JP2020126931A - フェライト焼結磁石 - Google Patents
フェライト焼結磁石 Download PDFInfo
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- JP2020126931A JP2020126931A JP2019018621A JP2019018621A JP2020126931A JP 2020126931 A JP2020126931 A JP 2020126931A JP 2019018621 A JP2019018621 A JP 2019018621A JP 2019018621 A JP2019018621 A JP 2019018621A JP 2020126931 A JP2020126931 A JP 2020126931A
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- Prior art keywords
- core
- content
- sintered magnet
- ferrite
- shell
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 166
- 239000011258 core-shell material Substances 0.000 claims abstract description 59
- 239000002245 particle Substances 0.000 claims description 109
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 229910014230 BO 3 Inorganic materials 0.000 claims description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 5
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
- 230000004907 flux Effects 0.000 abstract description 9
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 239000011575 calcium Substances 0.000 description 60
- 239000002994 raw material Substances 0.000 description 47
- 238000010304 firing Methods 0.000 description 38
- 239000000203 mixture Substances 0.000 description 24
- 238000000465 moulding Methods 0.000 description 23
- 238000004458 analytical method Methods 0.000 description 20
- 238000010298 pulverizing process Methods 0.000 description 18
- 239000000463 material Substances 0.000 description 17
- 238000001354 calcination Methods 0.000 description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 15
- 238000000034 method Methods 0.000 description 14
- 239000002002 slurry Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- 229910004298 SiO 2 Inorganic materials 0.000 description 12
- 239000013078 crystal Substances 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 238000012935 Averaging Methods 0.000 description 8
- 238000009826 distribution Methods 0.000 description 8
- 229910052746 lanthanum Inorganic materials 0.000 description 8
- 229910052712 strontium Inorganic materials 0.000 description 8
- 229910052791 calcium Inorganic materials 0.000 description 7
- 150000005846 sugar alcohols Polymers 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 4
- 150000001340 alkali metals Chemical class 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 239000002612 dispersion medium Substances 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000003125 aqueous solvent Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 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 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
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000011802 pulverized particle Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000600 sorbitol Substances 0.000 description 2
- 238000004846 x-ray emission Methods 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
- 229910052684 Cerium Inorganic materials 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
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000007771 core particle Substances 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 229940050410 gluconate Drugs 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- CMGJQFHWVMDJKK-UHFFFAOYSA-N lanthanum;trihydrate Chemical compound O.O.O.[La] CMGJQFHWVMDJKK-UHFFFAOYSA-N 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 239000003921 oil Substances 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
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000000700 radioactive tracer Substances 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- 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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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
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- C04B35/2633—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium
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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
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- 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
- H01F1/11—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 in the form of particles
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- C04B2235/3215—Barium oxides or oxide-forming salts thereof
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- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3275—Cobalt oxides, cobaltates or cobaltites or oxide forming salts thereof, e.g. bismuth cobaltate, zinc cobaltite
- C04B2235/3277—Co3O4
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3409—Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
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Abstract
Description
Ca1−w−x−yRwSrxBayFezCom (1)、
0.25<w<0.5 (2)、
0.01<x<0.35 (3)、
0≦y<0.013 (4)、
y<x (5)、
8.5<z<9.9 (6)、
1.0<w/m<2.1 (7)、
0.017<m/z<0.055 (8)、
0<1−w−x−y<1 (9)。
0.350<w<0.420 (2a)
0.120<x<0.180 (3a)
0.200<m<0.280 (10)
図1中の(a)は、本実施形態に係る直方体状のフェライト焼結磁石2(フェライト永久磁石)の模式的な斜視図であり、図1中の(b)は、フェライト焼結磁石2の断面2csの模式図であり、図2は、フェライト焼結磁石2の断面2csの一部(領域II)の拡大図である。フェライト焼結磁石2の形状は、直方体に限定されない。例えば、フェライト焼結磁石2の形状は、アークセグメント形、C字形、瓦形、平板、円柱及び弓形からなる群より選ばれる一種であってよい。
Ca1−w−x−yRwSrxBayFezCom (1)
0.25<w<0.5 (2)
0.01<x<0.35 (3)
0≦y<0.013 (4)
y<x (5)
8.5<z<9.9 (6)
1.0<w/m<2.1 (7)
0.017<m/z<0.055 (8)
0<1−w−x−y<1 (9)
Ca1−w−x−yRwSrxBayFezComO19 (1a)
0.350<w<0.420、好ましくは0.360≦w≦0.420 (2a)
0.120<x<0.180、好ましくは0.110≦x≦0.173 (3a)
8.51≦z≦9.71 (4a)
0.200<m<0.280、好ましくは0.208≦m≦0.269 (10)
本実施形態に係るフェライト焼結磁石の製造方法は、配合工程、仮焼工程、粉砕工程、成形工程及び焼成工程を備えてよい。各工程については以下に説明する。
配合工程では、フェライト焼結磁石の原料を配合して、原料組成物を得る。まず、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種又は2種以上を含む化合物(原料化合物)が挙げられる。原料は、粉末であったほうがよい。原料化合物としては、各元素の酸化物、又は焼成により酸化物となる化合物(炭酸塩、水酸化物、硝酸塩等)が挙げられる。主相の原料(原料化合物)は、例えば、SrCO3、La(OH)3、Fe2O3、BaCO3、CaCO3、Co3O4、H3BO3、Al2O3、及びSiO2等であってよい。主相の原料には、必要に応じてその他の副成分(元素単体、酸化物等)を配合してもよい。原料化合物の粉末の平均粒径は、例えば、均質な配合を可能とする観点から、0.1〜2.0μm程度であってよい。
仮焼工程では、配合工程で得られた原料粉末を仮焼する。仮焼工程により、顆粒状又は塊状の仮焼体が得られる。仮焼は、例えば、空気等の酸化性雰囲気中で行うことが好ましい。仮焼の温度は、1100〜1400℃、1100〜1300℃、又は1100〜1250℃であってよい。仮焼の時間は、1秒間〜10時間、又は1秒間〜3時間であってよい。仮焼により得られる仮焼体は、上述したような主相(M相)を70%以上含む。主相の一次粒子径は、10μm以下、又は2μm以下であってよい。
粉砕工程では、仮焼体を粉砕し、再び粉末状にする。これにより、成形工程での成形が容易となる。粉砕工程では、組成の調整・制御のために、主相の原料又は副成分を仮焼体へ添加してもよい(原料の後添加)。粉砕工程は、例えば、仮焼体を粉砕して粗い粉末を得た後、粗い粉末を更に微細に粉砕してよい。つまり、粗粉砕と微粉砕の2段階の粉砕工程で行ってもよい。
成形工程では、粉砕工程で得られた粉砕材(好ましくは微粉砕材)を、磁場中で成形して、成形体を得る。成形は、乾式成形及び湿式成形のいずれの方法でも行うことができる。磁気的配向度を高くする観点からは、湿式成形が好ましい。
焼成工程では、成形工程で得られた成形体を焼成して、焼結体(フェライト焼結磁石)を得る。焼成工程では、成形体に含まれる主相粒子(粉砕材)が互いに焼結することにより、フェライト焼結磁石が形成される。
(フェライト焼結磁石の製造)
フェライト焼結磁石の主相の原料として、酸化鉄(Fe2O3)、炭酸カルシウム(CaCO3)、炭酸ストロンチウム(SrCO3)、酸化コバルト(Co3O4)、炭酸バリウム(BaCO3)及び水酸化ランタン(La(OH)3)を準備した。フェライト焼結磁石(主相)に含まれる金属成分の組成が下記式(1c)で表される組成になるように、上記の各原料を秤量した。つまり、下記式(1c)中の1−w−x−y、w、x、y、z及びm其々の値が、下記表1に示される値になるように、上記の各原料を秤量した。Si成分(副成分)として酸化ケイ素(SiO2)を準備した。主相の全原料の質量の合計100質量部に対するSiO2の割合(単位:質量部)は、下記表1に示される値に調整した。上記の原料を湿式アトライタで混合・粉砕した後、原料を乾燥して、原料粉末を得た。
Ca1−w−x−yLawSrxBayFezCom (1c)
仮焼工程では、1200℃の大気中で原料粉末を2時間加熱して、仮焼体を得た。粉砕工程では、仮焼体を小型ロッド振動ミルで粉砕して、粗粉砕材を得た。粗粉砕材に含まれる金属成分の組成を、より正確に上記式(1c)で表される組成に調整するために、CaCO3、La(OH)3、Co3O4、SiO2及びFe2O3を粗粉砕材へ添加した。つまり、粉砕工程において主相の原料の後添加を実施した。続いて粗粉砕材を、湿式ボールミルで更に32時間粉砕して、仮焼体からなる微粉砕粒子を含むスラリーを得た。スラリーを遠心分離機で脱水して、固形分(仮焼体からなる微粉砕粒子)の濃度を調整することにより、湿式成形用スラリーを得た。
成形工程では、湿式磁場成形機を使用して、10kOeの印加磁場中で湿式成形用スラリーを成形して、円柱状の成形体を得た。得られた成形体を、大気中において室温で十分に乾燥した。焼成工程では、大気で満たされた炉内に成形体を設置した。そして炉の内部を加熱して、炉内の温度を室温から下記表2に示される焼成温度まで上げた。炉内の温度が室温から焼成温度に達するまでの昇温速度は、下記表2に示される値に調整した。続いて、下記表2に示される焼成温度で成形体を1時間加熱した。続いて、炉の内部を冷却して、炉内の温度を焼成温度から室温まで下げた。炉内の温度が焼成温度から室温に至るまでの降温速度は、下記表2に示される値に調整した。
円柱状のフェライト焼結磁石の上面及び下面を加工した後、フェライト焼結磁石の残留磁束密度Br(mT)及び保磁力HcJ(kA/m)を測定した。測定には、最大印加磁場が25kOeであるB‐Hトレーサを用いた。実施例1のBr及びHcJは下記表2に示される。
XRF法により、フェライト焼結磁石全体の組成を分析した。実施例1のフェライト焼結磁石に含まれる金属成分の組成は、上記式(1c)で表され、1−w−x−y、w、x、y、z及びm其々の値が、下記表1に示される値であることが確認された。つまり、フェライト焼結磁石全体の組成は、下記式(1d)で表されることが確認された。
Ca1−w−x−yLawSrxBayFezComO19 (1d)
円柱状のフェライト焼結磁石の上面及び下面に対して垂直な方向においてフェライト焼結磁石を切断した。フェライト焼結磁石の断面を走査型電子顕微鏡及び透過型電子顕微鏡で観察した。走査型電子顕微鏡で撮影された実施例1のフェライト焼結磁石の断面の画像は、図3中の(a)に示される。透過型電子顕微鏡で撮影された実施例1のフェライト焼結磁石の断面の画像は、図4に示される。図3中の(a)に示されるように、フェライト焼結磁石は、互いに焼結した多数の主相粒子を含むことも確認された。多数の主相粒子の中には、コア7とコア7を覆うシェル9とを有するコアシェル構造粒子5Aが含まれることも確認された。フェライト焼結磁石は、コアシェル構造を有していない主相粒子も含むことも確認された。実施例1のフェライト焼結磁石の断面にある60個の主相粒子を無作為に選んで、60個の主相粒子のうちのコアシェル構造粒子の個数を数えた。主相粒子の総数のうちコアシェル構造粒子の個数の割合R‐CSを算出した。実施例1のR‐CSは、下記表2に示される。
特徴1: コアが、La、Sr、Co及びCaを含有していた。
特徴2: シェルが、La、Sr、Co及びCaを含有していた。
特徴3: コアにおけるSrの含有量(単位:原子%)が、シェルにおけるSrの含有量(単位:原子%)よりも高い傾向があった。
特徴4: シェルにおけるCaの含有量(単位:原子%)が、コアにおけるCaの含有量(単位:原子%)よりも高い傾向もあった。
特徴5: コアにおけるSrの含有量(単位:原子%)が、コアにおけるCaの含有量(単位:原子%)よりも高い傾向があった。
特徴6: シェルにおけるCaの含有量(単位:原子%)が、シェルにおけるSrの含有量(単位:原子%)よりも高い傾向があった。
実施例2の場合、上記式(1c)中の1−w−x−y、w、x、y、z及びm其々の値が、下記表1に示される値になるように、主相の各原料を秤量した。実施例2の場合、主相の各原料の質量の合計100質量部に対するSiO2の割合(単位:質量部)を、下記表1に示される値に調整した。実施例2の場合、主相の各原料の全量とH3BO3とAl2O3とを仮焼工程前に一括して混合した。つまり実施例2では、主相の原料の仮焼体への添加(後添加)が実施されなかった。実施例2の場合、焼成工程における昇温速度、焼成温度、及び降温速度は、下記表2に示される値に調整した。
実施例3の場合、上記式(1c)中の1−w−x−y、w、x、y、z及びm其々の値が、下記表1に示される値になるように、主相の各原料を秤量した。実施例3の場合、主相の各原料の質量の合計100質量部に対するSiO2の割合(単位:質量部)を、下記表1に示される値に調整した。実施例3の場合、主相の各原料の全量とH3BO3とAl2O3とを仮焼工程前に一括して混合した。つまり実施例3では、主相の原料の仮焼体への添加(後添加)が実施されなかった。実施例3の場合、焼成工程における昇温速度、焼成温度、及び降温速度は、下記表2に示される値に調整した。
比較例1の場合、上記式(1c)中の1−w−x−y、w、x、y、z及びm其々の値が、下記表1に示される値になるように、主相の各原料を秤量した。比較例1の場合、主相の各原料の質量の合計100質量部に対するSiO2の割合(単位:質量部)を、下記表1に示される値に調整した。比較例1の場合、焼成工程における昇温速度、焼成温度、及び降温速度は、下記表2に示される値に調整した。
Claims (9)
- 六方晶構造を有するフェライトを含む複数の主相粒子を備えるフェライト焼結磁石であって、
少なくとも一部の前記主相粒子が、コアと前記コアを覆うシェルとを有するコアシェル構造粒子であり、
前記コアにおけるLaの含有量の最小値が、[La]c原子%と表され、
前記コアにおけるCoの含有量の最小値が、[Co]c原子%と表され、
前記シェルにおけるLaの含有量の最大値が、[La]s原子%と表され、
前記シェルにおけるCoの含有量の最大値が、[Co]s原子%と表され、
[La]c+[Co]cが、3.08原子%以上4.44原子%以下であり、
[La]s+[Co]sが、7.60原子%以上9.89原子%以下である、
フェライト焼結磁石。 - ([La]s+[Co]s)/([La]c+[Co]c)が、1.75以上2.69以下である、
請求項1に記載のフェライト焼結磁石。 - 前記コアにおけるSrの含有量の最大値が、[Sr]c原子%と表され、
前記シェルにおけるSrの含有量の最小値が、[Sr]s原子%と表され、
[Sr]cが[Sr]sよりも高い、
請求項1又は2に記載のフェライト焼結磁石。 - 前記コアにおけるCaの含有量の最小値が、[Ca]c原子%と表され、
前記シェルにおけるCaの含有量の最大値が、[Ca]s原子%と表され、
[Ca]sが[Ca]cよりも高い、
請求項1〜3のいずれか一項に記載のフェライト焼結磁石。 - 前記コアにおけるSrの含有量の最大値が、[Sr]c原子%と表され、
前記コアにおけるCaの含有量の最小値が、[Ca]c原子%と表され、
[Sr]cが[Ca]cよりも高い、
請求項1〜4のいずれか一項に記載のフェライト焼結磁石。 - 前記シェルにおけるSrの含有量の最小値が、[Sr]s原子%と表され、
前記シェルにおけるCaの含有量の最大値が、[Ca]s原子%と表され、
[Ca]sが[Sr]sよりも高い、
請求項1〜5のいずれか一項に記載のフェライト焼結磁石。 - 前記フェライト焼結磁石に含まれる金属成分の少なくとも一部が、下記式(1)で表され、
Ca1−w−x−yRwSrxBayFezCom (1)、
前記式(1)中のRは、希土類元素及びBiからなる群より選ばれる少なくとも1種の元素であり、Rは少なくともLaを含み、
前記式(1)中のw、x、y、z及びmは、下記式(2)、(3)、(4)、(5)、(6)、(7)、(8)及び(9)を満たし、
0.25<w<0.5 (2)、
0.01<x<0.35 (3)、
0≦y<0.013 (4)、
y<x (5)、
8.5<z<9.9 (6)、
1.0<w/m<2.1 (7)、
0.017<m/z<0.055 (8)、
0<1−w−x−y<1 (9)、
前記フェライト焼結磁石は、Si成分を含む、
請求項1〜6のいずれか一項に記載のフェライト焼結磁石。 - 前記式(1)中のw、x及びmは、下記式(2a)、(3a)及び(10)を満たし、
0.350<w<0.420 (2a)
0.120<x<0.180 (3a)
0.200<m<0.280 (10)
前記フェライト焼結磁石におけるBの含有量が、H3BO3換算で0.037〜0.181質量%である、
請求項7に記載のフェライト焼結磁石。 - 前記フェライト焼結磁石におけるAlの含有量が、Al2O3換算で0.05〜0.3質量%である、
請求項1〜8のいずれか一項に記載のフェライト焼結磁石。
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CN114133233A (zh) * | 2022-01-30 | 2022-03-04 | 天通控股股份有限公司 | 一种高频高Bs复合铁氧体材料及其制备方法 |
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