JP7347296B2 - フェライト焼結磁石および回転電気機械 - Google Patents
フェライト焼結磁石および回転電気機械 Download PDFInfo
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- 229910000859 α-Fe Inorganic materials 0.000 title claims description 98
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 9
- 229910052791 calcium Inorganic materials 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 5
- 229910052788 barium Inorganic materials 0.000 claims description 4
- 229910052712 strontium Inorganic materials 0.000 claims description 4
- 229910052745 lead Inorganic materials 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 description 38
- 238000000465 moulding Methods 0.000 description 36
- 238000004519 manufacturing process Methods 0.000 description 25
- 238000010304 firing Methods 0.000 description 23
- 230000007423 decrease Effects 0.000 description 17
- 239000002994 raw material Substances 0.000 description 16
- 239000011651 chromium Substances 0.000 description 14
- 238000010298 pulverizing process Methods 0.000 description 14
- 239000002002 slurry Substances 0.000 description 14
- 239000000203 mixture Substances 0.000 description 11
- 238000001354 calcination Methods 0.000 description 10
- 239000011575 calcium Substances 0.000 description 9
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000003125 aqueous solvent Substances 0.000 description 6
- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 239000006247 magnetic powder Substances 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- -1 CaO Inorganic materials 0.000 description 4
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000002612 dispersion medium Substances 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 239000011572 manganese Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 229910052804 chromium Inorganic materials 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000007088 Archimedes method Methods 0.000 description 2
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 1
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 1
- RGHNJXZEOKUKBD-SQOUGZDYSA-M D-gluconate Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O RGHNJXZEOKUKBD-SQOUGZDYSA-M 0.000 description 1
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229940050410 gluconate Drugs 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000000700 radioactive tracer Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
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- H01F1/342—Oxides
- H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
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- C01G51/66—Cobaltates containing alkaline earth metals, e.g. SrCoO3
- C01G51/68—Cobaltates containing alkaline earth metals, e.g. SrCoO3 containing rare earth, e.g. La0.3Sr0.7CoO3
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Description
A,R,FeおよびCoを含み、A1-xRx(Fe12-yCoy)zO19(原子数比)と表すことができる六方晶M型フェライトを有するフェライト焼結磁石フェライト焼結磁石であり、
AはSr,BaおよびPbから選択される1種以上であり、
Rは希土類元素から選択される1種以上であり、Rとして少なくともLaを含み、
0.14≦x≦0.22
11.60≦(12-y)z≦11.99
0.13≦yz≦0.17
を満たし、
前記フェライト焼結磁石に含まれるCaを酸化物に換算したときに、CaOの含有量をMc(質量%)として、
0.30≦Mc≦0.63を満たす。
0.35≦Ms≦0.60を満たしてもよい。
0≦Mb≦0.15を満たしてもよい。
0≦Ma≦0.90を満たしてもよい。
0≦Mr≦0.10を満たしてもよい。
Aはストロンチウム(Sr),バリウム(Ba)および鉛(Pb)から選択される1種以上である。
Rは希土類元素から選択される1種以上であり、Rとして少なくともランタン(La)を含み、x、(12-y)z及びyzは以下の式を満たす。
0.14≦x≦0.22
11.60≦(12-y)z≦11.99
0.13≦yz≦0.17
0.30≦Mc≦0.63を満たす。
0.35≦Ms≦0.60を満たしてもよく、0.46≦Ms≦0.60を満たしてもよい。
0≦Mb≦0.15を満たしてもよく、0.03≦Mb≦0.15を満たしてもよく、0.03≦Mb≦0.12を満たしてもよい。
0≦Ma≦0.90を満たしてもよく、0.05≦Ma≦0.90を満たしてもよく、0.10≦Ma≦0.70を満たしてもよい。
0≦Mr≦0.10を満たしてもよく、0.05≦Mr≦0.10を満たしてもよい。
配合工程では、フェライト焼結磁石の原料を配合して、原料混合物を得る。フェライト焼結磁石の原料としては、これを構成する元素のうちの1種または2種以上を含む化合物(原料化合物)が挙げられる。原料化合物は、例えば粉末状のものが好適である。
仮焼工程では、配合工程で得られた原料混合物を仮焼する。仮焼は、例えば、空気中等の酸化性雰囲気中で行うことができる。仮焼の温度は、1100°C~1300°Cの温度範囲とすることが好ましい。仮焼の時間は、1秒~10時間とすることができる。
粉砕工程では、仮焼工程で顆粒状や塊状となった仮焼体を粉砕し、粉末状にする。これにより、後述する成形工程での成形が容易となる。粉砕工程では、前述したように、配合工程で配合しなかった原料を添加してもよい(原料の後添加)。粉砕工程は、例えば、仮焼体を粗い粉末となるように粉砕(粗粉砕)した後、これをさらに微細に粉砕(微粉砕)する2段階の工程で行ってもよい。
成形・焼成工程では、粉砕工程後に得られた粉砕材(好ましくは微粉砕材)を成形して成形体を得た後、この成形体を焼成して焼結体を得る。成形は、乾式成形、湿式成形またはCeramic Injection Molding(CIM)のいずれの方法でも行うことができる。
湿式成形法によってフェライト焼結磁石を得る場合は、上述した微粉砕工程を湿式で行うことでスラリーを得る。このスラリーを所定の濃度に濃縮して湿式成形用スラリーを得る。これを用いて成形を行うことができる。
出発原料として、SrCO3、La2O3、Fe2O3、Co3O4、CaCO3、SiO2、BaCO3、Al2O3およびCr2O3を準備し、フェライト焼結磁石の最終的な組成が表1~表9に記載された各試料の組成になるように秤量した。
この原料混合物を乾燥後、大気中、1200°Cで2時間保持する仮焼処理を行い、仮焼体を得た。
得られた仮焼体をロッドミルにて粗粉砕し、粗粉砕材を得た。次に、La2O3およびCo3O4を添加して湿式ボールミルにて微粉砕を28時間行い、スラリーを得た。得られたスラリーを固形分濃度が70~75質量%となるように調整して湿式成形用スラリーとした。
次に、湿式磁場成形機を使用して予備成形体を得た。成形圧力は、50MPa、印加磁場は800kA/mとした。また、成形時の加圧方向と磁場印加方向は、同一方向に設定した。湿式成形で得られた予備成形体は円板状であり、直径30mm、高さ15mmであった。
各実験例において最適焼結温度で焼結して得られた各フェライト焼結磁石の上下面を加工した後、25°Cの大気雰囲気中にて、最大印加磁場1989kA/mのB-Hトレーサを使用して磁気特性を測定した。結果を表1~表9に示す。本実施例では、Brが435.0mTを上回り、Hcjが345.0kA/mを上回る場合に磁気特性が良好であるとした。
最適焼成温度-10℃、最適焼成温度、最適焼成温度+10℃でそれぞれ焼成した場合におけるHcjを測定した。そして、Hcjの最大値と最小値との差をΔHcjとした。ΔHcjが小さいほど製造安定性が良好であり、ΔHcjが10.0kA/m未満である場合に製造安定性が良好である。
本実験例のコスト欄では、高コストな原料であるCoの含有量(yz)について、yz≦0.17である場合を可とし、yz>0.17である場合を不可とした。
Claims (5)
- A,R,FeおよびCoを含み、A1-xRx(Fe12-yCoy)zO19(原子数比)と表すことができる六方晶M型フェライトを有するフェライト焼結磁石であり、
AはSr,BaおよびPbから選択される1種以上であり、
Rは希土類元素から選択される1種以上であり、Rとして少なくともLaを含み、
0.14≦x≦0.22
11.60≦(12-y)z≦11.99
0.13≦yz≦0.17
を満たし、
前記フェライト焼結磁石が前記六方晶M型フェライトに加えてさらにCaおよびAlを含み、
前記フェライト焼結磁石に含まれるCaを酸化物に換算したときに、CaOの含有量をMc(質量%)とし、前記フェライト焼結磁石に含まれるAlを酸化物に換算したときに、Al 2 O 3 の含有量をMa(質量%)として、
0.30≦Mc≦0.63および0.05≦Ma≦0.90を満たすフェライト焼結磁石。 - 前記フェライト焼結磁石が前記六方晶M型フェライト、CaおよびAlに加えてさらにSiを含み、
前記フェライト焼結磁石に含まれるSiを酸化物に換算したときに、SiO2の含有量をMs(質量%)として、
0.35≦Ms≦0.60を満たす請求項1に記載のフェライト焼結磁石。 - 前記フェライト焼結磁石が前記六方晶M型フェライト、CaおよびAlに加えてさらにBaを含んでもよく、
前記フェライト焼結磁石に含まれるBaを酸化物に換算したときに、BaOの含有量をMb(質量%)として、
0≦Mb≦0.15を満たす請求項1または2に記載のフェライト焼結磁石。 - 前記フェライト焼結磁石が前記六方晶M型フェライト、CaおよびAlに加えてさらにCrを含んでもよく、
前記フェライト焼結磁石に含まれるCrを酸化物に換算したときに、Cr2O3の含有量をMr(質量%)として、
0≦Mr≦0.10を満たす請求項1~3のいずれかに記載のフェライト焼結磁石。 - 請求項1~4のいずれかに記載のフェライト焼結磁石を有する回転電気機械。
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