JP7026192B6 - 異方性ボンド磁性粉及びその作製方法 - Google Patents
異方性ボンド磁性粉及びその作製方法 Download PDFInfo
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Description
母合金を精錬して、固体インゴットR1TB、及びR1R2Tをそれぞれ形成するステップと、
前記固体インゴットR1TBをHDDR炉に入れて、水素吸蔵、高温水素化、水素排出の工程を経て、希土類水素化物R1TBHXを作製するステップと、
前記固体インゴットR1R2Tに対して、温度500℃未満の水素処理を行い、水素化物拡散源R1R2THxを作製するステップと、
前記希土類水素化物R1TBHXと拡散源R1R2THxを混合するステップと、
混合された希土類水素化物R1TBHXと拡散源R1R2THxを熱処理するステップと、
高真空脱水素を行い、前記異方性ボンド磁性粉を得るステップ、
を含む。
所定の配合の原料合金を真空誘導炉でアルゴン雰囲気中で精錬して、高温で溶解した原料を厚さ30~35mmの金型に流し込み、金属液体を金型の中で急速に水冷させてインゴットを成形することと、
前記インゴットを真空熱処理炉に入れて、高真空環境で、温度1000℃~1100℃で20時間保温することと、
アルゴンガスを-0.01MPaまで充填し、定圧状態で急速空冷し、室温まで冷却した後、炉から取り出すこと、を含む。
固体インゴットR1TBをHDDR炉に入れて、真空状態で300℃まで昇温し、この温度で水素ガスを充填してガス圧を95~100kPaに維持し、300℃に1~2時間保温して水素吸蔵処理を完了することと、
30~35kPaまで真空引きし、790℃まで昇温し、この温度と圧力に180~200分間維持して高温水素化処理を完了することと、
水素ガスを50~70kPaまで充填するとともに、820℃まで昇温して30分間保温することと、
0.1~4kPaまで真空引きし、20分間保温して水素排出工程を完了することを含む。
前記固体インゴットR1R2Tを粗粉砕した後、気固反応炉に入れて、真空状態で300~500℃まで昇温し、この温度で水素ガスを充填してガス圧を95~100kPaに維持し、80分間保温して水素吸蔵・分解することと、
真空引きすると同時に、室温まで冷却して水素化物拡散源R1R2THxを得ることを含む。
ブレンダーによってArとN2の混合雰囲気で15~30分間混合することを含む。
ArとN2の混合雰囲気を熱処理雰囲気として選択することが好ましく、希土類水素化物R1TBHxと拡散源R2TBHxの混合粉末を400~700℃且つ真空状態で、0.5~2時間保温して熱処理工程を完了することを含む。
その後、室温まで急速に冷却することを含む。
本発明の第2の形態では、希土類異方性ボンド磁性粉R1R2TBの作製方法が提供され、前記作製方法は、以下のステップを含む。
実施例1:A1-B1~B3
一:R1TB及びR1R2Tインゴット原料の製造
表1と表2の組成に従って原料合金を秤量する。ここで、合金全体を100%として、各元素は質量分率wt%で表される。真空誘導炉により、高純度のアルゴン雰囲気中で精錬し、高温で溶解した原料を厚さ30~35mmの金型に流し込み、金属液体を金型の中で急速に水冷させてインゴットを成形した。
固体インゴット又はSC法で作製したストリップであるR1TBをHDDR炉に入れて、真空状態で300℃まで昇温し、その後、この温度で水素ガスを充填してガス圧を95~100kPaに維持し、300℃に1~2時間保温して、水素吸蔵・分解工程を完了した。水素ガス圧を30~35kPaに制御し、790℃まで昇温し続け、この温度と圧力に180~200分間維持して、そして50~70kPaまで水素ガスを充填し、さらに820℃まで昇温し続け、30分間保温して高温水素化工程を完了した。0.1~4kPaまで真空引きし、20分間保温して、第1排気工程を完了して、R1TBHXを得た。
R1TBHXとR1R2THX微粉末を混合するステップである。
四:拡散熱処理
混合粉末を400~700℃、10-2Paの真空状態で熱処理する。
五:高真空脱水素
熱処理した粉末を600~850℃、10-4Paの真空状態で熱処理する。
実施例2:A1-B4~B6、実施例1と同じ方法で得た。
実施例3:A1又はA2-B7、実施例1と同じ方法で得た。
Claims (8)
- 異方性ボンド磁性粉の作製方法であって、
前記異方性ボンド磁性粉の一般式は、R 1 R 2 TB(ここで、R 1 はNd又はPrNdを含有する希土類元素であり、R 2 はLa、Ceの1種又は2種であり、Tは遷移元素であり、Bはホウ素である)であり、
前記異方性ボンド磁性粉R 1 R 2 TBの各成分の質量分率は、Ndが28%~34.5%であり、Prの含有量が≦5%であり、Bの含有量が0.8%~1.2%であり、全質量に占めるLaとCeとの質量の合計の割合は≦0.1%であり、Tは残部であり、
前記異方性ボンド磁性粉は、R 1 R 2 Tの水素化物R 1 R 2 TH x を希土類元素の拡散源として使用して、NdTB又はPrNdTBの水素化物R 1 TBH x に対して400~700℃の作業温度で粒界拡散を行い、HDDRの高温脱水素工程により得られるものであり、
前記作製方法は、
母合金を精錬して、固体インゴットR1TB、及びR1R2Tをそれぞれ形成するステップと、
前記固体インゴットR1TBをHDDR炉に入れて、水素吸蔵、高温水素化、水素排出の工程を経て、希土類水素化物R1TBHXを作製するステップと、
前記固体インゴットR1R2Tに対して、温度500℃未満の水素処理を行い、水素化物拡散源R1R2THxを作製するステップと、
前記希土類水素化物R1TBHXと拡散源R1R2THxを混合するステップと、
混合された希土類水素化物R1TBHXと拡散源R1R2THxを熱処理するステップと、
高真空脱水素を行い、前記異方性ボンド磁性粉を得るステップ、
を含み、
前記母合金を精錬して、固体インゴットR 1 TB、及びR 1 R 2 Tをそれぞれ形成するステップは、
所定の配合の原料合金を真空誘導炉でアルゴン雰囲気中で精錬して、高温で溶解した原料を厚さ30~35mmの金型に流し込み、金属液体を金型の中で急速に水冷させてインゴットを成形することと、
前記インゴットを真空熱処理炉に入れて、高真空環境で、温度1000℃~1100℃で20時間保温することと、
アルゴンガスを-0.01MPaまで充填し、定圧状態で急速空冷し、室温まで冷却した後、炉から取り出すことを含むことを特徴とする、異方性ボンド磁性粉の作製方法。 - 前記R 2 元素の粒界相における含有量と主相における含有量との比は、3より大きいことを特徴とする、請求項1に記載の方法。
- 前記異方性ボンド磁性粉は、2:14:1を粒界構造とする主相R 1 TBと、主相を囲む粒界相を含むことを特徴とする、請求項1に記載の方法。
- 前記固体インゴットR1TBをHDDR炉に入れて、水素吸蔵、高温水素化、水素排出の工程を経て、希土類水素化物R1TBHXを作製するステップは、
固体インゴットR1TBをHDDR炉に入れて、真空状態で300℃まで昇温し、この温度で水素ガスを充填してガス圧を95~100kPaに維持し、300℃に1~2時間保温して水素吸蔵処理を完了することと、
30~35kPaまで真空引きし、790℃まで昇温し、この温度と圧力に180~200分間維持して高温水素化処理を完了することと、
水素ガスを50~70kPaまで充填するとともに、820℃まで昇温して30分間保温することと、
0.1~4kPaまで真空引きし、20分間保温して水素排出工程を完了すること、
を含むことを特徴とする、請求項1に記載の方法。 - 前記固体インゴットR1R2Tに対して、温度500℃未満の水素処理を行い、水素化物拡散源R1R2THxを作製するステップは、
前記固体インゴットR1R2Tを粗粉砕した後、気固反応炉に入れて、真空状態で300~500℃まで昇温し、この温度で水素ガスを充填してガス圧を95~100kPaに維持し、80分間保温して水素吸蔵・分解することと、
真空引きすると同時に、室温まで冷却して水素化物拡散源R1R2THxを得ること、
を含むことを特徴とする、請求項1に記載の方法。 - 前記希土類水素化物R1TBHXと拡散源R1R2THxを混合するステップは、
ブレンダーによってArとN2の混合雰囲気で15~30分間混合することを含むことを特徴とする、請求項1に記載の方法。 - 前記混合された希土類水素化物R1TBHXと拡散源R1R2THxを熱処理するステップは、
ArとN2の混合雰囲気を熱処理雰囲気として選択し、希土類水素化物R1TBHxと拡散源R2TBHxの混合粉末を400~700℃且つ真空状態で、0.5~2時間保温して熱処理工程を完了することを含むことを特徴とする、請求項1に記載の方法。 - 前記高真空脱水素を行い、前記異方性ボンド磁性粉を得るステップは、
温度600~850℃でガス圧を0.1Pa以下に維持し、真空引きを60~80分間続け、
その後、室温まで急速に冷却すること、
を含むことを特徴とする、請求項1に記載の方法。
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