され、Nd原子と元素Lの原子との分布がそれぞれ前記結晶のC軸方向に沿って複数の周期で現れ、元素Lの原子の周期とNdの原子の周期とが一致する領域を備える、ものである請求項3に記載の製造方法。
Priority Applications (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2016212359A JP6852351B2 (ja) | 2016-10-28 | 2016-10-28 | 希土類永久磁石の製造方法 |
PCT/JP2017/039015 WO2018079755A1 (ja) | 2016-10-28 | 2017-10-27 | 希土類永久磁石および希土類永久磁石の製造方法 |
EP17864421.7A EP3534381B1 (en) | 2016-10-28 | 2017-10-27 | Method for manufacturing rare-earth permanent magnet |
CN201780066952.5A CN109891524B (zh) | 2016-10-28 | 2017-10-27 | 稀土永磁体以及稀土永磁体的制造方法 |
AU2017351516A AU2017351516A1 (en) | 2016-10-28 | 2017-10-27 | Rare-earth permanent magnet and method for manufacturing rare-earth permanent magnet |
KR1020197015115A KR20190077021A (ko) | 2016-10-28 | 2017-10-27 | 희토류 영구자석 및 희토류 영구자석의 제조 방법 |
US16/345,270 US11264154B2 (en) | 2016-10-28 | 2017-10-27 | Rare earth permanent magnet and rare earth permanent magnet manufacturing method |
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KR (1) | KR20190077021A (ja) |
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CN111936029A (zh) | 2018-04-06 | 2020-11-13 | 松下i-PRO传感解决方案株式会社 | 相机模块、相机以及相机模块的电缆连接方法 |
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JP2960629B2 (ja) | 1992-06-24 | 1999-10-12 | 住友特殊金属株式会社 | 射出成形法によるR−Fe−B系焼結磁石の製造方法 |
JPH07201619A (ja) * | 1993-12-27 | 1995-08-04 | Sumitomo Special Metals Co Ltd | R−Fe−B系焼結異方性永久磁石の製造方法 |
JP3143396B2 (ja) * | 1996-06-28 | 2001-03-07 | 信越化学工業株式会社 | 焼結希土類磁石の製造方法 |
JP3728316B2 (ja) * | 2004-01-08 | 2005-12-21 | Tdk株式会社 | R−t−b系希土類永久磁石 |
US7199690B2 (en) * | 2003-03-27 | 2007-04-03 | Tdk Corporation | R-T-B system rare earth permanent magnet |
JP4879503B2 (ja) * | 2004-04-07 | 2012-02-22 | 昭和電工株式会社 | R−t−b系焼結磁石用合金塊、その製造法および磁石 |
JP4732459B2 (ja) * | 2005-08-08 | 2011-07-27 | 日立金属株式会社 | 希土類合金系バインダレス磁石およびその製造方法 |
US8152936B2 (en) | 2007-06-29 | 2012-04-10 | Tdk Corporation | Rare earth magnet |
JP5434869B2 (ja) * | 2009-11-25 | 2014-03-05 | Tdk株式会社 | 希土類焼結磁石の製造方法 |
CN103231059B (zh) * | 2013-05-05 | 2015-08-12 | 沈阳中北真空磁电科技有限公司 | 一种钕铁硼稀土永磁器件的制造方法 |
US10388442B2 (en) * | 2013-08-12 | 2019-08-20 | Hitachi Metals, Ltd. | R-T-B based sintered magnet and method for producing R-T-B based sintered magnet |
CN109887697B (zh) | 2013-11-05 | 2021-07-20 | 株式会社Ihi | 稀土永磁材料以及稀土永磁材料的制造方法 |
CN103996521B (zh) * | 2014-05-11 | 2016-05-25 | 沈阳中北通磁科技股份有限公司 | 一种钕铁硼稀土永磁体的真空预烧结方法和设备 |
CN103996520B (zh) * | 2014-05-11 | 2016-10-05 | 沈阳中北通磁科技股份有限公司 | 一种钕铁硼稀土永磁体的烧结方法和设备 |
CN103996517B (zh) * | 2014-05-11 | 2016-10-05 | 沈阳中北通磁科技股份有限公司 | 一种钕铁硼稀土永磁材料的半自动成型方法 |
KR20180025844A (ko) | 2015-04-30 | 2018-03-09 | 가부시키가이샤 아이에이치아이 | 희토류 영구 자석 및 희토류 영구 자석의 제조 방법 |
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JP2018074004A (ja) | 2018-05-10 |
US11264154B2 (en) | 2022-03-01 |
KR20190077021A (ko) | 2019-07-02 |
EP3534381A1 (en) | 2019-09-04 |
CN109891524A (zh) | 2019-06-14 |
CN109891524B (zh) | 2021-07-23 |
US20190295753A1 (en) | 2019-09-26 |
AU2017351516A1 (en) | 2019-05-23 |
WO2018079755A1 (ja) | 2018-05-03 |
EP3534381B1 (en) | 2023-12-06 |
EP3534381A4 (en) | 2020-07-08 |
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