JP2022176506A - 異方性希土類焼結磁石及びその製造方法 - Google Patents
異方性希土類焼結磁石及びその製造方法 Download PDFInfo
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- JP2022176506A JP2022176506A JP2021082977A JP2021082977A JP2022176506A JP 2022176506 A JP2022176506 A JP 2022176506A JP 2021082977 A JP2021082977 A JP 2021082977A JP 2021082977 A JP2021082977 A JP 2021082977A JP 2022176506 A JP2022176506 A JP 2022176506A
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- rare earth
- sintered magnet
- anisotropic rare
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 64
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 55
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
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- 230000005291 magnetic effect Effects 0.000 claims abstract description 40
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 13
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 12
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- 229910052748 manganese Inorganic materials 0.000 claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 9
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 9
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- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 9
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 9
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- 229910052759 nickel Inorganic materials 0.000 claims abstract description 8
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 7
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
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- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
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- 238000009499 grossing Methods 0.000 description 1
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- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910001068 laves phase Inorganic materials 0.000 description 1
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- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
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- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
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- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/0536—Alloys characterised by their composition containing rare earth metals sintered
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- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
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Abstract
Description
(1)組成が式 (R1-aZra)v(Fe1-bCob)100-v-w-x-y(M1 1-cM2 c)wOxCy(Rは希土類元素から選ばれる1種以上でSmを必須とし、M1はV、Cr、Mn、Ni、Cu、Zn、Ga、Al、Siからなる群より選ばれる1種以上の元素、M2はTi、Nb、Mo、Hf、Ta、Wからなる群より選ばれる1種以上の元素であり、v、w、x、y、a、b、cは各々、7≦v≦15原子%、4≦w≦20原子%、0.2≦x≦4原子%、0.2≦y≦2原子%、0≦a≦0.2、0≦b≦0.5、0≦c≦0.9)で表される異方性希土類焼結磁石であって、ThMn12型結晶の化合物からなる主相を80体積%以上含み、前記主相の平均結晶粒径が1μm以上であり、Rのオキシカーバイドを粒界部に含み、かつ密度が7.3g/cm3以上であることを特徴とする異方性希土類焼結磁石。
(2)前記オキシカーバイドが、R(C,O)相、R(C,O)2相、及びR2(C,O)3相からなる群より選ばれる1種以上のオキシカーバイドであることを特徴とする(1)に記載の異方性希土類焼結磁石。
(3)前記オキシカーバイドを1体積%以上含むことを特徴とする(1)又は(2)に記載の異方性希土類焼結磁石。
(4)前記焼結体の組成において、R中のSmの比率が原子割合で0.05以上であることを特徴とする(1)~(3)のいずれかに記載の異方性希土類焼結磁石。
(5)Rリッチ相及びR(Fe,Co)2相を粒界部に含み、
前記Rリッチ相及び前記R(Fe,Co)2相の形成量の合計が1体積%以上であることを特徴とする(1)~(4)のいずれかに記載の異方性希土類焼結磁石。
(6)前記R(Fe,Co)2相が、室温以上でフェロ磁性又はフェリ磁性を示す相であることを特徴とする(5)に記載の異方性希土類焼結磁石。
(7)隣接する主相粒の間に2粒子間粒界相が形成されていることを特徴とする(1)~(6)のいずれかに記載の異方性希土類焼結磁石。
(8)室温で5kOe以上の保磁力を示し、保磁力の温度係数βが-0.5%/K以上であることを特徴とする(1)~(7)のいずれかに記載の異方性希土類焼結磁石。
(9)ThMn12型結晶の化合物相を含み、かつオキシカーバイドを含まない合金を粉砕し、磁場印加中で圧粉成形して成形体とした後、800℃以上1400℃以下の温度で焼結して、オキシカーバイドを粒界部に形成させることを特徴とする(1)~(8)のいずれかに記載の異方性希土類焼結磁石の製造方法。
(10)前記焼結後に300~900℃の温度で熱処理を施すことを特徴とする(9)に記載の異方性希土類焼結磁石の製造方法。
(R1-aZra)v(Fe1-bCob)100-v-w-x-y(M1 1-cM2 c)wOxCy
で表され、ThMn12型結晶の化合物が主相であり、ThMn12型結晶の化合物からなる主相を80体積%以上含み、主相の平均結晶粒径が1μm以上であり、Rのオキシカーバイドを粒界部に含み、かつ密度が7.3g/cm3以上である異方性希土類焼結磁石である。まず各成分について以下に説明する。なお、v、w、x、y、a、b、cは各々、7≦v≦15原子%、4≦w≦20原子%、0.2≦x≦4原子%、0.2≦y≦2原子%、0≦a≦0.2、0≦b≦0.5、0≦c≦0.9である。
なお、オキシカーバイドは、好ましくはR(C,O)相、R(C,O)2相、及びR2(C,O)3相からなる群より選ばれる1種以上のオキシカーバイドである。このように、組成範囲が広いため、本発明の異方性希土類焼結磁石を再現性良く作製することが容易である。
本発明の異方性希土類焼結磁石における主相は、ThMn12型結晶構造の化合物からなり、好ましくはR(Fe,Co,M)12化合物からなる。焼結磁石を作製する工程で不可避的に混入するC、N、Oなどの元素は、主相に含まれないことが好ましい。ただし、EPMA(電子線マイクロアナライザ)を用いた組成分析で、測定ばらつき、観察試料の調整方法や他元素の検出信号の影響などによりC、N、O元素が検出される場合、主相のHAを良好に得る観点から、その上限は各々1原子%までが好ましい。主相の平均結晶粒径は1μm以上であり、1μm以上30μm以下が好ましい。1.5μm以上20μm以下の範囲であればさらに好ましく、2μm以上10μm以下が特に好ましい。平均結晶粒径をこのような範囲とすることで、結晶粒の配向度の低下による残留磁束密度Brの減少や、保磁力HcJの低下を抑制できる。主相の体積率は、良好なBrやHcJを得る観点から、磁石全体に対して80体積%以上であり、80体積%以上99体積%未満が好ましく、90体積%以上95体積%以下であればさらに好ましい。
なお、主相の平均結晶粒径は以下のようにして測定した値である。
焼結磁石の断面を鏡面になるまで研磨した後、エッチング液(硝酸+塩酸+グリセリンの混合液など)に浸漬して粒界相を選択的に除去し、この断面の任意の10箇所以上についてレーザー顕微鏡で観察を行った。得られた観察像から画像解析により各粒子の断面積を算出し、これらを円とみなした時の平均直径を平均結晶粒径とした。
また、主相の体積率は以下のようにして測定した値である。
EPMAを用いて異方性希土類焼結磁石の組織観察と各相の組成分析を行い、主相、Rリッチ相及びR(Fe,Co)2相を確認した。そして、各相の体積率は、反射電子像の画像における面積比に等しいものとして算出した。
Smメタル、電解鉄、Coメタル、Vメタル、純Si、及びAlメタルを用いて組成を調整し、高周波誘導炉を用いてArガス雰囲気中で溶解して鋳造合金を作製した。初晶α-Feを消失させるため、合金には900℃20時間の熱処理を施した。合金の断面を研磨してエッチング処理後、レーザー顕微鏡(オリンパス株式会社製、LEXT OLS4000)にて組織観察を行った。観察した画像から主相の平均結晶粒径が5μm以上であることを確認した。この合金の一部を粉砕して得た粉末のX線回折測定より、この合金がThMn12型結晶の化合物を含むことを確認した。またEPMA装置(日本電子株式会社製、JXA-8500F)を用いた観察より、この合金中にオキシカーバイドは形成されていないことを確認した。合金に水素吸蔵処理及び真空中400℃で加熱する脱水素化処理を施して粗粉末とした後、ステアリン酸の混合比を変えて混合し、窒素気流中のジェットミルで粉砕していずれも平均粒径1.9μmの微粉末とした。さらに不活性ガス雰囲気中で成形装置の金型に充填して磁界中成形で圧粉成形体とし、Arガス雰囲気で1140℃3時間の焼結熱処理を施して、冷却速度12℃/分で室温まで冷却した。これら焼結体は、いずれも10×10×12mmのサイズに切削加工した。得られた焼結体サンプルのうち、ステアリン酸を0.1、0.15、0.2,0.3重量%混合して作製した各サンプルを、順に実施例1~4とし、ステアリン酸を加えなかったものを比較例1とする。
Smメタル、Ceメタル、電解鉄、Coメタル、Vメタル、Gaメタル及びカーボンブラックを用いて組成を調整し、高周波誘導炉を用いてArガス雰囲気中で溶解後、高周波誘導炉を用いてArガス雰囲気中で溶解してC含有量の異なる複数の鋳造合金を作製した。初晶α-Feを消失させるため、合金にはいずれも830℃30時間の熱処理を施した。各合金の断面を研磨してエッチング処理後、レーザー顕微鏡で組織観察を行い、主相の平均結晶粒径がいずれも5μm以上であることを確認した。この合金の一部を粉砕して得た粉末のX線回折測定より、この合金がThMn12型結晶の化合物を含むことを確認した。またEPMA観察より、これらの合金中にはいずれもオキシカーバイドは形成されておらず、カーボンブラックを添加した合金中にはSm3C相が存在していることを確認した。いずれの合金も水素吸蔵処理及び真空中400℃で加熱する脱水素化処理を施して粗粉末とした後、ステアリン酸0.02重量%と混合し、窒素気流中のジェットミルで粉砕していずれも平均粒径2.1μmの微粉末とした。さらに不活性ガス雰囲気中で成形装置の金型に充填して磁界中成形で圧粉成形体とし、Arガス雰囲気で1110℃3時間の焼結熱処理を施して、冷却速度12℃/分で室温まで冷却した。カーボンブラックを添加した合金を用いて作製した焼結体サンプルを実施例5~7とし、カーボンブラックを添加しない合金で作製したものを比較例2とした。
Smメタル、Ndメタル、Yメタル、電解鉄、Crメタル、Niメタル、スポンジチタン、及び活性炭素を用いて組成を調整し、高周波誘導炉を用いてArガス雰囲気中で溶解後、水冷Cuロール上でストリップキャストすることにより、厚さ0.2~0.4mm程度の合金薄帯を製造した。薄帯が冷却ロールに接触した面から約0.15mmの位置をレーザー顕微鏡で観察し、主相の短軸方向平均結晶粒径が1μm以上であることを確認した。この合金の一部を粉砕して得た粉末のX線回折測定より、この合金がThMn12型結晶の化合物を含むことを確認した。またEPMA観察より、合金中にオキシカーバイドは存在せず、Sm3C相が形成されていることを確認した。合金に水素吸蔵処理及び脱水素化処理を施して粗粉末とした後、窒素気流中のジェットミルで粉砕して平均粒径2.7μmの微粉末とした。さらに不活性ガス雰囲気中で成形装置の金型に充填して磁界中成形で圧粉成形体とし、Arガス雰囲気で1170℃4時間の焼結熱処理を施して、冷却速度14℃/分で室温まで冷却した。
Smメタル、Prメタル、Laメタル、電解鉄、Coメタル、純Si、Mnメタル、Alメタル、Nbメタル、及び高炭素フェロマンガンを用いて組成を調整し、ストリップキャスト法で合金薄帯を製造した。薄帯のロール接触面から約0.15mmの位置における主相の短軸方向平均結晶粒径は1μm以上であることを確認した。この合金の一部を粉砕して得た粉末のX線回折測定より、この合金がThMn12型結晶の化合物を含むことを確認した。またEPMA観察より、合金中にオキシカーバイドは存在せず、Sm3C相及びNbC相が形成されていることを確認した。合金に水素吸蔵処理及び脱水素化処理を施して粗粉末とした後、窒素気流中のジェットミルで粉砕して平均粒径2.3μmの微粉末とした。さらに不活性ガス雰囲気中で成形装置の金型に充填して磁界中成形で圧粉成形体とし、Arガス雰囲気で1120℃2時間の焼結熱処理を施して、冷却速度10℃/分で室温まで冷却した。
Smメタル、Zrメタル、電解鉄、Vメタル、純Si、及びCuメタルを用いて組成を調整し、ストリップキャスト法で合金薄帯を製造した。薄帯のロール接触面から約0.15mmの位置における主相の短軸方向平均結晶粒径は1μm以上であることを確認した。この合金の一部を粉砕して得た粉末のX線回折測定より、この合金がThMn12型結晶の化合物を含むことを確認した。またEPMA観察より、合金中にオキシカーバイドは確認されなかった。合金に水素吸蔵処理及び脱水素化処理を施して粗粉末とした後、粉末状のカーボンブラック0.2重量%と混合し、窒素気流中のジェットミルで粉砕して平均粒径2.4μmの微粉末とした。さらに不活性ガス雰囲気中で成形装置の金型に充填して磁界中成形で圧粉成形体とし、Arガス雰囲気で1160℃3時間の焼結熱処理を施して、冷却速度10℃/分で室温まで冷却した。これを実施例10とした。上記と同様に作製し、カーボンブラックを添加しなかったサンプルを比較例3とした。
Smメタル、電解鉄、Vメタルを用いて組成を調整し、原料溶湯を周速度20m/secで回転するCuロール上で冷却して、急冷薄帯の原料合金を作製した。薄帯の厚みは10~50μmであり、レーザー顕微鏡により得られた合金の組織観察を行い、観察した画像から平均結晶粒径は細かすぎて測定し難いものの、少なくとも1μmより小さいことを確認した。この合金薄帯をボールミルで粉砕した後、篩で300μm以下の粉末を選別し、さらにステアリン酸を0.2重量%添加した。これをAr雰囲気中720℃で5分間保持した後、約500MPaの圧力でホットプレスした。得られた試料の密度は7.12g/cm3であった。主相粒の平均結晶粒径は0.3~0.4μm程度であり、EPMAでは主相、粒界相の組成を同定できなかった。また主相の磁化容易軸が揃わないため、低いBrしか得られなかった。結果を表1,2,5に示す。
Claims (10)
- 組成が式 (R1-aZra)v(Fe1-bCob)100-v-w-x-y(M1 1-cM2 c)wOxCy(Rは希土類元素から選ばれる1種以上でSmを必須とし、M1はV、Cr、Mn、Ni、Cu、Zn、Ga、Al、Siからなる群より選ばれる1種以上の元素、M2はTi、Nb、Mo、Hf、Ta、Wからなる群より選ばれる1種以上の元素であり、v、w、x、y、a、b、cは各々、7≦v≦15原子%、4≦w≦20原子%、0.2≦x≦4原子%、0.2≦y≦2原子%、0≦a≦0.2、0≦b≦0.5、0≦c≦0.9)で表される異方性希土類焼結磁石であって、ThMn12型結晶の化合物からなる主相を80体積%以上含み、前記主相の平均結晶粒径が1μm以上であり、Rのオキシカーバイドを粒界部に含み、かつ密度が7.3g/cm3以上であることを特徴とする異方性希土類焼結磁石。
- 前記オキシカーバイドが、R(C,O)相、R(C,O)2相、及びR2(C,O)3相からなる群より選ばれる1種以上のオキシカーバイドであることを特徴とする請求項1に記載の異方性希土類焼結磁石。
- 前記オキシカーバイドを1体積%以上含むことを特徴とする請求項1又は2に記載の異方性希土類焼結磁石。
- 前記焼結体の組成において、R中のSmの比率が原子割合で0.05以上であることを特徴とする請求項1~3のいずれか一項に記載の異方性希土類焼結磁石。
- Rリッチ相及びR(Fe,Co)2相を粒界部に含み、
前記Rリッチ相及び前記R(Fe,Co)2相の形成量の合計が1体積%以上であることを特徴とする請求項1~4のいずれか一項に記載の異方性希土類焼結磁石。 - 前記R(Fe,Co)2相が、室温以上でフェロ磁性又はフェリ磁性を示す相であることを特徴とする請求項5に記載の異方性希土類焼結磁石。
- 隣接する主相粒の間に2粒子間粒界相が形成されていることを特徴とする請求項1~6のいずれか一項に記載の異方性希土類焼結磁石。
- 室温で5kOe以上の保磁力を示し、保磁力の温度係数βが-0.5%/K以上であることを特徴とする請求項1~7のいずれか一項に記載の異方性希土類焼結磁石。
- ThMn12型結晶の化合物相を含み、かつオキシカーバイドを含まない合金を粉砕し、磁場印加中で圧粉成形して成形体とした後、800℃以上1400℃以下の温度で焼結して、オキシカーバイドを粒界部に形成させることを特徴とする請求項1~8のいずれか一項に記載の異方性希土類焼結磁石の製造方法。
- 前記焼結後に300~900℃の温度で熱処理を施すことを特徴とする請求項9に記載の異方性希土類焼結磁石の製造方法。
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