JP5640946B2 - 希土類磁石前駆体である焼結体の製造方法 - Google Patents
希土類磁石前駆体である焼結体の製造方法 Download PDFInfo
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Description
図1a、1b、1cはこの順に、急冷リボンの製造、次いでこの急冷リボンを粉砕してなる磁性粉末を用いた焼結体の製造、次いでこの焼結体に熱間塑性加工を施してなる成形体の製造というフロー図になっている。図1aは急冷リボンの製造方法を説明する図であり、図2は急冷速度に応じた急冷リボンの組織を説明した図であって、図2aは急冷速度が107K/s程度の速度で製造された場合の組織図、図2bは106〜107K/sの速度で製造された場合の組織図、図2cは105〜106K/sの速度で製造された場合の組織図、図2dは105よりも遅い速度で製造された場合の組織図をそれぞれ示している。
図1bは焼結体の製造方法を説明した図である。製造された磁性粉末pを図1bで示すように超硬ダイスDとこの中空内を摺動する超硬パンチPで画成されたキャビティ内に充填し、超硬パンチPで加圧しながら(X方向)加圧方向に電流を流して通電加熱することにより、ナノ結晶組織のNd-Fe-B系の主相(20nm〜200nm程度の粒径範囲の結晶粒)と、主相の周りにあるNd-X合金(X:金属元素)等の粒界相からなる焼結体Sが製造される。
図1cは成形体の製造方法を説明した図である。製造された焼結体Sをその長手方向(図1bでは水平方向が長手方向)の端面に超硬パンチPを当接させ、超硬パンチPで加圧しながら(X方向)熱間塑性加工(強加工)を施すことにより、磁気的異方性を有するナノ結晶粒からなる結晶組織の成形体Cが製造される。
本発明者等は、以下の方法で実施例1〜3の成形体と比較例の成形体を製作し、各成形体の前駆体である焼結体のTEM画像から結晶方位を解析してc軸方向の短辺長さの平均値を短辺t1とし、c軸方向に直交するa軸方向の長辺長さの平均値を長辺t2として双方のアスペクト比を測定し、さらに、それぞれの成形体の配向度をVSM(試料振動型磁化測定装置)を使用して測定した。以下、実施例1〜3と比較例の製作方法を説明するとともに、各焼結体のアスペクト比と成形体の配向度に関する実験結果を表1と図7に示す。また、実施例2、3と比較例のSEM画像図、TEM画像を図6に示す。
片側冷却により、粗大粒を含有しないNd13.64Pr0.19Fe75.66Co4.47B5.47Ga0.57(mass%)組成の急冷粉を作製し、粉砕した後、磁気分離によって非晶質と結晶質に分離した。次に、非晶質の磁性粉末のみを集め、温度650℃、30分間熱処理を実施した後に、400MPa印加し、620℃、5分間保持して焼結体を製作した。TEMにて焼結体の組織観察を実施した後に、温度780℃、歪速度:8/sで熱間塑性加工を実施して実施例1の成形体を製作した。
片側冷却により、粗大粒を含有しないNd13.64Pr0.19Fe75.66Co4.47B5.47Ga0.57(mass%)組成の急冷粉を作製し、粉砕した後、磁気分離によって非晶質と結晶質に分離した。次に、結晶質の磁性粉末のみを集め、400MPa印加し、620℃、5分間保持して焼結体を製作した。TEMにて焼結体の組織観察を実施した後に、温度780℃、歪速度:8/sで熱間塑性加工を実施して実施例2の成形体を製作した。
片側冷却により、粗大粒を含有しないNd16Fe77.4B5.4Ga0.5Al0.5Cu0.2(at%)組成の急冷粉を作製し、粉砕した後、磁気分離によって非晶質と結晶質に分離した。次に、非晶質の磁性粉末のみを集め、温度575℃、30分間熱処理を実施した後に、300MPa印加し、570℃、5分間保持して焼結体を製作した。TEMにて焼結体の組織観察を実施した後に、温度650℃、歪速度0.02/sで熱間塑性加工を実施して実施例3の成形体を製作した。
片側冷却により、粗大粒を含有しないNd16Fe77.4B5.4Ga0.5Al0.5Cu0.2(at%)組成の急冷粉を作製し、粉砕した後、磁気分離によって非晶質と結晶質に分離した。次に、非晶質の磁性粉末のみを集め、300MPa印加し、570℃、5分間保持して焼結体を製作した。TEMにて焼結体の組織観察を実施した後に、温度650℃、歪速度0.1/sで熱間塑性加工を実施して比較例の成形体を製作した。
Claims (1)
- ナノ結晶組織のNd-Fe-B系の主相である結晶粒と、該主相の周りにある粒界相からなる焼結体であって、該焼結体に異方性を与える熱間塑性加工が施され、さらに保磁力を向上させる合金が拡散されて形成される希土類磁石の前駆体である焼結体において、焼結体を構成する前記結晶粒は、容易磁化方向(c軸方向)に直交する方向から見た結晶粒の平面形状がc軸方向の辺とこれに直交する方向(a軸方向)の辺からなる長方形もしくはこれに近似した形状となっている、希土類磁石前駆体である焼結体の製造方法であって、
結晶粒の前記平面形状において、c軸方向の辺長をt1、a軸方向の辺長をt2とした際に、アスペクト比t2/t1が1.4≦t2/t1≦10の範囲にあり、前記t1、t2が20nm以上200nm以下の範囲となるように調整しながら磁性粉末を以下のいずれかの方法で製造する第1のステップ、
(1)Nd-Fe-B系の金属溶湯を冷却ロール表面に吐出し、急冷速度が105〜106K/sの範囲で液体急冷して金属溶湯を凝固させて結晶質のみの急冷リボンを製造し、これを粉砕して磁性粉末を製造する、
(2)Nd-Fe-B系の金属溶湯を冷却ロール表面に吐出し、急冷速度が105〜106K/sの範囲外で液体急冷して金属溶湯を凝固させて非晶質を一部に含む急冷リボンを製造し、次いで該急冷リボンを500〜800℃で熱処理をおこなって結晶質のみの急冷リボンを製造し、これを粉砕して磁性粉末を製造する、
次に、製造された磁性粉末を加圧および加熱して焼結体を製造する第2のステップからなる希土類磁石前駆体である焼結体の製造方法。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2011224071A JP5640946B2 (ja) | 2011-10-11 | 2011-10-11 | 希土類磁石前駆体である焼結体の製造方法 |
EP12840239.3A EP2767987A4 (en) | 2011-10-11 | 2012-10-09 | SINTERING BODY FROM A RARE MOLDING PROCESSOR AND METHOD FOR PRODUCING A FINE MAGNETIC POWDER FOR PRODUCING THE SINTERED BODY |
US14/350,418 US20140238553A1 (en) | 2011-10-11 | 2012-10-09 | Sintered body that is precursor of rare-earth magnet, and method for producing magnetic powder for forming the same |
PCT/JP2012/076066 WO2013054779A1 (ja) | 2011-10-11 | 2012-10-09 | 希土類磁石前駆体の焼結体とこれを形成する磁性粉末の製造方法 |
CN201280049369.0A CN103875044A (zh) | 2011-10-11 | 2012-10-09 | 作为稀土类磁铁前驱体的烧结体和形成该烧结体的磁性粉末的制造方法 |
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DE102012216668A1 (de) * | 2012-09-18 | 2014-03-20 | Siemens Aktiengesellschaft | Verfahren zum Herstellen eines anisotropen Magneten und anisotroper Magnet |
JP6238444B2 (ja) * | 2013-01-07 | 2017-11-29 | 昭和電工株式会社 | R−t−b系希土類焼結磁石、r−t−b系希土類焼結磁石用合金およびその製造方法 |
JP5924335B2 (ja) | 2013-12-26 | 2016-05-25 | トヨタ自動車株式会社 | 希土類磁石とその製造方法 |
JP5983598B2 (ja) * | 2013-12-27 | 2016-08-31 | トヨタ自動車株式会社 | 希土類磁石の製造方法 |
JP6221978B2 (ja) * | 2014-07-25 | 2017-11-01 | トヨタ自動車株式会社 | 希土類磁石の製造方法 |
JP2016076614A (ja) * | 2014-10-07 | 2016-05-12 | トヨタ自動車株式会社 | 希土類磁石の製造方法 |
JP6358085B2 (ja) * | 2014-12-26 | 2018-07-18 | トヨタ自動車株式会社 | 希土類磁石の磁気性能の特定方法 |
EP3625807B1 (en) * | 2017-05-19 | 2021-03-24 | Robert Bosch GmbH | Hot deformed magnet, and a method for preparing said hot deformed magnet |
CN111599561B (zh) * | 2019-02-21 | 2021-12-14 | 有研稀土新材料股份有限公司 | 一种钕铁硼磁体及其制备方法 |
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CA1269029A (en) * | 1986-01-29 | 1990-05-15 | Peter Vernia | Permanent magnet manufacture from very low coercivity crystalline rare earth-transition metal-boron alloy |
US4867809A (en) * | 1988-04-28 | 1989-09-19 | General Motors Corporation | Method for making flakes of RE-Fe-B type magnetically aligned material |
JP2596835B2 (ja) * | 1989-08-04 | 1997-04-02 | 新日本製鐵株式会社 | 希土類系異方性粉末および希土類系異方性磁石 |
JP2001319821A (ja) * | 2000-05-10 | 2001-11-16 | Sumitomo Special Metals Co Ltd | 鉄基合金磁石の製造方法および製造装置 |
JP2003243209A (ja) * | 2002-02-14 | 2003-08-29 | Asahi Kasei Corp | 磁性固形材料とその製造方法 |
CN100480412C (zh) * | 2006-05-23 | 2009-04-22 | 钢铁研究总院 | 单织构RE-Fe-B磁性化合物速凝带及其制备方法 |
JP5504832B2 (ja) | 2009-11-06 | 2014-05-28 | トヨタ自動車株式会社 | ナノコンポジット磁石の製造方法 |
JP5093215B2 (ja) * | 2009-11-26 | 2012-12-12 | トヨタ自動車株式会社 | 焼結希土類磁石の製造方法 |
JP5163630B2 (ja) * | 2009-12-18 | 2013-03-13 | トヨタ自動車株式会社 | 希土類磁石およびその製造方法 |
JP2011159733A (ja) * | 2010-01-29 | 2011-08-18 | Toyota Motor Corp | ナノコンポジット磁石の製造方法 |
JP5691989B2 (ja) * | 2011-10-11 | 2015-04-01 | トヨタ自動車株式会社 | 希土類磁石前駆体の焼結体を形成する磁性粉体の製造方法 |
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- 2012-10-09 WO PCT/JP2012/076066 patent/WO2013054779A1/ja active Application Filing
- 2012-10-09 CN CN201280049369.0A patent/CN103875044A/zh active Pending
- 2012-10-09 EP EP12840239.3A patent/EP2767987A4/en not_active Withdrawn
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EP2767987A4 (en) | 2015-06-03 |
CN103875044A (zh) | 2014-06-18 |
EP2767987A1 (en) | 2014-08-20 |
US20140238553A1 (en) | 2014-08-28 |
WO2013054779A1 (ja) | 2013-04-18 |
JP2013084802A (ja) | 2013-05-09 |
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