CN113436823A - 铁氧体烧结磁铁 - Google Patents
铁氧体烧结磁铁 Download PDFInfo
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- CN113436823A CN113436823A CN202110300566.6A CN202110300566A CN113436823A CN 113436823 A CN113436823 A CN 113436823A CN 202110300566 A CN202110300566 A CN 202110300566A CN 113436823 A CN113436823 A CN 113436823A
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- Prior art keywords
- mass
- sintered magnet
- ferrite sintered
- ferrite
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 105
- 229910052788 barium Inorganic materials 0.000 claims description 11
- 229910052712 strontium Inorganic materials 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 9
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052681 coesite Inorganic materials 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052682 stishovite Inorganic materials 0.000 claims description 4
- 229910052905 tridymite Inorganic materials 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 description 51
- 238000000465 moulding Methods 0.000 description 38
- 238000000034 method Methods 0.000 description 21
- 239000000203 mixture Substances 0.000 description 20
- 239000011777 magnesium Substances 0.000 description 16
- 238000010298 pulverizing process Methods 0.000 description 16
- 239000002994 raw material Substances 0.000 description 15
- 239000002002 slurry Substances 0.000 description 15
- 238000010304 firing Methods 0.000 description 14
- 238000001354 calcination Methods 0.000 description 10
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- 238000001878 scanning electron micrograph Methods 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 239000000395 magnesium oxide Substances 0.000 description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 8
- 239000011575 calcium Substances 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 239000006247 magnetic powder Substances 0.000 description 5
- 230000005415 magnetization Effects 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 4
- 239000002612 dispersion medium Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 239000011572 manganese Substances 0.000 description 4
- 238000011282 treatment Methods 0.000 description 4
- 239000003125 aqueous solvent Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
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- 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
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 2
- 229910000018 strontium carbonate Inorganic materials 0.000 description 2
- 239000008096 xylene Substances 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
- 238000007088 Archimedes method Methods 0.000 description 1
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
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- 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
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-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
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000013528 artificial neural network Methods 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005238 degreasing Methods 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 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
- 229910052746 lanthanum Inorganic materials 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
- 230000005381 magnetic domain Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 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
- 230000003647 oxidation Effects 0.000 description 1
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- 230000001590 oxidative effect Effects 0.000 description 1
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- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
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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
- H01F1/10—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 non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
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- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B35/6262—Milling of calcined, sintered clinker or ceramics
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- 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
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- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
本发明涉及得到一种在维持高的HcJ的状态下进一步提高了Br的铁氧体烧结磁铁。所述铁氧体烧结磁铁包含以MgO换算为0.010质量％以上0.090质量％以下的Mg。
Description
技术领域
本发明涉及一种铁氧体烧结磁铁。
背景技术
专利文献1及2中记载了通过用Mg取代Fe的一部分等的结构，从而改善了磁特性的铁氧体烧结磁铁。
现有技术文献
专利文献
专利文献1：日本专利第5521622号公报
专利文献2：日本专利第4543849号公报
发明内容
发明所要解决的技术问题
本发明的目的在于得到一种在维持高的矫顽力(HcJ)的状态下进一步提高剩余磁通密度(Br)的铁氧体烧结磁铁。
用于解决技术问题的技术方案
为了实现上述目的，本发明的铁氧体烧结磁铁包含以MgO换算为0.010质量％以上0.090质量％以下的Mg。
本发明的铁氧体烧结磁铁通过具有上述的特征，成为在维持高的HcJ的状态下提高了Br的铁氧体烧结磁铁。
所述铁氧体烧结磁铁也可以包含Ca、R、A、Fe及Co，由Ca1-w-xRwAxFezCom(原子数比)表示组成式时，
R为选自稀土元素中的1种以上，并且至少包含La，
A为选自Ba及Sr中的1种以上，并且
满足：
0.364≤w≤0.495、
0.038≤x≤0.136、
8.280≤z≤10.45、
0.257≤m≤0.338。
所述铁氧体烧结磁铁也可以包含Ca、R、A、Fe及Co，由Ca1-w-xRwAxFezCom(原子数比)表示组成式时，
R为选自稀土元素中的1种以上，并且至少包含La，
A为选自Ba及Sr中的1种以上，
并且满足：
0.459≤w≤0.474、
0.054≤x≤0.120、
9.837≤z≤9.934、
0.293≤m≤0.311。
所述铁氧体烧结磁铁也可以包含Ca、R、A、Fe及Co，
R为选自稀土元素中的1种以上，并且至少包含La，
A为选自Ba及Sr中的1种以上，
也可以包含以CaO换算为2.505质量％以上2.951质量％以下的Ca、以R2O3换算为8.028质量％以上8.239质量％以下的R、以AO换算为0.666质量％以上1.666质量％以下的A、以Fe2O3换算为84.564质量％以上84.937质量％以下的Fe、以CoO换算为2.341质量％以上2.521质量％以下的Co。
也可以包含以B2O3换算为0.005质量％以上0.058质量％以下的B。
也可以包含以Al2O3换算为0.049质量％以上0.065质量％以下的Al。
也可以包含以SiO2换算为0.315质量％以上0.353质量％以下的Si。
也可以包含以MnO换算为0.288质量％以上0.341质量％以下的Mn。
具体实施方式
以下，基于实施方式对本发明进行说明。
本实施方式的铁氧体烧结磁铁包含以氧化镁(MgO)换算为0.010质量％以上0.090质量％以下的镁(Mg)。可以包含0.020质量％以上0.070质量％以下，也可以包含0.034质量％以上0.052质量％以下。本实施方式的铁氧体烧结磁铁通过在上述的范围内含有Mg，从而能够在维持高的HcJ状态下进一步提高Br。
以下，对通过控制Mg的含量，在维持高的HcJ的状态下进一步提高Br的机理进行说明。
本实施方式的铁氧体烧结磁铁包含铁氧体颗粒。对铁氧体颗粒的晶体结构没有特别限定，铁氧体颗粒也可以为具有六方晶结构的结晶颗粒。另外，结晶颗粒也可以具有磁铅石型的晶体结构。铁氧体烧结磁铁由铁氧体颗粒和晶界构成。
铁氧体烧结磁铁在与易磁化轴平行的截面中，铁氧体颗粒的圆形度越小，则铁氧体颗粒的扁平程度越高，铁氧体颗粒越接近板状。其结果，铁氧体颗粒容易在一定方向上取向，且磁化的方向朝向一定方向。而且，磁场取向度变大，Br提高。在此，本发明者们发现Mg的含量越多，铁氧体颗粒的圆形度越小。
但是，Mg为非磁性的。因此，如果Mg的含量过多，则磁特性容易降低。进而，如果铁氧体颗粒的圆形度过小，则铁氧体颗粒更偏平。铁氧体颗粒越偏平，则铁氧体颗粒越容易变大。而且，偏平的大的铁氧体颗粒容易成为多磁畴颗粒。多磁畴颗粒是在一个颗粒内具有多个磁畴的颗粒。通过铁氧体颗粒中多磁畴颗粒所占的比例增加，磁取向度变小，Br降低。进而，反向磁场变大，HcJ也降低。
因此，本发明者们发现：通过将Mg的含量设为上述的范围内，从而在维持高的HcJ的状态下，能进一步提高Br。
以下，对本实施方式的铁氧体烧结磁铁的组成进行进一步地说明。
如上所述，铁氧体烧结磁铁包含Mg。铁氧体烧结磁铁包含以氧化镁(MgO)换算为0.010质量％以上0.090质量％以下的镁(Mg)。可以包含0.020质量％以上0.070质量％以下，也可以包含0.034质量％以上0.052质量％以下。对于Mg以外的组成没有特别限定。优选为可以得到具有六方晶结构的铁氧体颗粒的组成。
例如，铁氧体烧结磁铁可以包含钙(Ca)、R、A、铁(Fe)及钴(Co)。在由Ca1-w- xRwAxFezCom(原子数比)表示组成式时，
R可以为选自稀土元素中的1种以上，并且至少包含镧(La)。
A为选自钡(Ba)及锶(Sr)中的1种以上。
上述组成式的w、x、z、m可以为满足以下的范围的组成。
0.364≤w≤0.495
0.038≤x≤0.136
8.280≤z≤10.45
0.257≤m≤0.338
R的含量(w)也可以满足0.415≤w≤0.485，也可以满足0.459≤w≤0.474。A的含量(x)也可以满足0.046≤x≤0.128，也可以满足0.054≤x≤0.120。Fe的含量(z)也可以满足9.100≤z≤10.20，也可以满足9.837≤z≤9.934。Co的含量(m)也可以满足0.278≤m≤0.327，也可以满足0.293≤m≤0.311。
另外，将R整体设为100at％，可以包含90at％以上的La。通过R中La所占的比例为上述的范围内，容易提高磁各向异性。另外，R也可以单独为La。由此，能够减少元素的种类，能够减少制造的操作负荷及制造成本。
另外，如果以氧化物换算后的质量比例表达，则将铁氧体烧结磁铁整体设为100质量％，
R为选自稀土元素中的1种以上，并且至少包含La，
A为选自Ba及Sr中的1种以上，
可以为包含：以CaO换算为2.505质量％以上2.951质量％以下的Ca、以R2O3换算为8.028质量％以上8.239质量％以下的R、以AO换算为0.666质量％以上1.666质量％以下的A、以Fe2O3换算为84.564质量％以上84.937质量％以下的Fe、以CoO换算为2.341质量％以上2.521质量％以下的Co的组成。
A为选自Ba及Sr中的至少1种的元素。本实施方式的铁氧体烧结磁铁可以包含Ba及Sr两者作为A，也可以仅包含Ba或仅包含Sr作为A。
通过Ca、R、A、Fe及Co的含量为上述的范围内，容易得到高的Br及HcJ。
进而，可以包含以氧化硼(B2O3)换算为0.005质量％以上0.058质量％以下的硼(B)，也可以包含0.015质量％以上0.048质量％以下，也可以包含0.022质量％以上0.041质量％以下。通过在上述的范围内包含B，容易提高Br及HcJ。
进而，可以包含以氧化铝(Al2O3)换算为0.010质量％以上0.160质量％以下的铝(Al)，也可以包含0.035质量％以上0.110质量％以下，也可以包含0.049质量％以上0.065质量％以下。通过在上述的范围内包含Al，容易提高Br及HcJ。
进而，可以包含以氧化硅(SiO2)换算为0.102质量％以上0.752质量％以下的硅(Si)，也可以包含0.224质量％以上0.603质量％以下，也可以包含0.315质量％以上0.353质量％以下。通过在上述的范围内包含Si，容易提高Br及HcJ。
进而，可以包含以氧化锰(MnO)换算为0.010质量％以上0.450质量％以下的锰(Mn)，也可以包含0.220质量％以上0.439质量％以下，也可以包含0.288质量％以上0.341质量％以下。通过在上述的范围内包含Mn，容易提高Br及HcJ。
以下，对圆形度的平均值的算出方法进行说明。
在本实施方式中，也可以将与易磁化轴平行的截面上的铁氧体颗粒的面积设为S，将铁氧体颗粒的周长设为L，将4πS/L2设为铁氧体颗粒的圆形度。此外，圆形度在圆的情况下成为作为最大值的1，越偏平，越接近0。然后，也可以算出各铁氧体颗粒的圆形度，并进行平均，由此，算出圆形度的平均值。
具体而言，首先，在与易磁化轴平行的截面中，拍摄SEM图像。SEM图像的大小没有特别限定，但设为至少包含100个铁氧体颗粒的大小。观察多张SEM图像，各SEM图像中所含的铁氧体颗粒的合计也可以至少为100个。SEM图像的倍率没有特别限定，只要为能够测定各铁氧体颗粒的圆形度的倍率即可。
接着，使用Deep Neural Network(DNN)分析SEM图像，制作对铁氧体颗粒和晶界进行了2值化的分析用图像。然后，通过使用Open Source Computer Vision Library(OpenCV)进行图像处理，对分析用图像中完全包含的各铁氧体颗粒算出圆形度。然后，通过对关于各铁氧体颗粒算出的圆形度进行平均，算出圆形度的平均值。
铁氧体颗粒的圆形度的平均值没有特别限定，可以将通过上述的方法算出的圆形度的平均值设为W，满足0.56≤W≤0.68，也可以满足0.58≤W≤0.67，也可以满足0.60≤W≤0.66。
铁氧体颗粒的粒径没有特别限定，但算出了上述的圆形度的铁氧体颗粒的Heywood直径的平均值可以为0.87μm以上1.60μm以下，也可以为1.00μm以上1.23μm以下。
通常，铁氧体颗粒的粒径越小，铁氧体烧结磁铁的磁特性越容易提高。但是，铁氧体颗粒的粒径小的铁氧体烧结磁铁的制造困难，因此，从降低制造成本的观点来看，铁氧体颗粒的粒径越大越优选。本实施方式的铁氧体烧结磁铁通过铁氧体颗粒的Heywood直径的平均值为上述的范围内，降低制造成本，并且更容易提高Br及HcJ。
此外，Heywood直径为投影面积圆当量直径。本实施方式中的铁氧体颗粒的Heywood直径为(4S/π)1/2。
本实施方式的铁氧体烧结磁铁的密度(df)没有特别限定。例如，通过阿基米德法测定的df也可以为5.0600g/cm3以上5.1500g/cm3以下。通过df为上述的范围内、特别是为5.0600g/cm3以上，Br容易变得良好。
以下，对本实施方式的铁氧体烧结磁铁的制造方法进行说明。
在以下的实施方式中，示出铁氧体烧结磁铁的制造方法的一例。在本实施方式中，铁氧体烧结磁铁能够经由配合工序、煅烧工序、粉碎工序、成型工序及烧成工序进行制造。以下对各工序进行说明。
＜配合工序＞
在配合工序中，配合铁氧体烧结磁铁的原料，得到原料混合物。作为铁氧体烧结磁铁的原料，可以举出包含构成其的元素中的1种或2种以上的化合物(原料化合物)。原料化合物例如优选为粉末状。
作为原料化合物，可以举出各元素的氧化物、或通过烧成成为氧化物的化合物(碳酸盐、氢氧化物、硝酸盐等)。例如能够例示CaCO3、La2O3、SrCO3、BaCO3、Fe2O3、Co3O4、MgO、B2O3、Al2O3、SiO2及MnO等。原料化合物的粉末的平均粒径也可以为0.1μm～2.0μm左右。
配合例如以得到期望的铁氧体磁性材料的组成的方式称量各原料。然后，使用湿式磨碎机、球磨机等，能够混合、粉碎0.1小时～20小时左右。此外，在该配合工序中，不需要混合全部的原料，也可以在后述的煅烧后添加一部分。
＜煅烧工序＞
在煅烧工序中，煅烧在配合工序中得到的原料混合物。煅烧例如能够在空气中等氧化性气氛中进行。煅烧的温度优选为1100℃～1300℃的温度范围。煅烧的时间能够设为1秒～10小时。
通过煅烧得到的煅烧体的一次粒径可以为10μm以下。
＜粉碎工序＞
在粉碎工序中，将在煅烧工序中成为颗粒状或块状的煅烧体粉碎，制成粉末状。由此，后述的成型工序中的成型变得容易。在粉碎工序中，如上所述，也可以添加在配合工序中没有配合的原料(原料的后添加)。粉碎工序例如也可以以在将煅烧体粉碎成粗的粉末(粗粉碎)后，将其进一步微细地粉碎(微粉碎)的2阶段的工序进行。
粗粉碎例如使用振动磨机等，进行至平均粒径成为0.5μm～10.0μm。在微粉碎中，通过湿式磨碎机、球磨机、气流磨等进一步粉碎在粗粉碎中得到的粗粉碎材料。
在微粉碎中，以得到的微粉碎粉的平均粒径优选成为0.08μm～1.00μm左右的方式进行微粉碎。微粉碎粉的比表面积(例如，通过BET法求出。)能够设为4m2/g～12m2/g左右。粉碎时间根据粉碎方法而不同，例如，在湿式磨碎机情况下，能够设为30小时～20小时左右，在利用球磨机的湿式粉碎中，能够设为1小时～50小时左右。
在微粉碎工序中，在湿式法的情况下，除了水等水系溶剂以外，还能够使用甲苯、二甲苯等非水系溶剂作为分散介质。使用非水系溶剂时在后述的湿式成型时有得到高取向性的趋势。另一方面，在使用水等水系溶剂的情况下，在生产性的观点上是有利的。
另外，在微粉碎工序中，为了提高在烧成后得到的烧结体的取向度，例如也可以添加公知的多元醇或分散剂。
＜成型·烧成工序＞
成型·烧成工序中，将粉碎工序后得到的粉碎材料(优选为微粉碎粉)成型而得到成型体后，烧成该成型体，得到烧结体。成型也能够通过干式成型、湿式成型或陶瓷注射成型(Ceramic Injection Molding(CIM))的任一方法进行。
干式成型法中，例如将干燥后的磁性粉末进行加压成型且施加磁场，形成成型体，然后，烧成成型体。一般而言，干式成型法中，将干燥后的磁性粉末在金属模具内进行加压成型，因此，具有成型工序所需要的时间较短的优点。
湿式成型法中，例如一边将包含磁性粉末的浆料在磁场施加中进行加压成型一边除去液体成分，形成成型体，然后，烧成成型体。湿式成型法中，通过成型时的磁场，磁性粉末容易取向，具有烧结磁铁的磁特性良好的优点。
另外，使用了CIM的成型法是将干燥后的磁性粉末与粘合剂树脂一起加热混炼，将形成的粒料在施加有磁场的金属模具内进行注塑成型，得到预成型体，对该预成型体进行脱粘合剂处理后进行烧成的方法。
以下，对湿式成型进行详细地说明。
(湿式成型·烧成)
在通过湿式成型法得到铁氧体烧结磁铁的情况下，通过以湿式进行上述的微粉碎工序而得到浆料。将该浆料浓缩成规定的浓度，得到湿式成型用浆料。能够使用该浆料进行成型。
浆料的浓缩能够通过离心分离或压滤机等进行。湿式成型用浆料中的微粉碎粉的含量在湿式成型用浆料的总量中能够设为30质量％～80质量％左右。
浆料中，作为分散微粉碎粉的分散介质，能够使用水。在该情况下，浆料中可以添加葡萄糖酸、葡萄糖酸盐、山梨糖醇等的表面活性剂。另外，作为分散介质，也可以使用非水系溶剂。作为非水系溶剂，能够使用甲苯或二甲苯等的有机溶剂。在该情况下，能够添加油酸等的表面活性剂。
此外，湿式成型用浆料也可以通过向微粉碎后的干燥状态的微粉碎粉中添加分散介质等而制备。
湿式成型中，接着，对于该湿式成型用浆料进行磁场中成型。在该情况下，成型压力能够设为9.8MPa～98MPa(0.1ton/cm2～1.0ton/cm2)左右。施加磁场能够设为400kA/m～1600kA/m左右。另外，成型时的加压方向与磁场施加方向可以是同一方向，也可以是正交方向。
通过湿式成型得到的成型体的烧成能够在大气中等的氧化性气氛中进行。烧成温度能够设为1050℃～1270℃。另外，烧成时间(保持在烧成温度的时间)能够设为0.5小时～3小时左右。
此外，在以湿式成型得到成型体的情况下，在到达烧成温度之前，能够从室温以2.5℃/分钟左右的升温速度加热到100℃左右。通过使成型体充分干燥，能够抑制裂纹的产生。
另外，在添加表面活性剂(分散剂)等的情况下，例如，通过在100℃～500℃左右的温度范围，以2.0℃/分钟左右的升温速度进行加热，能够将它们充分除去(脱脂处理)。此外，这些处理可以在烧成工序的最初进行，也可以在烧成工序之前另外进行。
以上，对铁氧体烧结磁铁的优选的制造方法进行了说明，但制造方法不限定于上述，制造条件等能够适当变更。
通过本发明得到的铁氧体烧结磁铁只要是具有本发明的铁氧体的组成的铁氧体烧结磁铁，形态就没有限定。例如，铁氧体烧结磁铁能够具备具有各向异性的弧段形状、平板状、圆柱状、筒状等各种形状。根据本发明的铁氧体烧结磁铁，无论磁铁的形状，都能够维持高的HcJ，且得到高的Br。
本实施方式中的铁氧体烧结磁铁能够用于通常的马达、旋转机、传感器等。
实施例
以下，通过实施例对发明进行更详细地说明，但本发明不限定于这些实施例。
＜配合工序＞
作为起始原料，准备CaCO3、La2O3、SrCO3、BaCO3、Fe2O3、Co3O4、MgO、B2O3、Al2O3、SiO2及MnO，以成为表1、表2中记载的各试样的组成的方式进行秤量。此外，表1中记载了Ca1-w- xRwAxFezCom的原子数比。表2中以质量％单位分别记载了以各元素的氧化物换算的含量。
表1中的Ba的含量和Sr的含量的合计有时与Ba+Sr的含量不一致是因为表1中记载的各个含量将小数点第4位四舍五入。
表2中记载的各成分的含量的合计不成为100质量％是因为省略了来自杂质的成分。作为来自杂质的成分，例如可以举出P2O5、SO3、Cl、K2O、V2O5、Cr2O3、NiO、CuO、ZnO、MoO3。
将上述起始原料通过湿式磨碎机进行混合、粉碎，得到浆料状的原料混合物。
＜煅烧工序＞
在将该原料混合物干燥后，在大气中，进行在1200℃下保持2小时的煅烧处理，得到煅烧体。
＜粉碎工序＞
将得到的煅烧体通过棒磨机进行粗粉碎，得到粗粉碎材料。接着，通过湿式球磨机进行28小时微粉碎，得到浆料。将得到的浆料以固体成分浓度成为70～75质量％的方式进行调整，制成湿式成型用浆料。
＜成型·烧成工序＞
接着，使用湿式磁场成型机，得到预成型体。成型压力设为50MPa，施加磁场设为800kA/m。另外，成型时的加压方向和磁场施加方向设定为同一方向。通过湿式成型得到的预成型体为圆板状，直径30mm、高度15mm。
将预成型体进行在大气中在1190℃～1230℃下保持1小时的烧成，得到作为烧结体的铁氧体烧结磁铁。
对各铁氧体烧结磁铁进行荧光X射线定量分析，能够确认各铁氧体烧结磁铁分别成为表1、表2中所示的组成。
另外，通过X射线衍射测定确认了表1、表2的各铁氧体烧结磁铁的铁氧体颗粒具有六方晶结构。
＜磁特性(Br、HcJ)的测定＞
在对实施例1～3、比较例1～3的各铁氧体烧结磁铁的上下表面进行加工后，在25℃的大气气氛中，使用最大施加磁场1989kA/m的B-H回线仪，测定磁特性。将结果示于表1。
＜密度(df)的测定＞
实施例1～3、比较例1～3的各铁氧体烧结磁铁的密度通过阿基米德法来测定。将结果示于表1。
＜铁氧体颗粒的圆形度的平均值及Heywood直径的平均值＞
首先，在与各铁氧体烧结磁铁的易磁化轴平行的截面上，拍摄SEM图像。将倍率设为5000倍，拍摄26μm×19μm的SEM图像。此外，在各SEM图像中确认了至少含有100个铁氧体颗粒。
接着，使用DNN分析SEM图像，制作对铁氧体颗粒和晶界进行了2值化的分析用图像。然后，使用OpenCV进行图像处理，对分析用图像中完全包含的铁氧体颗粒算出圆形度，并进行平均，由此，算出圆形度的平均值。将结果示于表1。
进而，通过对分析用图像中完全包含的铁氧体颗粒算出Heywood直径，并进行平均，由此，算出Heywood直径的平均值。将结果示于
表1。
根据表1、表2，Mg的含量以MgO换算为0.010质量％以上0.090质量％以下的实施例1～3中，HcJ为良好，且与Mg的含量为上述的范围外的比较例1～3相比较，Br变高。具体来说，全部实施例的Br为460mT以上。另外，全部实施例的HcJ为320kA/m，实施例2和3的HcJ为350kA/m以上。
Claims (8)
1.一种铁氧体烧结磁铁，其中，
所述铁氧体烧结磁铁包含以MgO换算为0.010质量％以上0.090质量％以下的Mg。
2.根据权利要求1所述的铁氧体烧结磁铁，其中，
所述铁氧体烧结磁铁包含Ca、R、A、Fe及Co，以原子数比计用Ca1-w-xRwAxFezCom表示组成式时，
R为选自稀土元素中的1种以上，并且至少包含La，
A为选自Ba及Sr中的1种以上，并且
满足：
0.364≤w≤0.495、
0.038≤x≤0.136、
8.280≤z≤10.45、
0.257≤m≤0.338。
3.根据权利要求1或2所述的铁氧体烧结磁铁，其中，
所述铁氧体烧结磁铁包含Ca、R、A、Fe及Co，以原子数比计用Ca1-w-xRwAxFezCom表示组成式时，
R为选自稀土元素中的1种以上，并且至少包含La，
A为选自Ba及Sr中的1种以上，并且
满足：
0.459≤w≤0.474、
0.054≤x≤0.120、
9.837≤z≤9.934、
0.293≤m≤0.311。
4.根据权利要求1所述的铁氧体烧结磁铁，其中，
所述铁氧体烧结磁铁包含Ca、R、A、Fe及Co，
R为选自稀土元素中的1种以上，并且至少包含La，
A为选自Ba及Sr中的1种以上，
所述铁氧体烧结磁铁包含以CaO换算为2.505质量％以上2.951质量％以下的Ca、以R2O3换算为8.028质量％以上8.239质量％以下的R、以AO换算为0.666质量％以上1.666质量％以下的A、以Fe2O3换算为84.564质量％以上84.937质量％以下的Fe、以CoO换算为2.341质量％以上2.521质量％以下的Co。
5.根据权利要求1、2、4中任一项所述的铁氧体烧结磁铁，其中，
所述铁氧体烧结磁铁包含以B2O3换算为0.005质量％以上0.058质量％以下的B。
6.根据权利要求1、2、4中任一项所述的铁氧体烧结磁铁，其中，
所述铁氧体烧结磁铁包含以Al2O3换算为0.049质量％以上0.065质量％以下的Al。
7.根据权利要求1、2、4中任一项所述的铁氧体烧结磁铁，其中，
所述铁氧体烧结磁铁包含以SiO2换算为0.315质量％以上0.353质量％以下的Si。
8.根据权利要求1、2、4中任一项所述的铁氧体烧结磁铁，其中，
所述铁氧体烧结磁铁包含以MnO换算为0.288质量％以上0.341质量％以下的Mn。
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| JP2011171568A (ja) * | 2010-02-19 | 2011-09-01 | Hitachi Metals Ltd | 酸化物磁性材料、フェライト焼結磁石及びフェライト焼結磁石の製造方法 |
| US20120161910A1 (en) * | 2009-07-08 | 2012-06-28 | Tdk Corporation | Ferrite magnetic material |
| CN102666431A (zh) * | 2010-03-17 | 2012-09-12 | Tdk株式会社 | 铁素体磁性材料、铁素体磁铁、铁素体烧结磁铁 |
| CN110323027A (zh) * | 2018-03-28 | 2019-10-11 | Tdk株式会社 | 铁氧体烧结磁铁及铁氧体烧结磁铁的制造方法 |
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| JP4316547B2 (ja) | 2005-09-12 | 2009-08-19 | 株式会社クボタ | エンジン |
| JP4254897B2 (ja) * | 2005-12-28 | 2009-04-15 | 日立金属株式会社 | 酸化物磁性材料 |
| JP6596829B2 (ja) | 2014-03-07 | 2019-10-30 | Ｔｄｋ株式会社 | フェライト焼結磁石及びそれを備えるモータ |
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| US20120161910A1 (en) * | 2009-07-08 | 2012-06-28 | Tdk Corporation | Ferrite magnetic material |
| JP2011171568A (ja) * | 2010-02-19 | 2011-09-01 | Hitachi Metals Ltd | 酸化物磁性材料、フェライト焼結磁石及びフェライト焼結磁石の製造方法 |
| CN102666431A (zh) * | 2010-03-17 | 2012-09-12 | Tdk株式会社 | 铁素体磁性材料、铁素体磁铁、铁素体烧结磁铁 |
| CN110323027A (zh) * | 2018-03-28 | 2019-10-11 | Tdk株式会社 | 铁氧体烧结磁铁及铁氧体烧结磁铁的制造方法 |
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| JP7367582B2 (ja) | 2023-10-24 |
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