JP6332479B2 - 希土類永久磁石および希土類永久磁石の製造方法 - Google Patents
希土類永久磁石および希土類永久磁石の製造方法 Download PDFInfo
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Description
本形態の希土類永久磁石の製造方法は、本形態の作用効果を得られる限り、特に制限されない。好ましい本形態の製造方法としては、微粒子化工程、着磁工程、脱脂工程、熱処理工程とを含む製造方法が挙げられる。上記の各工程により得られた生成物を冷却工程で室温になるまで冷却させて、本形態の希土類永久磁石を製造できる。
微粒子化工程では、NdとPrとからなる群から一種以上選択される元素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、TbとSmとGdとHoとErとからなる群から一種以上選択される元素Aと、Feと、Bとを上記に説明する化学量論比で溶解させ、原料合金を得る。
着磁工程においては、得られた原料合金微粒子を配向磁場下で圧縮成型する。さらに熱処理工程で、得られた成形体を真空下で焼結後、焼結物を室温まで急冷する。続いて不活性ガス雰囲気中で時効処理し、室温まで冷却する。
熱処理工程においては、所定の温度管理と時間管理とにより主相や粒界相が形成される。熱処理条件は、含有成分の融点に基づいて決定される。すなわち処理温度を主相形成温度まで昇温させて保持することで全ての含有成分を溶解させる。その後、主相形成温度から粒界相形成温度まで温度を低下させる過程で主相成分が固相となり、粒界相成分が固相表面に析出し始める。粒界相形成温度で保持することにより粒界相を形成できる。
図3に示す組成で各元素を含有する原料合金をボールミルで粗粉砕し、合金粒子を得た。その後合金粒子を溶媒に分散させた。分散溶液に、添加剤を導入して撹拌して還元反応を行い、合金粒子を微粒子化した。
図3に示す組成で各元素を含有する原料合金から、急冷凝固装置により、比較例1の合金を得た。表1は、比較例1の合金のICP発光分光分析による中点の分析値である。
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°
図10に示す組成で各元素を含有する原料合金をボールミルで粗粉砕し、合金粒子を得た。その後合金粒子を溶媒に分散させた。分散溶液に、添加剤を導入して撹拌して還元反応を行い、合金粒子を微粒子化した。
実施例3と実施例5との希土類永久磁石の主相の結晶構造を観察するため、サンプル用に3DAP解析に用いる針状物を、下記の方法により加工した。まず実施例のサンプルは、集束イオンビーム加工観察装置(Forcused Ion Beam、FIB)にセットされた後、磁化容易方向を含む面を観察するための溝が加工された。溝を加工することで現れたサンプルの磁化容易方向を含む面に、電子線を照射した。照射により試料から放射される反射電子線をSEMで観察することで、主相(粒内)を特定した。特定された主相を、3DAPにより解析するため針状に加工した。
装置名 : 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
図10に示す組成で各元素を含有する原料合金から、急冷凝固装置により、比較例2を得た。表2は、比較例2の合金のICP発光分光分析による分析値である。
本形態は、Bの含有量を抑制しCoで置換させることで残留磁束密度Brを向上できる。残留磁束密度Brは飽和磁化と比例するため、本形態の飽和磁化を測定し、その測定結果から本形態の残留磁束密度Brの向上効果を確認した。
101 Fe層
102 R-Fe-B層
200 主相
300 粒界相
400 副相
Claims (6)
- NdとPrとからなる群から、Nb、又は、Nb及びPrが選択される元素Rと、
CoとBeとLiとAlとSiとからなる群から一種以上選択される元素Lと、
TbとSmとGdとHoとErとからなる群から一種以上選択される元素Aと、
Feと、
Bと、
を含有する主相を備える希土類永久磁石であって、
この主相はP4 2 /mnmに属する結晶を形成し、当該結晶において、前記元素Lが、前記結晶の4fサイトのB原子の一部を置換し、そして、前記結晶の4fサイトのNd原子と、前記結晶の4cサイトのFe原子と、前記結晶の8jサイトのFe原子とからなる群から二種以上選択される原子の一部を置換し、
前記主相と主相間に形成される粒界相と、前記主相と前記粒界相との境界である界面と、をさらに備え、前記粒界相の成分であるCuの含有量は、前記希土類永久磁石の総重量に対して、0.01〜0.1重量%であり、前記界面のCu濃度が前記粒界相のCu濃度と比較して高い、
希土類永久磁石。 - 主相間に形成される粒界相が、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をさらに含有する、
請求項1に記載される希土類永久磁石。 - 前記希土類永久磁石の総重量に対する前記元素Rの含有量が20〜35重量%であり、
Bの含有量が0.80〜0.99重量%であり、
CoとBeとLiとAlとSiとからなる群から一種以上選択される元素、及び、CuとNbとZrとTiとGaとからなる群から、少なくともCuを含めた二種以上が選択される元素の含有量の合計が、0.8〜2.0重量%であり、
TbとSmとGdとHoとErとからなる群から一種以上選択される前記元素Aの含有量の合計が2.0〜10.0重量%である、
請求項2に記載される希土類永久磁石。 - 粉末粒径のD50が2〜18μmである合金粒子を用いて製造された、
請求項1乃至3の何れか1項に記載される希土類永久磁石。 - 焼結密度が、6〜8g/cm3である、
請求項1乃至4の何れか1項に記載される希土類永久磁石。 - NdとPrとからなる群から、Nb、又は、Nb及びPrが選択される元素Rと、
CoとBeとLiとAlとSiとからなる群から一種以上選択される元素Lと、
CuとNbとZrとTiとGaとからなる群から、少なくともCuを含めた二種以上が選択される元素と、
TbとSmとGdとHoとErとからなる群から一種以上選択される元素Aと、
Feと、
Bと、
を含有する原料合金を、
第一の処理温度で保持し、前記第一の処理温度の保持時間経過後、処理温度を第二の処理温度まで低下させ、前記第二の処理温度で保持して、希土類永久磁石を製造する方法であって、
前記希土類永久磁石の主相にP42/mnmに属する結晶を形成し、当該結晶において、前記元素Lが、前記結晶の4fサイトのB原子の一部を置換し、そして、前記結晶の4fサイトのNd原子と、前記結晶の4cサイトのFe原子と、前記結晶の8jサイトのFe原子とからなる群から二種以上選択される原子の一部を置換するようにし、
前記主相と主相間に粒界相を形成し、
前記主相と前記粒界相との境界に界面を形成し、
前記粒界相成分であるCuの含有量を、前記希土類永久磁石の総重量に対して、0.01〜0.1重量%にし、
前記界面のCu濃度が前記粒界相のCu濃度と比較して高くなるようにした、
希土類永久磁石の製造方法。
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