JP5261747B2 - 永久磁石及び永久磁石の製造方法 - Google Patents
永久磁石及び永久磁石の製造方法 Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 238000000034 method Methods 0.000 title description 15
- 150000001875 compounds Chemical class 0.000 claims description 53
- 239000002994 raw material Substances 0.000 claims description 28
- 239000002002 slurry Substances 0.000 claims description 26
- 238000005245 sintering Methods 0.000 claims description 22
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 18
- 230000003449 preventive effect Effects 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 10
- 238000000748 compression moulding Methods 0.000 claims description 5
- 239000003921 oil Substances 0.000 description 29
- 239000000843 powder Substances 0.000 description 26
- 239000002245 particle Substances 0.000 description 24
- 229910052692 Dysprosium Inorganic materials 0.000 description 23
- 230000005291 magnetic effect Effects 0.000 description 23
- 229910052771 Terbium Inorganic materials 0.000 description 17
- 239000010419 fine particle Substances 0.000 description 13
- 230000005415 magnetization Effects 0.000 description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 8
- -1 neodymium (III) acetylacetonate trihydrate Chemical class 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- 238000000465 moulding Methods 0.000 description 7
- 238000010298 pulverizing process Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 229910001172 neodymium magnet Inorganic materials 0.000 description 5
- 229910052761 rare earth metal Inorganic materials 0.000 description 5
- 239000003302 ferromagnetic material Substances 0.000 description 4
- 239000006104 solid solution Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 230000005381 magnetic domain Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000011859 microparticle Substances 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- JQBILSNVGUAPMM-UHFFFAOYSA-K terbium(3+);triacetate Chemical compound [Tb+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JQBILSNVGUAPMM-UHFFFAOYSA-K 0.000 description 2
- GFISHBQNVWAVFU-UHFFFAOYSA-K terbium(iii) chloride Chemical compound Cl[Tb](Cl)Cl GFISHBQNVWAVFU-UHFFFAOYSA-K 0.000 description 2
- LKNRQYTYDPPUOX-UHFFFAOYSA-K trifluoroterbium Chemical compound F[Tb](F)F LKNRQYTYDPPUOX-UHFFFAOYSA-K 0.000 description 2
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 1
- QBKTXRLYEHZACW-UHFFFAOYSA-K 2-ethylhexanoate;neodymium(3+) Chemical compound [Nd+3].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O QBKTXRLYEHZACW-UHFFFAOYSA-K 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 150000001217 Terbium Chemical class 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 150000004683 dihydrates Chemical class 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 150000004687 hexahydrates Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- DZVCFNFOPIZQKX-LTHRDKTGSA-M merocyanine Chemical compound [Na+].O=C1N(CCCC)C(=O)N(CCCC)C(=O)C1=C\C=C\C=C/1N(CCCS([O-])(=O)=O)C2=CC=CC=C2O\1 DZVCFNFOPIZQKX-LTHRDKTGSA-M 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- HZHUIQPXRWTHNF-UHFFFAOYSA-N neodymium(3+);propan-2-olate Chemical compound [Nd+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] HZHUIQPXRWTHNF-UHFFFAOYSA-N 0.000 description 1
- GMQPBTKWMZBSCT-UHFFFAOYSA-K neodymium(3+);triacetate;hydrate Chemical compound O.[Nd+3].CC([O-])=O.CC([O-])=O.CC([O-])=O GMQPBTKWMZBSCT-UHFFFAOYSA-K 0.000 description 1
- WYRSPTDNOIZOGA-UHFFFAOYSA-K neodymium(3+);trifluoromethanesulfonate Chemical compound [Nd+3].[O-]S(=O)(=O)C(F)(F)F.[O-]S(=O)(=O)C(F)(F)F.[O-]S(=O)(=O)C(F)(F)F WYRSPTDNOIZOGA-UHFFFAOYSA-K 0.000 description 1
- AIKYQURCXXBRLQ-UHFFFAOYSA-H oxalate terbium(3+) hexahydrate Chemical compound O.O.O.O.O.O.C(C(=O)[O-])(=O)[O-].[Tb+3].C(C(=O)[O-])(=O)[O-].C(C(=O)[O-])(=O)[O-].[Tb+3] AIKYQURCXXBRLQ-UHFFFAOYSA-H 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- LMEHHJBYKPTNLM-UHFFFAOYSA-H terbium(3+);tricarbonate Chemical compound [Tb+3].[Tb+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O LMEHHJBYKPTNLM-UHFFFAOYSA-H 0.000 description 1
- UTCARTSNNKGRTD-UHFFFAOYSA-N terbium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Tb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O UTCARTSNNKGRTD-UHFFFAOYSA-N 0.000 description 1
- OTUDGWGELZRVRY-UHFFFAOYSA-N terbium(3+);trisulfide Chemical compound [S-2].[S-2].[S-2].[Tb+3].[Tb+3] OTUDGWGELZRVRY-UHFFFAOYSA-N 0.000 description 1
- AZNZWHYYEIQIOC-UHFFFAOYSA-K terbium(iii) bromide Chemical compound [Br-].[Br-].[Br-].[Tb+3] AZNZWHYYEIQIOC-UHFFFAOYSA-K 0.000 description 1
- 150000004685 tetrahydrates Chemical class 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000010947 wet-dispersion method Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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Description
また、上記のように添加したDyが磁石粒子内に固溶化すると、磁石の残留磁化が低下する原因となっていた。
そこで、微量のDyによって残留磁化を低下させることなく磁石の保磁力を大きく向上させる技術が望まれていた。
また、Dy化合物又はTb化合物が、焼結後に磁石原料の粒界に偏在しているので、DyやTbの使用量を減少させつつもDy又はTbによる保磁力の向上を十分に図ることが可能となる。
また、Dy化合物又はTb化合物が、焼結後に磁石原料の粒界に偏在しているので、DyやTbの使用量を減少させつつもDy又はTbによる保磁力の向上を十分に図ることが可能となる。
先ず、図1〜図4を用いて永久磁石1の構成について説明する。
本実施形態に係る永久磁石1はNd−Fe−B系磁石である。また、永久磁石1の保磁力を高める為のDy(ジスプロシウム)が添加されている。尚、各成分の含有量はNd:27〜30wt%、Dy化合物に含まれるDy成分(又はTb化合物に含まれるTb成分):0.01〜8wt%、B:1〜2wt%、Fe(電解鉄):60〜70wt%とする。また、本実施形態に係る永久磁石1は、図1に示すように円柱形状を備えるが、永久磁石1の形状は成形に用いるキャビティの形状によって変化する。図1は本実施形態に係る永久磁石1を示した全体図である。
図3に示すように永久磁石の保磁力は、磁化された状態から逆方向への磁場を加えていった際に、磁気分極を0にする(即ち、磁化反転する)のに必要な磁場の強さである。従って、磁化反転を抑制することができれば、高い保磁力を得ることができる。尚、磁性体の磁化過程には、磁気モーメントの回転に基づく回転磁化と、磁区の境界である磁壁(90°磁壁と180°磁壁からなる)が移動する磁壁移動がある。
また、本実施形態では圧縮成形により成形された成形体を適切な焼成条件で焼成すれば、Dyが磁石粒子35内へと拡散浸透(固溶化)することを防止できる。ここで、Dyが磁石粒子35内へと拡散浸透すると、その磁石の残留磁化(磁場の強さを0にしたときの磁化)が低下することが知られている。従って、本実施形態では、永久磁石1の残留磁化が低下することを防止できる。
尚、Dy層36はDy化合物のみから構成される層である必要はなく、Dy化合物とNd化合物との混合体からなる層であっても良い。その場合には、Nd化合物を添加することによって、Dy化合物とNd化合物との混合体からなる層を形成する。その結果、Nd磁石粉末の焼結時の液相焼結を助長することができる。尚、添加するNd化合物としては、酢酸ネオジム水和物、ネオジム(III)アセチルアセトナート三水和物、2−エチルヘキサン酸ネオジム(III)、ネオジム(III)ヘキサフルオロアセチルアセトナート二水和物、ネオジムイソプロポキシド、リン酸ネオジニウム(III)n水和物、ネオジムトリフルオロアセチルアセトナート、トリフルオロメタンスルホン酸ネオジム等が望ましい。また、添加するTb化合物としては、酢酸テルビウム(III)n水和物、酢酸テルビウム(III)四水和物、テルビウム(III)アセチルアセトナート三水和物、シュウ酸テルビウム(III)六水和物、臭化テルビウム(III)、炭酸テルビウム(III)n水和物、塩化テルビウム(III)無水、塩化テルビウム(III)六水和物、ふっ化テルビウム(III)、ふっ化酸化テルビウム、水素化テルビウム(III)、硝酸テルビウム(III)六水和物、硫化テルビウムが望ましい。
更に、Dy化合物の替わりにDy微粒子やTb微粒子が溶解された防錆オイルを微粉砕された磁石粉末に混合することによっても、同様に永久磁石1の保磁力を向上させることが可能である。Dy微粒子を溶解した場合には、Nd磁石粒子35の表面にDy微粒子が付着し、Dyの層が形成される。一方、Tb微粒子を溶解した場合には、Nd磁石粒子35の表面にTb微粒子が付着し、Tbの層が形成される。
次に、本実施形態に係る永久磁石1の製造方法について図5を用いて説明する。図5は本実施形態に係る永久磁石1の製造工程を示した説明図である。
また、溶媒に非可溶でも、微粒子に粉砕したDy又はDy化合物を湿式分散時に添加し、均一分散する事でNd磁石粒子表面に均一付着させることが可能となる。
また、溶解させるDy化合物の量は特に制限されないが、磁石粉末に対してDy化合物に含まれるDy成分が0.01〜8wt%となる量とするのが好ましい。
尚、Dy化合物の代わりにTb化合物、Dy微粒子、Tb微粒子を防錆オイルに溶解させることとしても良い。
また、成形装置50には一対の磁界発生コイル55、56がキャビティ54の上下位置に配置されており、磁力線をキャビティ54に充填されたスラリー42に印加する。また、モールド51にはキャビティ54に開口するスラリー注入孔57が設けられている。
また、キャビティ54に磁場を印加しながらスラリーを注入し、注入途中又は注入終了後に、当初の磁場より強い磁場を印加して湿式成形しても良い。また、加圧方向に対して印加方向が垂直となるように磁界発生コイル55、56を配置しても良い。
また、混合した防錆オイル中に溶解された微量のDy化合物(又はTb化合物、Dy微粒子、Tb微粒子のいずれか)を磁石粒子の粒界に偏在配置することが可能となり、DyやTbの使用量を減少させつつもDy又はTbによる保磁力の向上を十分に図ることが可能となる。
更に、成形体を適切な焼成条件で焼成すれば、DyやTbが磁石粒子内に固溶化することを防止できる。従って、磁石の残留磁化が低下することを防止できる。
また、磁石粉末の粉砕条件、混練条件、焼結条件などは上記実施例に記載した条件に限られるものではない。
35 Nd磁石粒子
36 Dy層
42 スラリー
Claims (2)
- 磁石原料を粉砕する工程と、
前記粉砕された磁石原料と、Dy化合物又はTb化合物が溶解された防錆オイルとを混合してスラリーを生成する工程と、
前記スラリーを圧縮成形することで成形体を形成する工程と、
前記成形体を焼結する工程と、により製造され、
前記Dy化合物又はTb化合物が、焼結後に前記磁石原料の粒界に偏在していることを特徴とする永久磁石。 - 磁石原料を粉砕する工程と、
前記粉砕された磁石原料と、Dy化合物又はTb化合物が溶解された防錆オイルとを混合してスラリーを生成する工程と、
前記スラリーを圧縮成形することで成形体を形成する工程と、
前記成形体を焼結する工程と、を有し、
前記Dy化合物又はTb化合物が、焼結後に前記磁石原料の粒界に偏在した永久磁石を製造することを特徴とする永久磁石の製造方法。
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US12/937,870 US20110043311A1 (en) | 2008-04-15 | 2009-04-14 | Permanent magnet and process for producing permanent magnet |
EP09731890A EP2267733A4 (en) | 2008-04-15 | 2009-04-14 | PERMANENT MAGNET AND METHOD FOR MANUFACTURING PERMANENT MAGNET |
PCT/JP2009/057532 WO2009128460A1 (ja) | 2008-04-15 | 2009-04-14 | 永久磁石及び永久磁石の製造方法 |
CN200980113297XA CN102007548A (zh) | 2008-04-15 | 2009-04-14 | 永久磁铁和永久磁铁的制造方法 |
KR1020107023115A KR101479373B1 (ko) | 2008-04-15 | 2009-04-14 | 영구 자석 및 영구 자석의 제조 방법 |
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EP2503571B1 (en) * | 2010-03-31 | 2015-05-06 | Nitto Denko Corporation | Manufacturing method for permanent magnet |
JP2011216720A (ja) * | 2010-03-31 | 2011-10-27 | Nitto Denko Corp | 永久磁石及び永久磁石の製造方法 |
JP5501829B2 (ja) * | 2010-03-31 | 2014-05-28 | 日東電工株式会社 | 希土類永久磁石の製造方法 |
WO2011125584A1 (ja) * | 2010-03-31 | 2011-10-13 | 日東電工株式会社 | 永久磁石及び永久磁石の製造方法 |
JP2011216732A (ja) * | 2010-03-31 | 2011-10-27 | Nitto Denko Corp | 永久磁石及び永久磁石の製造方法 |
JP2011216724A (ja) * | 2010-03-31 | 2011-10-27 | Nitto Denko Corp | 永久磁石及び永久磁石の製造方法 |
CN102549685B (zh) * | 2010-03-31 | 2014-04-02 | 日东电工株式会社 | 永久磁铁及永久磁铁的制造方法 |
JP5501827B2 (ja) * | 2010-03-31 | 2014-05-28 | 日東電工株式会社 | 永久磁石及び永久磁石の製造方法 |
JP5501834B2 (ja) * | 2010-03-31 | 2014-05-28 | 日東電工株式会社 | 永久磁石及び永久磁石の製造方法 |
CN102842399B (zh) * | 2011-06-23 | 2016-04-13 | 比亚迪股份有限公司 | 一种钕铁硼永磁材料及其制备方法 |
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US9468972B2 (en) * | 2011-09-30 | 2016-10-18 | Gm Global Technology Operations, Llc | Method of making Nd—Fe—B sintered magnets with reduced dysprosium or terbium |
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