JPWO2013100008A1 - NdFeB系焼結磁石及び該NdFeB系焼結磁石の製造方法 - Google Patents
NdFeB系焼結磁石及び該NdFeB系焼結磁石の製造方法 Download PDFInfo
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Abstract
Description
プレス有り磁石製造方法では、圧縮成形体を作製するために大型のプレス機が必要となるため、密閉空間内で行うことが難しいのに対し、プレスなし磁石製造工程ではプレス機を用いないことから、密閉空間内で充填から焼結までの作業を行うことができるという特長がある。
a)NdFeB系焼結磁石中の主相粒子の平均粒径が4.5μm以下、
b)前記NdFeB系焼結磁石全体の炭素含有率が1000ppm以下、
c)前記NdFeB系焼結磁石中の粒界三重点における希土類リッチ相の体積の総計に対する、該希土類リッチ相中の炭素リッチ相の体積の総計の比率が50%以下、
であることを特徴とする。
上記NdFeB系焼結磁石を製造するための方法であって、
a)NdFeB系合金に水素を吸蔵させることにより該NdFeB系合金を粗解砕する水素解砕工程と、
b)粗解砕されたNdFeB系合金を、レーザ回折法で測定される粒度分布の中央値D50で3.2μm以下になるように微粉砕する微粉砕工程と、
c)前記NdFeB系合金の微粉末を充填容器に充填し、その後、充填容器に充填したまま該微粉末の配向及び焼結を行うプレスなし磁石製造工程と、
を有し、
前記水素解砕工程において吸蔵された水素を脱離させるための脱水素加熱を行うことなく、前記微粉砕工程と前記プレスなし磁石製造工程を行い、
前記水素解砕工程から前記プレスなし磁石製造工程までを無酸素雰囲気下で行う、
ことを特徴とする。
また、プレスなし磁石製造方法でも上記の第1の理由から脱水素加熱が行われていた。
本発明に係るNdFeB系焼結磁石の製造方法では、上記の通り、NdFeB系合金の粉砕から焼結までの工程をすべて無酸素雰囲気下で行うため、合金粉末の平均粒径を3.2μm以下という非常に小さなものとしても、酸化による磁気特性の低下や事故の発生を抑えることができる。これにより、高い保磁力を有するNdFeB系焼結磁石を製造することができる。
また、実験の結果、本発明に係るNdFeB系焼結磁石の製造方法では、微粉砕工程における出発合金の粉砕速度を従来よりも高くすることができること、プレスなし工程中の焼結処理において、最適な焼結温度を従来よりも5〜20℃程度下げることができることが分かった。粉砕速度が高くなることは製造時間の短縮に、最適焼結温度が低くなることはエネルギーの節約や充填容器の長寿命化に、それぞれ繋がる。
なお、ステップA3〜A5の工程はプレスなし工程により行われる。また、ステップA1〜A5の工程は、一貫して無酸素雰囲気下で行われる。
なお、昇温配向とは、配向工程の際に合金粉末を加熱することにより、合金粉末の各粒子の保磁力を低下させ、配向後の粒子間の反発を抑える方法のことである。この方法により、製造後のNdFeB系焼結磁石の配向度を向上させることができる。
一方、本実施例のNdFeB系焼結磁石の製造方法では脱水素加熱を行わない。そのため、図3に示すように、発熱に伴う温度上昇後、真空脱気しつつ室温まで冷却させる時間を多少長めに取っても、約400分で水素解砕工程を終了することができる。従って、図4の例と比べると、約1000分(16.7時間)ほど製造時間を短縮することができる。
なお、表2の結果は、いずれも微粉砕後の合金粉末の粒径が、レーザ回折法のD50で2.82μmになるように調整した場合のものである。また、微粉砕工程に用いるジェットミル装置には、ホソカワミクロン製100AFG型ジェットミル装置を用いた。磁気特性の測定には、日本電磁測器株式会社製のパルス磁化測定装置(商品名:パルスBHカーブトレーサPBH-1000)を用いた。
また、表2の脱水素無し、昇温配向無しの結果が、本実施例のNdFeB系焼結磁石の製造方法を、脱水素有り、昇温配向有りの結果が、比較例のNdFeB系焼結磁石の製造方法を、それぞれ示している。
さらに、被測定物の表面をイオンスパッタ(例えばArイオンによるスパッタ)していくことで、被測定物の深さ方向の元素分布を調べることができる。
本実施例のNdFeB系焼結磁石では、殆どの小領域において、20%以下の低いC/Ndが得られた。一部の小領域で50%のC/Ndを示す分布が見られたが、50%を超えるC/Ndを示す小領域はなかった。また、領域全体(全ての小領域を合わせた領域)でのC/Ndは26.5%であった。
一方、比較例のNdFeB系焼結磁石では、ほぼ全ての小領域で90%以上という高いC/Ndが得られた。また、領域全体のC/Ndは93.1%であった。
表3の実施例1〜4は、上記(i)〜(iii)の特徴を有する、それぞれ組成番号1〜4の合金に対して本実施例の製造方法により製造した、厚さ方向が磁化方向である縦7mm×横7mm×厚さ3mmのNdFeB系焼結磁石である。また、表3の比較例1〜4は、上記(ii)及び(iii)の特徴を有さない、それぞれ組成番号1〜4の合金から比較例の製造方法により製造した実施例1〜4と同じ大きさのNdFeB系焼結磁石である。これら実施例1〜4及び比較例1〜4のNdFeB系焼結磁石は、後述する粒界拡散法の基材として使用される。
まず、Tb:92wt%、Ni:4.3wt%、Al:3.7wt%のTbNiAl合金粉末とシリコーングリースを重量比で80:20の割合で混合した混合物10gにシリコーンオイルを0.07g添加したペーストを基材の両磁極面(7mm×7mmの面)にそれぞれ10mgずつ塗布した。
次に、上記ペーストを塗布した直方体基材を、複数の尖形状の支持部が設けられたモリブデン製のトレイに載せ、直方体基材を該支持部によって支持しつつ、10-4Paの真空中で加熱した。加熱温度と加熱時間はそれぞれ880℃、10時間とした。その後室温付近まで急冷して、次に500℃で2時間加熱して、再度室温まで急冷した。
このように本実施例の粒界拡散処理前及び粒界拡散処理後のNdFeB系焼結磁石の磁気特性が高いことの要因は、第一に、NdFeB系焼結磁石中の炭素含有率が低いため、Ndリッチな粒界三重点領域内に炭素リッチな領域が生成されることが抑制されるためと考えられる。第二に、Ndリッチな粒界三重点領域におけるCリッチな領域の量が少ないため、Ndリッチ相の通路を通って、十分な量のRH(本実施例ではTb)が基材内部まで拡散するためであると考えられる。
11…Ndリッチ相の存在する領域
12…Cが分布する領域
Claims (2)
- a)NdFeB系焼結磁石中の主相粒子の平均粒径が4.5μm以下、
b)前記NdFeB系焼結磁石全体の炭素含有率が1000ppm以下、
c)前記NdFeB系焼結磁石中の粒界三重点における希土類リッチ相の体積の総計に対する、該希土類リッチ相中の炭素リッチ相の体積の総計の比率が50%以下、
であることを特徴とするNdFeB系焼結磁石。 - 請求項1に記載のNdFeB系焼結磁石を製造するための方法であって、
a)NdFeB系合金に水素を吸蔵させることにより該NdFeB系合金を粗解砕する水素解砕工程と、
b)粗解砕されたNdFeB系合金を、レーザ回折法で測定される粒度分布の中央値D50で3.2μm以下になるように微粉砕する微粉砕工程と、
c)前記NdFeB系合金の微粉末を充填容器に充填し、その後、充填容器に充填したまま該微粉末の配向及び焼結を行うプレスなし磁石製造工程と、
を有し、
前記水素解砕工程において吸蔵された水素を脱離させるための脱水素加熱を行うことなく、前記微粉砕工程と前記プレスなし磁石製造工程を行い、
前記水素解砕工程から前記プレスなし磁石製造工程までを無酸素雰囲気下で行う、
ことを特徴とするNdFeB系焼結磁石の製造方法。
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US9837207B2 (en) | 2012-07-24 | 2017-12-05 | Intermetallics Co., Ltd. | Method for producing NdFeB system sintered magnet |
JP6303356B2 (ja) * | 2013-09-24 | 2018-04-04 | 大同特殊鋼株式会社 | RFeB系磁石の製造方法 |
JP2015228431A (ja) * | 2014-06-02 | 2015-12-17 | インターメタリックス株式会社 | RFeB系磁石及びRFeB系磁石の製造方法 |
CN107112125A (zh) * | 2015-01-09 | 2017-08-29 | 因太金属株式会社 | RFeB系烧结磁体的制造方法 |
JP6572550B2 (ja) | 2015-02-04 | 2019-09-11 | Tdk株式会社 | R−t−b系焼結磁石 |
KR101711859B1 (ko) * | 2015-12-21 | 2017-03-03 | 주식회사 포스코 | 희토류 영구 자석의 제조 방법 |
US10784028B2 (en) * | 2016-02-26 | 2020-09-22 | Tdk Corporation | R-T-B based permanent magnet |
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