JP2022052787A - フェライト仮焼体、フェライト焼結磁石及びその製造方法 - Google Patents
フェライト仮焼体、フェライト焼結磁石及びその製造方法 Download PDFInfo
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- JP2022052787A JP2022052787A JP2020159217A JP2020159217A JP2022052787A JP 2022052787 A JP2022052787 A JP 2022052787A JP 2020159217 A JP2020159217 A JP 2020159217A JP 2020159217 A JP2020159217 A JP 2020159217A JP 2022052787 A JP2022052787 A JP 2022052787A
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- calcined body
- ferrite
- sintered magnet
- ferrite sintered
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 86
- 238000004519 manufacturing process Methods 0.000 title claims description 20
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 13
- 229910052742 iron Inorganic materials 0.000 claims abstract description 11
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims description 53
- 238000001354 calcination Methods 0.000 claims description 34
- 238000010304 firing Methods 0.000 claims description 28
- 239000002994 raw material Substances 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 23
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 20
- 238000000465 moulding Methods 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 36
- 239000011575 calcium Substances 0.000 description 25
- 239000012071 phase Substances 0.000 description 21
- 239000000654 additive Substances 0.000 description 17
- 239000000203 mixture Substances 0.000 description 16
- 150000001875 compounds Chemical class 0.000 description 13
- 238000010298 pulverizing process Methods 0.000 description 10
- 239000002002 slurry Substances 0.000 description 10
- 230000000996 additive effect Effects 0.000 description 9
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 6
- 239000002612 dispersion medium Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 150000001805 chlorine compounds Chemical class 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000005347 demagnetization Effects 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 150000004679 hydroxides Chemical class 0.000 description 3
- 230000001965 increasing effect Effects 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- -1 CoOOH and Co (OH) 2 Chemical class 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910018916 CoOOH Inorganic materials 0.000 description 1
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
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- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229960004494 calcium gluconate Drugs 0.000 description 1
- 235000013927 calcium gluconate Nutrition 0.000 description 1
- 239000004227 calcium gluconate Substances 0.000 description 1
- NEEHYRZPVYRGPP-UHFFFAOYSA-L calcium;2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(O)C([O-])=O.OCC(O)C(O)C(O)C(O)C([O-])=O NEEHYRZPVYRGPP-UHFFFAOYSA-L 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
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- 238000004140 cleaning Methods 0.000 description 1
- 230000002301 combined effect Effects 0.000 description 1
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- 230000003247 decreasing effect Effects 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- HZZOEADXZLYIHG-UHFFFAOYSA-N magnesiomagnesium Chemical compound [Mg][Mg] HZZOEADXZLYIHG-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910001172 neodymium magnet Inorganic materials 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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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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Abstract
Description
特許文献1におけるCaLaCo磁石は、原子比で0.3程度のCoを含有し、高いBrとHcJを有するもののHk/HcJに関するデータは一切開示されていない。
Ca、R、Sr、Fe及びCoの金属元素(ただし、Rは希土類元素の少なくとも一種であってLaを必須に含む元素)の原子比を示す一般式:Ca1-x-yRxAyFe2n-zCozにおいて、
前記x、y及びz、並びにn(ただし、2nはモル比であって、2n=(Fe+Co)/(Ca+R+Sr)で表される)が、
0.4≦x<0.5、
0<y≦0.2、
0.18<z<0.3、
1.6≦x/z≦2.25、及び
8.5≦2n-z≦10、
を満足する。
ある実施形態において、1.6≦x/z≦2.0である。
Ca、R、Sr、Fe及びCoの金属元素(ただし、Rは希土類元素の少なくとも一種であってLaを必須に含む元素)の原子比を示す一般式:Ca1-x-yRxAyFe2n-zCozにおいて、
前記x、y及びz、並びにn(ただし、2nはモル比であって、2n=(Fe+Co)/(Ca+R+Sr)で表される)が、
0.35≦x<0.5、
0<y≦0.2、
0.18<z<0.3、
1.6≦x/z≦2.25、及び
7.5≦2n-z≦10、
を満足する。
ある実施形態において、1.6≦x/z≦2.0である。
Ca、R、Sr、Fe及びCoの金属元素(ただし、Rは希土類元素の少なくとも一種であってLaを必須に含む元素)の原子比を示す一般式:Ca1-x-yRxAyFe2n-zCozにおいて、
前記x、y及びz、並びにn(ただし、2nはモル比であって、2n=(Fe+Co)/(Ca+R+Sr)で表される)が、
0.4≦x<0.5、
0<y≦0.2、
0.18<z<0.3、
1.6≦x/z≦2.25、及び
8.5≦2n-z≦10、
を満足する原料粉末を混合し、混合原料粉末を得る原料粉末混合工程、
前記混合原料粉末を仮焼し、仮焼体を得る仮焼工程、
前記仮焼体を粉砕し、仮焼体の粉末を得る粉砕工程、
前記仮焼体の粉末を成形し、成形体を得る成形工程、
前記成形体を焼成し、焼結体を得る焼成工程、
を含み、
前記焼成工程において、室温から1100℃までの温度範囲における平均昇温速度を600℃/時以上1000℃/時以下、1100℃から焼成温度までの温度範囲における平均昇温速度を1℃/分以上10℃/分以下とし、焼成温度から800℃までの温度範囲における平均降温速度を1000℃/時以上とする。
ある実施形態において、1.6≦x/z≦2.0である。
本開示の実施形態のフェライト仮焼体は、
Ca、R、Sr、Fe及びCoの金属元素(ただし、Rは希土類元素の少なくとも一種であってLaを必須に含む元素)の原子比を示す一般式:Ca1-x-yRxAyFe2n-zCozにおいて、
前記x、y及びz、並びにn(ただし、2nはモル比であって、2n=(Fe+Co)/(Ca+R+Sr)で表される)が、
0.4≦x<0.5、
0<y≦0.2、
0.18<z<0.3、
1.6≦x/z≦2.25、及び
8.5≦2n-z≦10、
を満足する。
原料粉末としては、価数にかかわらず、それぞれの金属の酸化物、炭酸塩、水酸化物、硝酸塩、塩化物等の化合物を使用することができる。原料粉末を溶解した溶液であってもよい。Caの化合物としては、Caの炭酸塩、酸化物、塩化物等が挙げられる。Rの化合物としては、Laを例にすると、La2O3等の酸化物、La(OH)3等の水酸化物、La2(CO3)3・8H2O等の炭酸塩等が挙げられる。Srの化合物としては、Srの炭酸塩、酸化物、塩化物等が挙げられる。Feの化合物としては、酸化鉄、水酸化鉄、塩化鉄、ミルスケール等が挙げられる。Coの化合物としては、CoO、Co3O4等の酸化物、CoOOH、Co(OH)2等の水酸化物、CoCO3等の炭酸塩、及びm2CoCO3・m3Co(OH)2・m4H2O等の塩基性炭酸塩(m2、m3、m4は正の数である)が挙げられる。
式:(CaCO3の分子量×CaO換算での添加量)/CaOの分子量
によって求めることができる。例えば、CaO換算で0.5mass%のCaCO3を添加する場合、
{(40.08[Caの原子量]+12.01[Cの原子量]+48.00[Oの原子量×3]=100.09[CaCO3の分子量])×0.5mass%[CaO換算での添加量]}/(40.08[Caの原子量]+16.00[Oの原子量]=56.08[CaOの分子量])=0.892mass%[CaCO3の添加量]、となる。
前記の通り、本開示の実施形態のフェライト仮焼体は、SiO2やCaCO3などの添加物を添加しなくても、液相が生成し、焼結することができ、本開示の実施形態のフェライト焼結磁石を得ることができる。この時、フェライト仮焼体の成分、組成と、フェライト焼結磁石の成分、組成は、基本的に同じとなる(製造工程における不純物の混入などは考慮しない)。
Ca、R、Sr、Fe及びCoの金属元素(ただし、Rは希土類元素の少なくとも一種であってLaを必須に含む元素)の原子比を示す一般式:Ca1-x-yRxAyFe2n-zCozにおいて、
前記x、y及びz、並びにn(ただし、2nはモル比であって、2n=(Fe+Co)/(Ca+R+Sr)で表される)が、
0.35≦x<0.5、
0<y≦0.2、
0.18<z<0.3、
1.6≦x/z≦2.25、及び
7.5≦2n-z≦10、
を満足するものとなる。
本開示の実施形態に基づく実験例として、一般式Ca1-x-yLaxSryFe2n-zCozにおいて、原子比が表1の試料No.1~15に示す1-x-y、x、y、z及び2n-zになるようにCaCO3粉末、La(OH)3粉末、SrCO3粉末、Fe2O3粉末及びCo3O4粉末を所定の組成で秤量し、秤量後の粉末の合計100mass%に対してH3BO3粉末を0.1mass%添加後、それぞれ湿式ボールミルで4時間混合した後、乾燥、整粒して6種類の混合原料粉末を得た。得られた混合原料粉末をそれぞれ大気中において1200℃で3時間仮焼し、6種類の仮焼体を得た。
Claims (14)
- Ca、R、Sr、Fe及びCoの金属元素(ただし、Rは希土類元素の少なくとも一種であってLaを必須に含む元素)の原子比を示す一般式:Ca1-x-yRxAyFe2n-zCozにおいて、
前記x、y及びz、並びにn(ただし、2nはモル比であって、2n=(Fe+Co)/(Ca+R+Sr)で表される)が、
0.4≦x<0.5、
0<y≦0.2、
0.18<z<0.3、
1.6≦x/z≦2.25、及び
8.5≦2n-z≦10、
を満足するフェライト仮焼体。 - 9<2n-z≦10である請求項1に記載のフェライト仮焼体。
- 1.6≦x/z≦2.0である請求項1又は2に記載のフェライト仮焼体。
- Ca、R、Sr、Fe及びCoの金属元素(ただし、Rは希土類元素の少なくとも一種であってLaを必須に含む元素)の原子比を示す一般式:Ca1-x-yRxAyFe2n-zCozにおいて、
前記x、y及びz、並びにn(ただし、2nはモル比であって、2n=(Fe+Co)/(Ca+R+Sr)で表される)が、
0.35≦x<0.5、
0<y≦0.2、
0.18<z<0.3、
1.6≦x/z≦2.25、及び
7.5≦2n-z≦10、
を満足するフェライト焼結磁石。 - 8<2n-z≦10である請求項4に記載のフェライト焼結磁石。
- 1.6≦x/z≦2.0である請求項4又は5に記載のフェライト焼結磁石。
- Cr2O3換算で1.5mass%以下(0mass%は含まず)のCrをさらに含有する請求項4~6のいずれかに記載のフェライト焼結磁石。
- SiO2換算で1.0mass%以下(0mass%は含まず)のSiをさらに含有する請求項4~7のいずれかに記載のフェライト焼結磁石。
- Ca、R、Sr、Fe及びCoの金属元素(ただし、Rは希土類元素の少なくとも一種であってLaを必須に含む元素)の原子比を示す一般式:Ca1-x-yRxAyFe2n-zCozにおいて、
前記x、y及びz、並びにn(ただし、2nはモル比であって、2n=(Fe+Co)/(Ca+R+Sr)で表される)が、
0.4≦x<0.5、
0<y≦0.2、
0.18<z<0.3、
1.6≦x/z≦2.25、及び
8.5≦2n-z≦10、
を満足する原料粉末を混合し、混合原料粉末を得る原料粉末混合工程、
前記混合原料粉末を仮焼し、仮焼体を得る仮焼工程、
前記仮焼体を粉砕し、仮焼体の粉末を得る粉砕工程、
前記仮焼体の粉末を成形し、成形体を得る成形工程、
前記成形体を焼成し、焼結体を得る焼成工程、
を含み、
前記焼成工程において、室温から1100℃までの温度範囲における平均昇温速度を600℃/時以上1000℃/時以下、1100℃から焼成温度までの温度範囲における平均昇温速度を1℃/分以上10℃/分以下とし、焼成温度から800℃までの温度範囲における平均降温速度を1000℃/時以上とするフェライト焼結磁石の製造方法。 - 9<2n-z≦10である請求項9に記載のフェライト焼結磁石の製造方法。
- 1.6≦x/z≦2.0である請求項9又は10に記載のフェライト焼結磁石の製造方法。
- 前記仮焼工程後、前記成形工程前に、前記仮焼体又は仮焼体の粉末100mass%に対して1.5mass%以下(0mass%は含まず)のCr2O3を添加する工程をさらに含む請求項9~11のいずれかに記載のフェライト焼結磁石の製造方法。
- 前記仮焼工程後、前記成形工程前に、前記仮焼体又は仮焼体の粉末100mass%に対して1.0mass%以下(0mass%は含まず)のSiO2を添加する工程をさらに含む請求項9~12のいずれかに記載のフェライト焼結磁石の製造方法。
- 前記仮焼工程後、前記成形工程前に、前記仮焼体又は仮焼体の粉末100mass%に対してCaO換算で1.0mass%以下(0mass%は含まず)のCaCO3を添加する工程をさらに含む請求項9~13のいずれかに記載のフェライト焼結磁石の製造方法。
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