JP6414598B2 - R−t−b系焼結磁石の製造方法 - Google Patents
R−t−b系焼結磁石の製造方法 Download PDFInfo
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Description
まず、本発明では、重希土類元素RHの拡散の対象とするR−T−B系焼結磁石母材を準備する。なお、本明細書では、わかりやすさのため、重希土類元素RHの拡散の対象とするR−T−B系焼結磁石をR−T−B系焼結磁石母材と厳密に称することがあるが、「R−T−B系焼結磁石」の用語はそのような「R−T−B系焼結磁石母材」を含むものとする。このR−T−B系焼結磁石母材は公知のものが使用でき、例えば以下の組成を有する。
希土類元素R:12〜17原子%
B(B(ボロン)の一部はC(カーボン)で置換されていてもよい):5〜8原子%
添加元素M´(Al、Ti、V、Cr、Mn、Ni、Cu、Zn、Ga、Zr、Nb、Mo、Ag、In、Sn、Hf、Ta、W、Pb、およびBiからなる群から選択された少なくとも1種):0〜2原子%
T(Feを主とする遷移金属元素であって、Coを含んでもよい)および不可避不純物:残部
ここで、希土類元素Rは、主として軽希土類元素RL(Ndおよび/またはPr)であるが、重希土類元素を含有していてもよい。なお、重希土類元素を含有する場合は、重希土類元素RHであるDyおよびTbの少なくとも一方を含むことが好ましい。
拡散助剤としては、アトマイズ法で作製されたRLM合金の粉末を用いる。RLとしてはRH化合物を還元する効果の高い軽希土類元素が適しており、RLはNdおよび/またはPrとする。またMはCu、Fe、Ga、Co、Ni、Alから選ばれる1種以上の元素とする。中でもNd−Cu合金やNd−Al合金を用いると、NdによるRH化合物の還元能力が効果的に発揮され、HcJの向上効果がより高いので好ましい。また、RLM合金はRLを50原子%以上含み、かつ、その融点が熱処理温度以下の合金を用いる。RLM合金はRLを65原子%以上含むことが好ましい。RLの含有割合が50原子%以上のRLM合金は、RLがRH化合物を還元する能力が高く、かつ、融点が熱処理温度以下であるので熱処理時に溶融してRH化合物を効率よく還元し、より高い割合で還元されたRHがR−T−B系焼結磁石中に拡散して少量でも効率よくR−T−B系焼結磁石のHcJを向上させることができる。
拡散剤としては、RH化合物(RHはDyおよび/またはTb、RH化合物はRHフッ化物、RH酸化物、RH酸フッ化物から選ばれる1種以上)の粉末を用いる。RH化合物粉末はRLM合金粉末よりも質量比率で等しいか少ないため、RH化合物粉末を均一に塗布するには、RH化合物粉末の粒度が小さいことが好ましい。本発明者の検討によれば、RH化合物の粉末の粒度は凝集した2次粒子の大きさにおいて20μm以下が好ましく、10μm以下がより好ましい。小さいものは1次粒子で数μm程度である。
拡散剤と拡散助剤をR−T−B系焼結磁石表面に存在させる方法は特に限定されず、どのような方法であってもよいが、例えば、R−T−B系焼結磁石表面に、RLM合金粉末とRH化合物粉末の混合粉末とバインダおよび/または溶媒を混合して作製したスラリーを塗布する方法などであってもよい。本発明のRLM合金粉末はアトマイズ法で作製された球状粉末であるので非常に流動性に優れ、均一な塗布層を形成することができる。スラリーを塗布する方法については、例えば、ノズルからR−T−B系焼結磁石表面にスラリーを注出することによって塗布する方法や、スクリーンメッシュを通して塗布する方法などがあげられる。
RLM合金の粉末とRH化合物の粉末とをR−T−B系焼結磁石の表面に存在させた状態で熱処理を行う。なお、熱処理の開始後、RLM合金の粉末は溶融するため、RLM合金が熱処理中に常に「粉末」の状態を維持する必要は無い。熱処理の雰囲気は真空または不活性ガス雰囲気が好ましい。熱処理温度はR−T−B系焼結磁石の焼結温度以下(具体的には例えば1000℃以下)であり、かつ、RLM合金の融点よりも高い温度である。熱処理時間は例えば10分〜72時間である。また前記熱処理の後必要に応じてさらに400〜700℃で10分〜72時間の熱処理を行ってもよい。
まず、公知の方法で、組成比Nd=13.4、B=5.8、Al=0.5、Cu=0.1、Co=1.1、残部=Fe(原子%)のR−T−B系焼結磁石を作製した。これを機械加工することにより、6.9mm×7.4mm×7.4mmのR−T−B系焼結磁石母材を得た。得られたR−T−B系焼結磁石母材の磁気特性をB−Hトレーサーによって測定したところ、HcJは1035kA/m、Brは1.45Tであった。なお、後述の通り、熱処理後のR−T−B系焼結磁石の磁気特性は、R−T−B系焼結磁石の表面を機械加工にて除去してから測定するので、R−T−B系焼結磁石母材もそれに合わせて、表面をさらにそれぞれ0.2mmずつ機械加工にて除去し、大きさ6.5mm×7.0mm×7.0mmとしてから測定した。なお、別途R−T−B系焼結磁石母材の不純物量をガス分析装置によって測定したところ、酸素が760質量ppm、窒素が490質量ppm、炭素が905質量ppmであった。
表4に示す組成の拡散助剤(遠心アトマイズ法によって作製された粒度50μm以下の球状粉末)を使用し表4で示す混合比でTbF3粉末と混合した混合粉末を用いること以外は実験例1と同様にしてサンプル13〜20を得た。得られたサンプル13〜20の磁気特性をB−Hトレーサーによって測定し、HcJとBrの変化量を求めた。結果を表5に示す。
表6に示す組成の拡散助剤を使用し、拡散助剤と拡散剤の混合質量比およびR−T−B系焼結磁石表面(拡散面)1mm2あたりのRH量が表6の値となるように塗布したこと以外は実験例1と同様にしてサンプル21〜26を得た。サンプル24は、実験例1において好ましい結果が得られなかったサンプル1(本発明で規定する混合質量比よりもRH化合物が多いもの)と同じ拡散助剤と拡散剤、混合質量比で、R−T−B系焼結磁石表面(拡散面)1mm2あたりのRH量を表6に示す値に増やしたものであり、サンプル25は、実験例2において好ましい結果が得られなかったサンプル16(RLが50原子%未満の拡散助剤を使用したもの)と同じ拡散助剤と拡散剤、混合質量比で、R−T−B系焼結磁石表面(拡散面)1mm2あたりのRH量を表6に示す値に増やしたものであり、サンプル26は拡散助剤としてRHM合金を用いたものである。得られたサンプル21〜26の磁気特性をB−Hトレーサーによって測定し、HcJとBrの変化量を求めた。結果を表7に示す。なお、それぞれの表には比較対象の実施例としてサンプル5の値を示している。
組成がNd70Cu30(原子%)の拡散助剤(遠心アトマイズ法によって作製された粒度150μm以下の球状粉末)とTbF3粉末(拡散剤)を、拡散助剤:拡散剤が9:1となるように混合してスラリーを作製し、表8に示す条件で熱処理を行ったこと以外は、実験例1と同様にしてサンプル27〜29を得た。得られたサンプル27〜29の磁気特性をB−Hトレーサーによって測定し、HcJとBrの変化量を求めた。結果を表9に示す。
R−T−B系焼結磁石母材を表10に示す組成、焼結温度、不純物量、および磁気特性のものとしたこと以外はサンプル5と同様にしてサンプル30〜33を得た。得られたサンプル30〜33の磁気特性をB−Hトレーサーによって測定し、HcJとBrの変化量を求めた。結果を表11に示す。
酸フッ化物を含有する拡散剤を使用し、表12に示す拡散助剤と表12に示す混合質量比で混合した混合粉末を用いること以外は、実験例1と同様にしてサンプル36を得た。得られたサンプル36の磁気特性をB−Hトレーサーによって測定し、HcJとBrの変化量を求めた。結果を表13に示す。表13には、比較のため、拡散剤としてTbF3を用いて同じ条件でサンプルを作製したサンプル4の結果も示している。
拡散助剤を常温大気中に50日間放置することにより、表面を酸化させた拡散助剤を用意した。この点以外はサンプル5と同様にしてサンプル37を作製した。なお、50日間の放置後の拡散助剤は、放置前に1800ppmであった酸素含有量が4700ppmに上昇した。
Claims (5)
- R−T−B系焼結磁石を用意する工程と、
前記R−T−B系焼結磁石の表面に、アトマイズ法で作製されたRLM合金(RLはNdおよび/またはPr、MはCu、Fe、Ga、Co、Ni、Alから選ばれる1種以上の元素)の粉末と、RH化合物(RHはDyおよび/またはTb、RH化合物はRH酸化物、RHフッ化物、RH酸フッ化物から選ばれる一種以上)の粉末と、を存在させた状態でR−T−B系焼結磁石の焼結温度以下で熱処理する工程を含み、
前記RLM合金はRLを50原子%以上含み、かつ、前記RLM合金の融点は前記熱処理の温度以下であり、
前記熱処理は、前記RLM合金の粉末と前記RH化合物の粉末とが、RLM合金:RH化合物=9.6:0.4〜5:5の質量比率で前記R−T−B系焼結磁石の表面に存在する状態で行われる、R−T−B系焼結磁石の製造方法。 - 前記R−T−B系焼結磁石の表面において、前記RH化合物の粉末に含まれるRHの質量は、前記表面の1mm2あたりで0.03〜0.35mgである請求項1に記載のR−T−B系焼結磁石の製造方法。
- 前記R−T−B系焼結磁石の表面にRLM合金粉末とRH化合物粉末の混合粉末とバインダおよび/または溶媒を含むスラリーを塗布する工程を含む、請求項1または2に記載のR−T−B系焼結磁石の製造方法。
- 前記R−T−B系焼結磁石の上面の表面にRLM合金粉末とRH化合物粉末の混合粉末とバインダおよび/または溶媒を含むスラリーを塗布し、R−T−B系焼結磁石の前記表面に1粒子層以上のRLM合金粉末粒子層を形成する、請求項1から3のいずれかに記載のR−T−B系焼結磁石の製造方法。
- 前記RH化合物はRHフッ化物および/またはRH酸フッ化物である、請求項1から4のいずれかに記載のR−T−B系焼結磁石の製造方法。
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