JP5059955B2 - 磁石用粉末 - Google Patents
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Description
準備工程:希土類-鉄-ホウ素系合金からなる合金粉末を準備する工程。
水素化工程:上記合金粉末を、水素元素を含む雰囲気中、上記希土類-鉄-ホウ素系合金の不均化温度以上の温度で熱処理して上記磁石用粉末を製造する工程。
[磁石用粉末]
本発明磁石用粉末を構成する各磁性粒子は、鉄含有物を主成分とし、その含有量を60体積%以上とする。鉄含有物の含有量が60体積%未満であると、硬質である希土類元素の水素化合物が相対的に多くなり、圧縮成形時、鉄含有物成分を十分に変形することが難しく、多過ぎると磁気特性の低下を招くことから90体積%以下が好ましい。
上記磁石用粉末は、希土類-鉄-ホウ素系合金からなる合金粉末(例えば、Nd2Fe14B)を用意し、この合金粉末を、水素元素を含む雰囲気中で熱処理して、上記合金中の希土類元素と鉄と鉄-ホウ素合金とを分離すると共に、当該希土類元素と水素とを化合することで得られる。上記合金粉末は、例えば、希土類-鉄-ホウ素系合金からなる溶解鋳造インゴットや急冷凝固法で得られる箔状体をジョークラッシャー、ジェットミルやボールミルなどの粉砕装置により粉砕したり、ガスアトマイズ法といったアトマイズ法を利用して製造することができる。特に、ガスアトマイズ法を利用する場合、非酸化性雰囲気で粉末を形成することで、実質的に酸素が含有されない粉末(酸素濃度:1000質量ppm以下、好ましくは500質量ppm以下)とすることができる。即ち、合金粉末を構成する磁性粒子中の酸素濃度が1000質量ppm以下であることは、非酸化性雰囲気のガスアトマイズ法により製造された粉末であることを示す指標の一つとなり得る。その他、上記希土類-鉄-ホウ素系合金からなる合金粉末には、公知の粉末の製造方法により得られたものやアトマイズ法により製造した粉末を更に粉砕したものを利用してもよい。粉砕条件や製造条件を適宜変更することで、磁石用粉末の粒度分布や磁性粒子の形状を調整することができる。例えば、アトマイズ法を利用すると、真球度が高く、成形時の充填性に優れた粉末が得られ易い。上記合金粉末を構成する各磁性粒子は多結晶体でも単結晶体でもよい。多結晶体からなる磁性粒子に適宜熱処理を加えて単結晶体からなる粒子とすることができる。
上記本発明磁石用粉末を圧縮成形することで、本発明粉末成形体が得られる。上述のように本発明磁石用粉末は、成形性に優れることから相対密度(粉末成形体の真密度に対する実際の密度)が高い粉末成形体を形成できる。例えば、本発明粉末成形体の一形態として、相対密度が85%以上、更には90%以上のものが挙げられる。このような高密度の粉末成形体を利用することで、磁性相の比率が高い希土類磁石が得られる。相対密度が高いほど、磁性相の比率が高められるため、相対密度の上限は特に設けない。
上記磁性粒子と反応せず、かつ水素を効率よく除去できるように非水素雰囲気にて、上記粉末成形体に熱処理(脱水素処理)を施して、上記希土類元素の水素化合物から水素を除去すると共に、鉄と、鉄-ホウ素合金と、水素が除去された希土類元素とを化合することで、本発明希土類-鉄-ホウ素系合金材が得られる。本発明希土類-鉄-ホウ素系合金材は、実質的に、希土類-鉄-ホウ素系合金の相から構成される単一形態、実質的に、鉄相、鉄-ホウ素合金相、及び希土類-鉄合金相から選択される少なくとも一種の相と、希土類-鉄-ホウ素系合金の相との組み合わせで構成される混合形態、例えば、鉄相と希土類-鉄-ホウ素系合金の相との形態、鉄-ホウ素合金相と希土類-鉄-ホウ素系合金の相との形態、希土類-鉄合金相と希土類-鉄-ホウ素系合金の相との形態が挙げられる。上記単一形態は、例えば、上記本発明磁石用粉末の原料に用いた希土類-鉄-ホウ素系合金と実質的に同じ組成からなるものが挙げられる。上記混合形態は、代表的には、原料に用いる希土類-鉄-ホウ素系合金の組成により変化し、例えば、鉄の比率(原子比)が高いものを用いると、鉄相と希土類-鉄-ホウ素系合金の相との形態を形成することができる。
上記本発明希土類-鉄-ホウ素系合金材を適宜着磁することで、希土類磁石を製造できる。特に、上述した相対密度が高い粉末成形体を利用することで、磁性相の比率が80体積%以上、更に90体積%以上といった希土類磁石が得られる。
希土類元素と鉄とホウ素とを含む粉末を種々作製し、得られた粉末を圧縮成形して、各粉末の成形性を調べた。
試験例1と同様にして希土類磁石を作製し、磁気特性を調べた。
脱水素処理時の条件を変えて希土類磁石を作製し、磁気特性を調べた。
4 粉末成形体 5 希土類-鉄-ホウ素系合金材 6 希土類-鉄-ホウ素系合金磁石
Claims (13)
- 希土類磁石に用いられる磁石用粉末であって、
前記磁石用粉末を構成する各磁性粒子は、
10体積%以上40体積%未満の希土類元素の水素化合物と、残部が鉄含有物とからなり、
前記鉄含有物は、鉄と、鉄及びホウ素を含む鉄-ホウ素合金とを含み、
前記希土類元素の水素化合物の相は、粒状であり、
前記鉄含有物の相中に、前記粒状の希土類元素の水素化合物が分散して存在すると共に、前記希土類元素の水素化合物の相と前記鉄含有物の相とが隣接して存在しており、
前記鉄含有物の相を介して隣り合う前記希土類元素の水素化合物の相間の間隔が3μm以下であることを特徴とする磁石用粉末。 - 前記希土類元素は、Nd,Pr,Ce,Dy,及びYから選択される少なくとも1種の元素を含むことを特徴とする請求項1に記載の磁石用粉末。
- 前記磁性粒子の平均粒径が10μm以上500μm以下であることを特徴とする請求項1又は2に記載の磁石用粉末。
- 前記鉄含有物中の前記鉄と、前記鉄-ホウ素合金とは、希土類元素とは独立的に存在することを特徴とする請求項1〜3のいずれか1項に記載の磁石用粉末。
- 請求項1〜4のいずれか1項に記載の磁石用粉末を圧縮成形して製造された粉末成形体であり、
前記粉末成形体の相対密度が85%以上であることを特徴とする粉末成形体。 - 請求項5に記載の粉末成形体を不活性雰囲気中、又は減圧雰囲気中で熱処理して製造されたことを特徴とする希土類-鉄-ホウ素系合金材。
- 請求項5に記載の粉末成形体を不活性雰囲気中、又は減圧雰囲気中で熱処理して製造され、鉄相、鉄-ホウ素合金相、及び希土類-鉄合金相から選択される少なくとも一種の相と、希土類-鉄-ホウ素合金相との混相材で構成されていることを特徴とする希土類-鉄-ホウ素系合金材。
- 請求項5に記載の粉末成形体に4T以上の磁界を印加した状態で不活性雰囲気中、又は減圧雰囲気中で熱処理を施して製造され、前記磁界の印加方向が法線方向となる面のX線回折パターンをとったとき、結晶面の面間隔が0.202nmから0.204nmの間に出現する回折ピークの相対強度が70以上であることを特徴とする希土類-鉄-ホウ素系合金材。
- 希土類磁石に用いられる磁石用粉末を製造する磁石用粉末の製造方法であって、
希土類-鉄-ホウ素系合金からなる合金粉末を準備する準備工程と、
前記合金粉末を、水素元素を含む雰囲気中、当該希土類-鉄-ホウ素系合金の不均化温度以上の温度で熱処理して前記磁石用粉末を製造する水素化工程とを具え、
前記磁石用粉末を構成する各磁性粒子は、
10体積%以上40体積%未満の希土類元素の水素化合物と残部が鉄含有物とからなり、
前記鉄含有物が鉄と、鉄及びホウ素を含む鉄-ホウ素合金とを含み、
前記希土類元素の水素化合物の相は、粒状であり、
前記鉄含有物の相中に、前記粒状の希土類元素の水素化合物が分散して存在すると共に、前記希土類元素の水素化合物の相と前記鉄含有物の相とが隣接して存在しており、
かつ前記鉄含有物の相を介して隣り合う前記希土類元素の水素化合物の相間の間隔が3μm以下であることを特徴とする磁石用粉末の製造方法。 - 前記鉄含有物中の前記鉄と、前記鉄-ホウ素合金とは、希土類元素とは独立的に存在することを特徴とする請求項9に記載の磁石用粉末の製造方法。
- 希土類磁石に用いられる希土類-鉄-ホウ素系合金材を製造する希土類-鉄-ホウ素系合金材の製造方法であって、
希土類-鉄-ホウ素系合金からなる合金粉末を準備する準備工程と、
前記合金粉末を、水素元素を含む雰囲気中、当該希土類-鉄-ホウ素系合金の不均化温度以上の温度で熱処理して、以下の磁石用粉末を製造する水素化工程と、
前記磁石用粉末を圧縮成形して、相対密度が85%以上である粉末成形体を成形する成形工程と、
前記粉末成形体を不活性雰囲気中、又は減圧雰囲気中、当該粉末成形体の再結合温度以上の温度で熱処理して、希土類-鉄-ホウ素合金相を形成する脱水素工程とを具えることを特徴とする希土類-鉄-ホウ素系合金材の製造方法。
前記磁石用粉末は、
10体積%以上40体積%未満の希土類元素の水素化合物と残部が鉄含有物とからなり、
前記鉄含有物が鉄と、鉄及びホウ素を含む鉄-ホウ素合金とを含み、
前記希土類元素の水素化合物の相は、粒状であり、
前記鉄含有物の相中に、前記粒状の希土類元素の水素化合物が分散して存在すると共に、前記希土類元素の水素化合物の相と前記鉄含有物の相とが隣接して存在しており、
かつ前記鉄含有物の相を介して隣り合う前記希土類元素の水素化合物の相間の間隔が3μm以下である磁性粒子から構成される。 - 希土類磁石に用いられる希土類-鉄-ホウ素系合金材を製造する希土類-鉄-ホウ素系合金材の製造方法であって、
希土類-鉄-ホウ素系合金からなる合金粉末を準備する準備工程と、
前記合金粉末を、水素元素を含む雰囲気中、当該希土類-鉄-ホウ素系合金の不均化温度以上の温度で熱処理して、以下の磁石用粉末を製造する水素化工程と、
前記磁石用粉末を圧縮成形して、相対密度が85%以上である粉末成形体を成形する成形工程と、
前記粉末成形体を不活性雰囲気中、又は減圧雰囲気中、当該粉末成形体の再結合温度以上の温度で熱処理して、鉄相、鉄-ホウ素合金相、及び希土類-鉄合金相から選択される少なくとも一種の相と、希土類-鉄-ホウ素合金相との混相を形成する脱水素工程とを具えることを特徴とする希土類-鉄-ホウ素系合金材の製造方法。
前記磁石用粉末は、
10体積%以上40体積%未満の希土類元素の水素化合物と残部が鉄含有物とからなり、
前記鉄含有物が鉄と、鉄及びホウ素を含む鉄-ホウ素合金とを含み、
前記希土類元素の水素化合物の相は、粒状であり、
前記鉄含有物の相中に、前記粒状の希土類元素の水素化合物が分散して存在すると共に、前記希土類元素の水素化合物の相と前記鉄含有物の相とが隣接して存在しており、
かつ前記鉄含有物の相を介して隣り合う前記希土類元素の水素化合物の相間の間隔が3μm以下である磁性粒子から構成される。 - 前記脱水素工程の熱処理は、前記粉末成形体に4T以上の磁界を印加した状態で行うことを特徴とする請求項11又は12に記載の希土類-鉄-ホウ素系合金材の製造方法。
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