JP2013138170A - 希土類焼結磁石 - Google Patents
希土類焼結磁石 Download PDFInfo
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- 150000001875 compounds Chemical class 0.000 description 5
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- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 description 2
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- -1 which are LR Inorganic materials 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
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Abstract
【解決手段】本発明に係る希土類焼結磁石は、R−T−B(RはY及び希土類元素から選ばれる1種以上の元素、TはFe又はFe及びCoを含む1種以上の金属元素、BはB又はB及びC)系の組成を有する希土類永久磁石であり、粒界3重点において原子比で(Fe+Co)/(LR+HR+Fe+Co)≦0.2(LRはY及び57Laから63Euまでの軽希土類元素、HRは64Gdから71Luまでの重希土類元素)であるRリッチ相(Rは希土類元素)が存在する時、前記Rリッチ相中にHR/(LR+HR)≧0.01(原子比)の領域が存在し、前記HR/(LR+HR)≧0.01の領域が粒界3重点に占める面積比が10%から90%である。
【選択図】図1
Description
本実施形態の希土類焼結磁石は、R−T−B系合金を用いて形成される焼結体である。
本実施形態に係る希土類焼結磁石は、主相(結晶粒)がR2Fe14B相と、主相よりRが多い粒界相と、3つ以上の主相によって囲まれた粒界3重点とを含む。該粒界3重点には原子比で(Fe+Co)/(LR+HR+Fe+Co)≦0.2であるRリッチ相が存在し、より好ましくは(Fe+Co)/(LR+HR+Fe+Co)≦0.1であることが望ましい。(Fe+Co)/(LR+HR+Fe+Co)>0.2である場合、粒界3重点にRに富んだFe及び/又はCoからなる磁性相が形成されることで、個々の主相同士の磁気的分離が十分でなくなり、保磁力HcJを低下させるおそれがある。(Fe+Co)/(LR+HR+Fe+Co)が0を含まないのは、Rリッチ相がFe及び/又はCoを不可避に含有しているためである。
上記で示した構成を有する希土類焼結磁石の好適な製造方法について図面を用いて説明する。
[実施例1]
ストリップキャスト法により表1に示す組成を有する磁石を、表1に記載した組成の第1合金1及び第2合金1を用いて作製した。第2合金にはDy−Cu系の組成を持った合金を選択した。第1合金1及び第2合金1からなる混合物に室温で水素吸蔵処理を施した後に、Ar雰囲気中にて600℃で1時間、脱水素処理を行って第1合金1及び第2合金1を粗粉砕した。粗粉砕した第1合金1及び第2合金1に、粉砕助剤としてオレイン酸アミドを粗粉砕粉に対し0.05質量%添加し、ジェットミルにて微粉砕を行って平均粒径が4.0μmの微粉を得た。得られた第1合金粉末及び第2合金粉末を、質量比が99.7対0.3となるように低酸素雰囲気で混合し、混合粉末を得た。得られた混合粉末を、印加磁場が1.2MA/m、成形圧力が120MPaとして磁場中で成形し、成形体を得た。得られた成形体は、真空中において1040℃で4時間保持し、焼結した。その後、Ar雰囲気中で時効処理を行い、焼結体を得た。時効処理は、550℃で1.5時間保持して行った。
実施例2から4及び比較例1、2は、第1合金1に類似した組成の第1合金2から第1合金4及び第1合金10と第1合金11を使用したことと、合金粉末の混合質量比を変更した以外は、実施例1と同様に行い焼結体を得た。第1合金2から第1合金4及び第1合金10と第1合金11及び第2合金1の組成とその混合比と得られたNd−Fe−B系焼結磁石の磁石組成とを表2から表6に示す。
実施例5から実施例7及び比較例3は、第1合金1に類似した組成の第1合金5から第1合金7、第1合金12を使用して、実施例1とは異なる磁石組成にしたこと以外は、実施例1と同様に行い焼結体を得た。第1合金5から第1合金7、第1合金12及び第2合金1の組成とその混合比と得られたNd−Fe−B系焼結磁石の磁石組成とを各々表7から表10に示す。
実施例8及び実施例9は、第1合金4を使用したことと、第2合金1とは組成の異なる第2合金2及び第2合金3を使用して、実施例4とは異なる磁石組成にしたこと以外は、実施例4と同様に行い焼結体を得た。第1合金4及び第2合金2及び第2合金3の組成とその混合比と得られたNd−Fe−B系焼結磁石の磁石組成とを各々表11及び表12に示す。
実施例10は、第1合金1の組成のうちNdをPrに、DyをTbに変更した第1合金8を使用したことと、第2合金1の組成のうちDyをTbに変更した第2合金4を使用したこと以外は、実施例1と同様に行い焼結体を得た。第1合金8及び第2合金4の組成とその混合比と得られたNd−Fe−B系焼結磁石の磁石組成とを表13に示す。
実施例11及び比較例4から比較例6は、第1合金1に類似した組成の第1合金9及び第1合金13から第1合金15を使用したことと、第2合金1とは組成の異なる第2合金5から第2合金8使用したこと以外は、実施例1と同様に行い焼結体を得た。第1合金9及び第1合金13から第1合金15及び第2合金5から第2合金8の組成とその混合比と得られたNd−Fe−B系焼結磁石の磁石組成とを表14から表17に示す。
比較例7は、実施例1に用いた第1合金1に類似した組成の第1合金16を使用したことと、第2合金を用いていないこと以外は、実施例1と同様に行い焼結体を得た。第1合金16及び得られたNd−Fe−B系焼結磁石の磁石組成を表18に示す。
(STEM−EDS及びEPMA)
実施例1から実施例11の希土類焼結磁石及び比較例1から比較例7の希土類焼結磁石について、STEM−EDS(走査透過型電子顕微鏡−エネルギー分散型X線分光器)を用いて粒界3重点の組織観察及び元素マッピングを行った。各々の実施例及び比較例に対し、LRであるNd及びPrとHRであるDy及びTbの元素マッピングによりRリッチ相を特定し、Rリッチ相の点分析を行い、Rリッチ相中での原子数換算での組成比(Fe+Co)/(LR+HR+Fe+Co)及びHR/(LR+HR)を算出した。実施例1から実施例11及び比較例1から比較例7の点分析結果によるRリッチ相中での原子比(Fe+Co)/(LR+HR+Fe+Co)及びHR/(LR+HR)を表20に示す。また、前述の組成分析及びマッピング結果を元に、組成比が(Fe+Co)/(LR+HR+Fe+Co)≦0.2かつHR/(LR+HR)≧0.01を満たすRリッチ相の面積が粒界3重点の面積に占める割合を百分率で面積比とし、表20に併せて示す。更に、実施例1から実施例11の希土類焼結磁石及び比較例1から比較例7の希土類焼結磁石について、EPMA(電子線マイクロアナライザー)を用いて、磁石表層から100μm離れた25μm×25μmの視野において元素マッピングを行った。実施例1から実施例11及び比較例1から比較例7の元素マッピング結果から、HRであるDy及びTbの検出信号のCV値(全分析点の標準偏差を全分析点の算術平均で割った値)を算出した結果を同じく表20に示す。
[耐食性及び磁気特性の評価]
5体積%硝酸−エタノール溶液を用いて希土類焼結磁石の表面を2分間エッチングした試料を、PCT(プレッシャークッカー試験)用試験機を用いて120℃、2atm、100%RHの条件下で腐食させ、磁石の表面の腐食物を除去し、希土類焼結磁石の質量減少率を求めた試験結果を図3に示す。また、実施例1から実施例11及び比較例1から比較例7による各希土類焼結磁石の磁気特性を、BHトレーサーにより測定を行った。測定された各希土類焼結磁石の残留磁束密度Br及び保磁力HcJを、表21に示す。
2.・・・粒界3重点
3・・・粒界相
4・・・Rリッチ相
5・・・HRリッチ相
Claims (4)
- R−T−B(RはY及び希土類元素から選ばれる1種以上の元素、TはFe又はFe及びCoを含む1種以上の金属元素、BはB又はB及びC)系の組成を有する希土類永久磁石であって、
粒界3重点において原子比で(Fe+Co)/(LR+HR+Fe+Co)≦0.2(LRはY及び57Laから63Euまでの軽希土類元素から選ばれる1種以上の元素、HRは64Gdから71Luまでの重希土類元素から選ばれる1種以上の元素)であるRリッチ相が存在し、当該Rリッチ相中にHR/(LR+HR)≧0.01(原子比)の領域が存在し、該領域の粒界3重点に占める面積比が10%から90%である希土類焼結磁石。 - 10〜100μm×10〜100μmの視野においてEPMAで観察した際に、磁石の表層50μmを除いた視野のHRの検出信号のCV値(全分析点の標準偏差を全分析点の算術平均値で割った値)が、0.15〜0.5である請求項1に記載の希土類焼結磁石。
- LRは少なくともNd又はPrを含み、HRは少なくともDy又はTbを含む請求項1及び2に記載の希土類焼結磁石。
- Rの含有量が25質量%以上35質量%以下、Bの含有量が0.9質量%以上1.1質量%以下、残部が実質的にTの組成を有する請求項1及び2に記載の希土類焼結磁石。
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CN106086418A (zh) * | 2016-06-30 | 2016-11-09 | 江西省钨与稀土产品质量监督检验中心(江西省钨与稀土研究院) | 一种烧结钕铁硼废旧器件性能恢复的方法 |
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JP6555170B2 (ja) * | 2015-03-31 | 2019-08-07 | 信越化学工業株式会社 | R−Fe−B系焼結磁石及びその製造方法 |
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