JP2020521316A - 焼結磁石の製造方法および焼結磁石 - Google Patents
焼結磁石の製造方法および焼結磁石 Download PDFInfo
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- 229910001172 neodymium magnet Inorganic materials 0.000 claims abstract description 53
- 238000005245 sintering Methods 0.000 claims abstract description 44
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 43
- -1 rare earth hydride Chemical class 0.000 claims abstract description 39
- 239000000203 mixture Substances 0.000 claims abstract description 38
- 238000002156 mixing Methods 0.000 claims abstract description 25
- 238000009792 diffusion process Methods 0.000 claims abstract description 21
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 42
- 238000010438 heat treatment Methods 0.000 claims description 16
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 14
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 9
- 229910052796 boron Inorganic materials 0.000 claims description 9
- 239000011575 calcium Substances 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 150000002910 rare earth metals Chemical class 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims 1
- 101100294913 Neurospora crassa (strain ATCC 24698 / 74-OR23-1A / CBS 708.71 / DSM 1257 / FGSC 987) ndh-2 gene Proteins 0.000 abstract 2
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- 239000002184 metal Substances 0.000 description 10
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- 229910000521 B alloy Inorganic materials 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 7
- 239000000956 alloy Substances 0.000 description 7
- 238000001000 micrograph Methods 0.000 description 7
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- 230000000052 comparative effect Effects 0.000 description 5
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- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 4
- 229920002274 Nalgene Polymers 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
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- 239000007864 aqueous solution Substances 0.000 description 3
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- 239000006247 magnetic powder Substances 0.000 description 2
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- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical group [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 229910016569 AlF 3 Inorganic materials 0.000 description 1
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- 229910016509 CuF 2 Inorganic materials 0.000 description 1
- 229910005269 GaF 3 Inorganic materials 0.000 description 1
- 208000012868 Overgrowth Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
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- 230000007797 corrosion Effects 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 239000012153 distilled water Substances 0.000 description 1
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- 238000010902 jet-milling Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910001512 metal fluoride Inorganic materials 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
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- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
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- 238000007670 refining Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
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- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
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Abstract
Description
本出願は、2017年11月28日付韓国特許出願第10−2017−0160623号および2018年11月6日付韓国特許出願第10−2018−0135441号に基づいた優先権の利益を主張し、当該韓国特許出願の文献に開示されたすべての内容は本明細書の一部として含まれている。
Nd2O3 3.2679g、B 0.1000g、Fe 7.2316g、Ca 1.75159gを、粒子の粒度および大きさ制御のための金属フッ化物(CaF2,CuF2)と均一に混合する。これを任意の形のステンレススチール容器に入れて圧搾した後、混合物を不活性ガス(Ar,He)雰囲気、950℃で0.5〜6時間チューブ電気炉の中で反応させる。
実施例1で提示した方法により製造したNdFeB系粉末粒子(Nd2Fe14B)8gに、質量比10〜25%のNdH2粉末を混合する。潤滑剤としてブタノールを添加して磁場成形後、真空焼結炉で脱脂工程を150℃で1時間、300℃で1時間行った。次に、脱水素工程として650℃で1時間熱処理過程を行い、1050℃で1時間焼結した。
前記実施例2でNdH2を12.5%重量比で添加して焼結磁石を製造した。
前記実施例1で製造したNdFeB系磁性粉末にNdH2を混合せず、潤滑剤としてブタノールを添加して磁場成形後、脱脂工程を150℃で1時間、300℃で1時間行った。次に、真空焼結炉において650℃で1時間熱処理過程を行い、1050℃で1時間焼結した。
Nd2.0Fe13BGa0.01,0.05Al0.05Cu0.05を製造するために、Nd2O3 33.24g、B 1.04g、AlF3 0.40g、CuCl2 0.65g、GaF3 0.12gをナルゲンボトルに入れてペイントシェーカーで30分混合した後、ここにFe 69.96gを入れてペイントシェーカーで30分混合し、最後にCa 16.65gを入れて管状ミキサーで1時間混合する。
実施例4と同様の方法により準備したNd系粉末8gに質量比10%〜25%のNdH2粉末を混合し、潤滑剤としてブタノールを添加して磁場成形後、真空焼結炉において1050℃で1時間焼結する。
Nd2.5Fe13.3B1.1Cu0.05Al0.15を製造するために、Nd2O3 37.48g、B 1.06g、Cu 0.28g、Al 0.36gをナルゲンボトルに入れてペイントシェーカーで30分混合した後、ここにFe 66.17gを入れてペイントシェーカーで30分混合し、最後にCa 20.08gを入れて管状ミキサーで1時間混合する。
実施例6と同様の方法によりNd系粉末8gを準備する。前記方法で準備したNd系粉末8gに重量比5%のNdH2粉末を添加し、潤滑剤としてブタノールを添加して磁場成形後に、真空焼結炉において1030℃で2時間焼結する。
実施例3で製造した焼結磁石(オレンジ線)と、比較例1で製造した焼結磁石(黒線)のXRDパターンを図1に示した。また、前記実施例3で製造した焼結磁石の走査電子顕微鏡イメージを図2に示した。
NdFeB系磁石粉末とNdH2粉末の含有量比を異にし、XRDパターンおよび走査電子顕微鏡イメージを測定し、これを図3および図4に示した。
実施例2で製造した焼結磁石の保磁力、残留磁化およびBH maxを測定し、これを図5に示した。
実施例4および実施例5で製造した焼結磁石のB−Hを測定し、これを下記表1および図6に示した。また、実施例4および実施例5により製造した焼結磁石のXRD結果を図7および図8に示した。図7は実施例4により製造した焼結磁石のXRD結果であり、図8は実施例5により製造した焼結磁石のXRD結果である。
実施例6および7により製造した焼結磁石のB−Hを測定し、これを下記表2および図9、10に示した。図9は実施例6に該当し、図10は実施例7に該当する。また、実施例6および実施例7により製造した焼結磁石のXRD結果を図11および図12に示した。図11は実施例6により製造した焼結磁石のXRD結果であり、図12は実施例7により製造した焼結磁石のXRD結果である。
Claims (11)
- 還元拡散法によりNdFeB系粉末を製造する段階;
前記NdFeB系粉末と希土類水素化物粉末を混合する段階;
前記混合物を600℃〜850℃の温度で熱処理する段階;
前記熱処理した混合物を1000℃〜1100℃の温度で焼結する段階を含み、
前記希土類水素化物粉末は、NdH2またはNdH2とPrH2の混合粉末である、焼結磁石の製造方法。 - 前記NdH2とPrH2の混合粉末において、NdH2とPrH2の混合重量比は75:25〜80:20である、請求項1に記載の焼結磁石の製造方法。
- 前記熱処理した混合物を1000℃〜1100℃の温度で焼結する段階は、30分〜4時間行われる、請求項1または2に記載の焼結磁石の製造方法。
- 前記NdFeB系粉末と希土類水素化物粉末を混合する段階において、
前記希土類水素化物粉末の含有量は、1〜25重量%である、請求項1ないし3のいずれか一項に記載の焼結磁石の製造方法。 - 前記製造された焼結磁石の結晶粒の大きさは、1μm〜10μmである、請求項1ないし4のいずれか一項に記載の焼結磁石の製造方法。
- 前記混合物を600℃〜850℃の温度で熱処理する段階において、
希土類水素化物が希土類金属とH2気体に分離され、H2気体が除去される、請求項1ないし5のいずれか一項に記載の焼結磁石の製造方法。 - 前記NdFeB系粉末と希土類水素化物粉末を混合する段階において、
Cu粉末がさらに含まれる、請求項1ないし6のいずれか一項に記載の焼結磁石の製造方法。 - 前記希土類水素化物粉末と前記Cu粉末の含有量比は、7:3重量比である、請求項7に記載の焼結磁石の製造方法。
- 前記還元拡散法によりNdFeB系粉末を製造する段階は、
酸化ネオジム、ホウ素、鉄を混合して1次混合物を製造する段階:
前記1次混合物にカルシウムを添加および混合して2次混合物を製造する段階;
前記2次混合物を800℃〜1100℃の温度で加熱する段階を含む、請求項1ないし8のいずれか一項に記載の焼結磁石の製造方法。 - 請求項1ないし9のいずれか一項に記載の製造方法で製造した焼結磁石。
- Nd2Fe14Bを含み、
結晶粒の大きさが1μm〜10μmであり、
添加する希土類水素化物の含有量が10重量%〜25重量%である、焼結磁石。
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