JP6960201B2 - Nd−Fe−B系焼結永久磁性体の製造方法 - Google Patents
Nd−Fe−B系焼結永久磁性体の製造方法 Download PDFInfo
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims description 149
- 239000000696 magnetic material Substances 0.000 title claims description 76
- 238000000034 method Methods 0.000 title claims description 36
- 238000004519 manufacturing process Methods 0.000 title claims description 20
- 239000000843 powder Substances 0.000 claims description 162
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 44
- 238000002156 mixing Methods 0.000 claims description 34
- 239000002245 particle Substances 0.000 claims description 28
- 238000003723 Smelting Methods 0.000 claims description 27
- 239000000956 alloy Substances 0.000 claims description 23
- 229910052786 argon Inorganic materials 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 22
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 20
- 239000000314 lubricant Substances 0.000 claims description 14
- 238000000748 compression moulding Methods 0.000 claims description 13
- 238000005266 casting Methods 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 10
- 150000002910 rare earth metals Chemical class 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 229910052779 Neodymium Inorganic materials 0.000 claims description 8
- 229910052771 Terbium Inorganic materials 0.000 claims description 7
- 239000011247 coating layer Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 238000005496 tempering Methods 0.000 claims description 6
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 239000003607 modifier Substances 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 229910052758 niobium Inorganic materials 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000003870 refractory metal Substances 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 24
- 229910001873 dinitrogen Inorganic materials 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 22
- 229910045601 alloy Inorganic materials 0.000 description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 17
- 230000001681 protective effect Effects 0.000 description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 10
- 238000005119 centrifugation Methods 0.000 description 10
- 239000001257 hydrogen Substances 0.000 description 10
- 229910052739 hydrogen Inorganic materials 0.000 description 10
- 239000012535 impurity Substances 0.000 description 10
- 239000000758 substrate Substances 0.000 description 10
- 239000013078 crystal Substances 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- 238000009826 distribution Methods 0.000 description 7
- 230000004907 flux Effects 0.000 description 7
- 238000000576 coating method Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 230000001965 increasing effect Effects 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 5
- 238000009792 diffusion process Methods 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
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- 239000010410 layer Substances 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 235000002905 Rumex vesicarius Nutrition 0.000 description 1
- 244000207667 Rumex vesicarius Species 0.000 description 1
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- 238000009499 grossing Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
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- 230000003647 oxidation Effects 0.000 description 1
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- 238000011084 recovery Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
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- 239000002344 surface layer Substances 0.000 description 1
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Description
(工程A)ストリップキャスト法を用いてNd−Fe−B系薄片を製造し、水素化処理、ジェットミルによってNd−Fe−B系粉末を製造し、
(工程B)ナノ改質粉末を前記Nd−Fe−B系粉末に添加・混合して混合粉末とし、前記ナノ改質粉末の重量は、前記Nd−Fe−B系粉末の重量に対して0.1〜3%であり、
(工程C)前記混合粉末を混合装置内へ投入し、不活性ガスを充填し、回転速度を350〜8000rpm、回転時間を5〜180分、温度を25〜500℃として混合し、前記混合粉末を球体化するとともにナノコーティングNd−Fe−B系粉末とし、
(工程D)前記ナノコーティングNd−Fe−B系粉末を圧縮成形処理、焼結処理及び時効処理を行い、最終的なNd−Fe−B系焼結永久磁性体を得る、ことを特徴とする。
質量%による各成分の組成は、REの含有量をa、Bの含有量をb、Mの含有量をcとした場合、それぞれの含有量は、
28%≦a≦32%、
0.8%≦b≦1.2%、
c≦5%であり、
Feの含有量は100−a−b−cであり、
溶錬工程は、アルゴンガスの保護条件下において溶錬され、溶錬温度は1350℃〜1500℃である、ことを特徴とする。
前記ナノ改質粉末の成分は、重希土類粉末又は低融点金属粉末又は高融点金属粉末のいずれか一つ又は複数であり、前記重希土類粉末はDy、Tbのいずれか一つ又は二つであり、前記低融点金属粉末はM1又は希土類合金材料RE−M1であり、REはPr、Nd、Dy、Tbのうちの一つ又は複数であり、M1はAl、Cu、Mg、Znのうちの一つ又は複数であり、前記高融点金属粉末はM2又はその酸化物であり、M2はTi、Zr、Nb、Moのうちの一つ又は複数である、ことを特徴とする。
ストリップキャスト法によりNd−Fe−B系薄片を製造した。各成分は、PrNd:32重量%、Co:1.0重量%、Al:0.35重量%、Ti:0.1重量%、B:1.0重量%、余りはFe及び不可避な不純物元素である。原料を配合した後、溶錬合金遠心分離法でNd−Fe−B系薄片を製造した。溶錬温度は1450℃であり、Nd−Fe−B系薄片の厚みを0.25〜0.35mmとした。
実施例1と対比する比較例1を作成した。比較例1はナノCu粉を添加する機械混合工程を行わない磁性体として製造した。具体的な方法は、下記のとおりである。
ストリップキャスト法によりNd−Fe−B系薄片を製造した。各成分は、PrNd:29.5重量%、Co:1.0重量%、Ga:0.2重量%、B:1.0重量%、余りはFe及び不可避な不純物元素である。原料を配合した後に、溶錬合金遠心分離法でNd−Fe−B系薄片を製造した。溶錬温度は1450℃であり、Nd−Fe−B系薄片の厚みを0.25〜0.35mmとした。
実施例2と対比する比較例2を作成した。比較例2はナノ改質粉末を添加する機械混合工程を行わない磁性体として製造した。具体的な方法は下記のとおりである。
ストリップキャスト法によりNd−Fe−B系薄片を製造した。各成分は、Nd:29重量%、Co:1.0重量%、Al:0.1重量%、Cu:0.1重量%、B:1.0重量%、余りはFe及び不可避な不純物元素である。原料を配合した後に、溶錬合金遠心分離法でNd−Fe−B系薄片を製造した。溶錬温度は1450℃であり、Nd−Fe−B系薄片の厚みを0.25〜0.35mmとした。
実施例3と対比する比較例3を作成した。比較例3はナノCu粉を添加する機械混合工程を行わない磁性体として製造した。具体的な方法は以下のとおりである。
ストリップキャストによりNd−Fe−B系薄片を製造した。各成分は、Nd:29.8重量%、Co:1.5重量%、Cu:0.15重量%、Ga:0.2重量%、Ti:0.1重量%、B:1.0重量%、余りはFe及び不可避な不純物元素である。原料を配合した後に、溶錬合金遠心分離法でNd−Fe−B系薄片を製造した。溶錬温度は1480℃であり、Nd−Fe−B系薄片の厚みを0.25〜0.35mmとした。
実施例4と対比する比較例4を作成した。比較例4は、ナノTb粉を添加する機械混合工程を行わない磁性体として製造した。具体的な方法は以下のとおりである。
ストリップキャスト法によりNd−Fe−B系薄片を製造した。各成分は、PrNd:29.5重量%、Co:1.0重量%、Al:0.1重量%、Cu:0.1重量%、B:1.0重量%、余りはFe及び不可避な不純物元素である。原料を配合した後に、溶錬合金遠心分離法でNd−Fe−B系薄片を製造した。溶錬温度は1450℃であり、Nd−Fe−B系薄片の厚みを0.25〜0.35mmとした。
実施例5と対比する比較例5を作成した。比較例5はナノPr68Cu32合金粉を添加する機械混合工程を行わない磁性体として製造した。具体的な方法は以下のとおりである。
実施例5との相違点は、添加したナノPr68Cu32合金粉のNd−Fe−B系粒子との重量比が1%である点であり、その他の条件は実施例5と同じである。測定結果を表6に示す。
実施例5との相違点は、添加したナノPr68Cu32合金粉のNd−Fe−B系粒子との重量比が1.5%である点であり、その他の条件は実施例5と同じである。測定結果を表6に示す。
実施例5との相違点は、添加したナノPr68Cu32合金粉のNd−Fe−B系粒子との重量比が2%である点であり、その他の条件は実施例5と同じである。測定結果を表6に示す。
Claims (9)
- Nd−Fe−B系焼結永久磁性体の製造方法であって、
(工程A)ストリップキャスト法を用いてNd−Fe−B系薄片を製造し、水素化処理、ジェットミルによってNd−Fe−B系粉末を製造し、
(工程B)ナノ改質粉末を前記Nd−Fe−B系粉末に添加・混合して混合粉末とし、前記ナノ改質粉末の重量は、前記Nd−Fe−B系粉末の重量に対して0.1〜3%であり、
前記ナノ改質粉末の粒子径は、20〜100nmであり、
前記ナノ改質粉末の成分は、重希土類粉末又は低融点金属粉末又は高融点金属粉末のいずれか一つ又は複数であり、前記重希土類粉末はDy、Tbのいずれか一つ又は二つであり、前記低融点金属粉末はM 1 又は希土類合金材料RE−M 1 であり、REはPr、Nd、Dy、Tbのうちの一つ又は複数であり、M 1 はAl、Cu、Mg、Znのうちの一つ又は複数であり、前記高融点金属粉末はM 2 又はその酸化物であり、M 2 はTi、Zr、Nb、Moのうちの一つ又は複数であり、
(工程C)前記混合粉末を混合装置内へ投入し、不活性ガスを充填し、回転速度を350〜8000rpm、回転時間を5〜180分、温度を25〜500℃として混合し、前記混合粉末を球体化するとともにナノコーティングNd−Fe−B系粉末とし、
(工程D)前記ナノコーティングNd−Fe−B系粉末を圧縮成形処理、焼結処理及び時効処理を行い、最終的なNd−Fe−B系焼結永久磁性体を得る、
ことを特徴とするNd−Fe−B系焼結永久磁性体の製造方法。 - 前記Nd−Fe−B系薄片は、原料としてNd、Fe及びBを配合して溶錬し、Nd−Fe−B成分はRE、Fe、B、Mを含み、REはNd、Pr、Dy、Tbのうちの一つ又は複数の混合であり、MはAl、Cu、Mg、Zn、Co、Ti、Zr、Nb、Moのうちの一つ又は複数の混合であり、
質量%による各成分の組成は、REの含有量をa、Bの含有量をb、Mの含有量をcとした場合、それぞれの含有量は、
28%≦a≦32%、
0.8%≦b≦1.2%、
c≦5%であり、
Feの含有量は100−a−b−cであり、
溶錬工程は、アルゴンガスの保護条件下において溶錬され、溶錬温度は1350℃〜1500℃である、
ことを特徴とする請求項1に記載のNd−Fe−B系焼結永久磁性体の製造方法。 - 前記(工程A)において、前記ジェットミルによって粉砕された前記Nd−Fe−B系粉末の粒子径は2.5〜5μmである、
ことを特徴とする請求項1又は2に記載のNd−Fe−B系焼結永久磁性体の製造方法。 - 前記(工程B)において製造される前記混合粉末は、前記ナノ改質粉末と前記Nd−Fe−B系粉末を三次元混合機で0.5〜3時間混合したものである、
ことを特徴とする請求項1ないし3のいずれか1項に記載のNd−Fe−B系焼結永久磁性体の製造方法。 - 前記(工程C)の混合工程において、前記ナノコーティングNd−Fe−B系粉末の表面が研磨されて球体化し、前記ナノ改質剤を前記Nd−Fe−B系粉末の粒子表面に均等に分布させてコーティング層を形成する、
ことを特徴とする請求項1ないし4のいずれか1項に記載のNd−Fe−B系焼結永久磁性体の製造方法。 - 前記(工程C)の混合工程において、前記ナノコーティングNd−Fe−B系粉末に潤滑剤を更に添加して1〜3時間混合し、前記潤滑剤の質量は、前記ナノコーティングNd−Fe−B系粉末の質量の0.05〜0.2%である、
ことを特徴とする請求項1ないし5のいずれか1項に記載のNd−Fe−B系焼結永久磁性体の製造方法。 - 前記(工程D)において、前記ナノコーティングNd−Fe−B系粉末は、1.8〜2.5Tの磁場で配向し圧縮成形される、
ことを特徴とする請求項1ないし6のいずれか1項に記載のNd−Fe−B系焼結永久磁性体の製造方法。 - 前記(工程D)において、前記焼結処理は真空焼結炉内で行われ、焼結温度は950〜1100℃であり、焼結時間は6〜12時間である、
ことを特徴とする請求項1ないし7のいずれか1項に記載のNd−Fe−B系焼結永久磁性体の製造方法。 - 前記(工程D)において、前記時効処理は2段階の焼き戻し処理であり、第1の焼き戻し処理は850〜900℃で3〜5時間行われ、第2の焼き戻し処理は460〜700℃で3〜6時間行われる、
ことを特徴とする請求項1ないし8のいずれか1項に記載のNd−Fe−B系焼結永久磁性体の製造方法。
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