CN107056270A - A kind of hexagonal sintered permanent ferrite magnet and preparation method thereof - Google Patents
A kind of hexagonal sintered permanent ferrite magnet and preparation method thereof Download PDFInfo
- Publication number
- CN107056270A CN107056270A CN201710399787.7A CN201710399787A CN107056270A CN 107056270 A CN107056270 A CN 107056270A CN 201710399787 A CN201710399787 A CN 201710399787A CN 107056270 A CN107056270 A CN 107056270A
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- Prior art keywords
- powder
- preparation
- sintered permanent
- alkali metal
- ferrite magnet
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 28
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 27
- 239000011575 calcium Substances 0.000 claims abstract description 27
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 25
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 23
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 239000011734 sodium Substances 0.000 claims abstract description 22
- 150000001342 alkaline earth metals Chemical class 0.000 claims abstract description 21
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 21
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 20
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 20
- 229910052788 barium Inorganic materials 0.000 claims abstract description 19
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 19
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 239000011591 potassium Substances 0.000 claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 11
- 238000007493 shaping process Methods 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 107
- 239000002245 particle Substances 0.000 claims description 61
- 239000000463 material Substances 0.000 claims description 38
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 31
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- 239000000654 additive Substances 0.000 claims description 22
- 230000000996 additive effect Effects 0.000 claims description 22
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 14
- 239000000377 silicon dioxide Substances 0.000 claims description 14
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 12
- 239000002270 dispersing agent Substances 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 12
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims description 11
- 229910001617 alkaline earth metal chloride Inorganic materials 0.000 claims description 10
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 10
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 10
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 10
- 229910052681 coesite Inorganic materials 0.000 claims description 9
- 229910052906 cristobalite Inorganic materials 0.000 claims description 9
- 229910052682 stishovite Inorganic materials 0.000 claims description 9
- 229910052905 tridymite Inorganic materials 0.000 claims description 9
- 229910001514 alkali metal chloride Inorganic materials 0.000 claims description 8
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 8
- 238000002791 soaking Methods 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 6
- 239000011668 ascorbic acid Substances 0.000 claims description 6
- 229960005070 ascorbic acid Drugs 0.000 claims description 6
- 235000010323 ascorbic acid Nutrition 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- 238000005660 chlorination reaction Methods 0.000 claims description 5
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 5
- 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 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- LBFUKZWYPLNNJC-UHFFFAOYSA-N cobalt(ii,iii) oxide Chemical compound [Co]=O.O=[Co]O[Co]=O LBFUKZWYPLNNJC-UHFFFAOYSA-N 0.000 claims description 2
- 238000010348 incorporation Methods 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- WJEIYVAPNMUNIU-UHFFFAOYSA-N [Na].OC(O)=O Chemical compound [Na].OC(O)=O WJEIYVAPNMUNIU-UHFFFAOYSA-N 0.000 claims 1
- 230000005415 magnetization Effects 0.000 abstract description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 18
- 238000004519 manufacturing process Methods 0.000 description 17
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical group [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 14
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 14
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- 229910001429 cobalt ion Inorganic materials 0.000 description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 description 9
- 229910017052 cobalt Inorganic materials 0.000 description 8
- 239000010941 cobalt Substances 0.000 description 8
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical group [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 8
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 8
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 7
- 239000001110 calcium chloride Substances 0.000 description 7
- 229910001628 calcium chloride Inorganic materials 0.000 description 7
- KAGOZRSGIYZEKW-UHFFFAOYSA-N cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Co+3].[Co+3] KAGOZRSGIYZEKW-UHFFFAOYSA-N 0.000 description 7
- 239000001103 potassium chloride Substances 0.000 description 7
- 235000011164 potassium chloride Nutrition 0.000 description 7
- 238000011160 research Methods 0.000 description 7
- QIMZHEUFJYROIY-UHFFFAOYSA-N [Co].[La] Chemical compound [Co].[La] QIMZHEUFJYROIY-UHFFFAOYSA-N 0.000 description 6
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 6
- 229910001626 barium chloride Inorganic materials 0.000 description 6
- 230000004907 flux Effects 0.000 description 6
- 238000003672 processing method Methods 0.000 description 6
- 239000011780 sodium chloride Substances 0.000 description 6
- 229910001631 strontium chloride Inorganic materials 0.000 description 6
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- CZMAIROVPAYCMU-UHFFFAOYSA-N lanthanum(3+) Chemical compound [La+3] CZMAIROVPAYCMU-UHFFFAOYSA-N 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000006467 substitution reaction Methods 0.000 description 5
- -1 cation metal oxide Chemical class 0.000 description 4
- ROYOLNQPXVHWNE-UHFFFAOYSA-N [Co].[Ca].[La] Chemical compound [Co].[Ca].[La] ROYOLNQPXVHWNE-UHFFFAOYSA-N 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000005389 magnetism Effects 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- QBYHSJRFOXINMH-UHFFFAOYSA-N [Co].[Sr].[La] Chemical compound [Co].[Sr].[La] QBYHSJRFOXINMH-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910002771 BaFe12O19 Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- RGHNJXZEOKUKBD-SQOUGZDYSA-N Gluconic acid Natural products OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 1
- LKDRXBCSQODPBY-AMVSKUEXSA-N L-(-)-Sorbose Chemical compound OCC1(O)OC[C@H](O)[C@@H](O)[C@@H]1O LKDRXBCSQODPBY-AMVSKUEXSA-N 0.000 description 1
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 description 1
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 1
- MMAFLWPTWXNMQO-UHFFFAOYSA-N [Ca]O[Fe] Chemical compound [Ca]O[Fe] MMAFLWPTWXNMQO-UHFFFAOYSA-N 0.000 description 1
- 150000001339 alkali metal compounds Chemical class 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 229910001422 barium ion Inorganic materials 0.000 description 1
- WETINTNJFLGREW-UHFFFAOYSA-N calcium;iron;tetrahydrate Chemical compound O.O.O.O.[Ca].[Fe].[Fe] WETINTNJFLGREW-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229910001172 neodymium magnet Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 229910001427 strontium ion Inorganic materials 0.000 description 1
- 150000005846 sugar alcohols Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/2608—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
- 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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- 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
- C04B35/2641—Compositions containing one or more ferrites of the group comprising rare earth metals and one or more ferrites of the group comprising alkali metals, alkaline earth metals or lead
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- C—CHEMISTRY; METALLURGY
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- 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
- H01F1/12—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 soft-magnetic materials
- H01F1/34—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 soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/342—Oxides
- H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
- H01F1/348—Hexaferrites with decreased hardness or anisotropy, i.e. with increased permeability in the microwave (GHz) range, e.g. having a hexagonal crystallographic structure
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01F41/0266—Moulding; Pressing
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
- C04B2235/3203—Lithium oxide or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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Abstract
The invention discloses a kind of hexagonal sintered permanent ferrite magnet and preparation method thereof, belong to Permanent magnetic ferrite field.Hexagonal sintered permanent ferrite its composition formula of magnet A of the present invention2+ 1‑x‑yB1+ yLa3+ xFe3+ n‑zCo2+ zO2‑ 19Represent, A is at least one of divalent alkaline-earth metal calcium, strontium, barium, B is at least one of monovalence alkali metal lithium, sodium, potassium, x, y, z, n are the adding proportion of each element, and wherein x is that 0.24 0.45, y is 0.03 0.10, z is 0.20 0.33, n is 10.0 12.0, and 1.1z≤x≤1.8z, y+z≤x.Its preparation method includes the processes such as dispensing mixing, pre-burning, coarse crushing, ball milling, shaping, sintering.The magnet of the present invention substantially has M type magnetoplumbite types, has higher remanent magnetization, HCJ and squareness ratio Hk/Hcj than traditional Permanent magnetic ferrite, and magnetic property is substantially optimized.
Description
Technical field
The present invention relates to Permanent magnetic ferrite technical field, more specifically to a kind of hexagonal sintering permanent magnet
Ferrimagnet and preparation method thereof.
Background technology
M type Magnetoplumbite permanent magnetic ferrite magnet is by divalent cation metal oxide (SrO and BaO) and di-iron trioxide
(Fe2O3) general name of compound that is constituted, Permanent magnetic ferrite is widely applicable for automobile, household electrical appliance, industrial automation
Etc. industry.As permanent-magnet ferrite material, the strontium ferrite (SrFe with M type magnetoplumbite types12O19) and barium ferrite
(BaFe12O19) be widely used.Main two parameters of the magnetic property of sintered permanent ferrite are influenceed, as residual flux is close
Spend (Br) and HCJ (Hcj).The residual magnetic flux density (Br) of magnet is by density, the degree of orientation and depending on crystal structure
Saturation magnetization (4 π Is) is determined that Br is expressed as the Br=4 π Is × degree of orientation × density；On the other hand, by 4 π I-H magnetic hysteresis
The HCJ (Hcj) that the intersection point of loop line and H axles is provided is proportional to HA× fc, wherein (HA=2K1/Is) it is anisotropy field,
Fc is the ratio of single domain particle, and K1 is anisotropy constant, is also determined as Is by crystal structure.
High performance sintered permanent ferrite magnet application is further extensive at present, in particular with intelligence machine, automobile electricity
The miniaturization of machine rotor and light weight development, and the Ferrite method (switching to ferrite by neodymium iron boron) of frequency-changeable compressor magnet are all needed
With high performance sintered permanent ferrite magnet.
In recent years, the developmental research on high performance sintered Permanent magnetic ferrite has pointed out：In above-mentioned strontium ferrite
(SrFe12O19) in, replace a part for strontium (Sr) with rare earth elements such as lanthanums (La), a part for iron (Fe) is replaced with cobalt (Co)
Strontium lanthanum cobalt (SrLaCo) ferrite, can improve residual magnetic flux density (Br) and HCJ (Hcj).In addition, also
There is research to have pointed out：In the same manner as the situation of strontium ferrite, in calcium ferrite (CaFe12O19) in also with lanthanum (La) replace calcium
(Ca) a part, replace a part for iron (Fe) with cobalt (Co) and generate calcium lanthanum cobalt (CaLaCo) ferrite, due to calcium iron oxygen
The lanthanum cobalt replacement amount of body is higher, thus can obtain higher residual magnetic flux density (Br) and HCJ (Hcj).At present this
Processing mode is planted in industry to be developed rapidly.
Through retrieval, China Patent Publication No. CN1472166A discloses a kind of citric acid complex and prepares M- type ferrites nanometer
The method of micro mist, replaces Ba or Sr ions with alkali metal group element portions, and the ion for generating nanometer can use 3d transition groups
Element and ionic radius replace Fe ions for 0.06-0.1 nanometers of ionic portions；But this application case is micro- for producing nanometer
Powder, has essence different with the production process of sintered permanent ferrite magnet.And for example Chinese patent publication No. CN104350029A is public
A kind of manufacture method of sintered magnet Sr ferrite particles is opened, with alkali metal compound mixing come modulating mixture, alkali gold
Accessory has K and Na at least one and without Cl and S as constitution element, but the purpose of this application case is by improving crystal grain
Shape obtain magnetic property improve, it is impossible to fundamentally improve magnet internal state, and this application case obtain magnetic property still compared with
It is low, it is impossible to meet production requirement.
Through retrieval, the existing patent of lasting research on high performance sintered Permanent magnetic ferrite is disclosed, such as Chinese patent
Application number 988001624 is there is provided a kind of strontium lanthanum cobalt (SrLaCo) ferrite lattice, and it is that 4480Gs, Hcj are to obtain Br
4510Oe preferable magnetic property, but such a magnet rectangular degree is relatively low, and Hk/Hcj only has 0.84.And for example Chinese patent notification number
CN101786869B is there is provided a kind of calcium lanthanum cobalt (CaLaCo) ferrite, and it is that 4200-4700Gs, Hcj are 4500- to obtain Br
6200Oe magnetic property, but this application case requires that cobalt must be added in Primary batching system during processing, and production cost is higher.For another example in
State patent publication No. CN101552069A is there is provided a kind of calcium lanthanum cobalt (CaLaCo) ferrite, while obtaining permanent-magnet ferrite
Br is more than 4500Gs, while Hcj is more than 5000Oe excellent magnetic energy, but this application case requires that shaping slurry particle mean size is less than
0.65 μm, difficulty of processing is larger.
Above-mentioned patent in order to obtain high remanent magnetism and high HCJ Permanent magnetic ferrite simultaneously, and its common ground is：1、
By increasing the replacement of lanthanum cobalt to improve the intrinsic magnetic parameter saturation magnetization (4 π Is) and anisotropy field (H of materialA=
2K1/Is)；2nd, the granularity that slurry is molded by reducing obtains high-performance to improve the single domain particle ratio of magnet；3rd, due into
The reduction of type Slurry Granularity, in order to improve the degree of orientation, dispersant is added in secondary ball milling；These have resulted in production cost
Increase and production efficiency decline, influence enterprise productivity effect.
The content of the invention
1. the invention technical problem to be solved
It is an object of the invention to overcome Permanent magnetic ferrite remanent magnetization and HCJ in the prior art
Not good not enough of magnetic property there is provided a kind of hexagonal sintered permanent ferrite magnet and preparation method thereof, the magnet base
In sheet have M type magnetoplumbite types, it is extremely useful for extensive magnetic application field, such as intelligence machine, automobile, household electrical appliance or
Electric tool etc., and there is higher remanent magnetization, HCJ and squareness ratio than traditional Permanent magnetic ferrite
Hk/Hcj, magnetic property is substantially optimized.
2. technical scheme
To reach above-mentioned purpose, the technical scheme that the present invention is provided is：
A kind of hexagonal sintered permanent ferrite magnet of the present invention, its composition formula A2+ 1-x-yB1+ yLa3+ xFe3+ n- zCo2+ zO2- 19Represent, A is at least one of divalent alkaline-earth metal calcium, strontium, barium, B be in monovalence alkali metal lithium, sodium, potassium extremely
Few one kind, x, y, z, n are the adding proportion of each element, and wherein x is 0.24-0.45, and y is 0.03-0.10, and z is 0.20-0.33, n
For 10.0-12.0, and 1.1z≤x≤1.8z, y+z≤x.
A kind of preparation method of hexagonal sintered permanent ferrite magnet of the present invention, comprises the following steps：
Step 1: dispensing is mixed：By A2+ 1-x-yB1+ yLa3+ xFe3+ n-zCo2+ zO2- 19Composition formula weigh and calculate containing required
The material powder of element, raw material is well mixed by wet process, and incorporation time is 1-3 hours, mixed mixed material
Particle mean size is 0.6-1.2um, and wherein A is at least one of divalent alkaline-earth metal calcium, strontium, barium, B be monovalence alkali metal lithium,
At least one of sodium, potassium, x, y, z, n are the adding proportion of each element, and x is 0.24-0.45, and y is 0.03-0.10, and z is
0.20-0.33, n are 10.0-12.0, and 1.1z≤x≤1.8z, y+z≤x；
Step 2: pre-burning：By the mixed material in step one, pre-burning obtains Preburning material particle in atmosphere, and calcined temperature is
1150-1250 DEG C, soaking time is 1-3 hours；
Step 3: coarse crushing：It is 3- that Preburning material particle in step 2 is carried out into dry type ball mill grinding to particle mean size
5um, obtains pre-burning feed powder；
Step 4: ball milling：Secondary additive is added in weight proportion mode into above-mentioned Preburning material powder, by gained mixture
0.7-1.1 μm is reached using the particle mean size of wet ball-milling mode continuously grinding to particle；
Step 5: shaping：The slurry dewatering processing that step 4 is obtained, then carries out pressing under magnetic field；
Step 6: sintering：Formed body in step 5 is sintered in oxidizing atmosphere.
Further, the A in step one be divalent alkaline-earth metal calcium, strontium, the mixing of barium, B be monovalence alkali metal lithium,
The mixing of sodium, potassium.
Further, the material powder in step one includes calcium carbonate powder, strontium carbonate powder, barium carbonate powder, carbon
Sour lithium powder, powdered sodium carbonate, potassium carbonate powder, lanthanum oxide powder, cobalt oxide powder and croci.
Further, dewater treatment is adjusted to pulp density in 60-65wt% in step 5, and forming magnetic field intensity is not small
In 500kA/m.
Further, sintering temperature is 1200-1250 DEG C in step 6, is incubated 1.0-3.0 hours.
Further, in the mixing of step one dispensing, in addition to additive silica, boric acid, an alkali metal chlorination
One kind or mixing of thing and alkaline earth metal chloride, its adding proportion is：Silica 0.05-0.5wt%, boric acid 0.05-
0.2wt%, alkali metal chloride 0.10-0.5wt%, alkaline earth metal chloride 0.10-0.50wt%, wherein alkali metal be lithium,
At least one of sodium, potassium, alkaline-earth metal are at least one of barium, strontium, calcium.
Further, secondary additive includes CaCO in step 43Powder, SiO2Powder, Al2O3Powder, Cr2O3Powder
End, H3BO3Powder, La2O3At least one of powder, alkali metal chloride powder and alkaline earth metal chloride powder, wherein respectively
The particle mean size of compound powder is not more than 2.0um, and wherein alkali metal is at least one of lithium, sodium, potassium, and alkaline-earth metal is
At least one of barium, strontium, calcium.
Further, the adding proportion of each secondary additive is：CaCO3：0.3~1.5wt%, SiO2：0.1~
0.5wt%, Al2O3：0.1~1.5wt%, Cr2O3：0.1~1.5wt%, H3BO3：0.05~0.2wt%, La2O3：0.05~
0.5wt%, alkali metal chloride：0.1-0.4wt%, alkaline earth metal chloride：0.1-0.5wt%.
Further, in step 4 ball milling process, a certain amount of dispersant need to be added, dispersant be calcium gluconae,
One or more in D-sorbite, ascorbic acid, addition is the 0.2-1.0wt% of total Ingredients Weight.
3. beneficial effect
The technical scheme provided using the present invention, compared with prior art, with following remarkable result：
(1) a kind of hexagonal sintered permanent ferrite magnet of the invention, is mended by adding monovalence alkali metal ion
The imbalance state of chemical valence, reduces the stacking fault problem of cobalt, with identical lanthanum again after ferrite is generated when repaying the substitution of lanthanum cobalt ions
Cobalt addition compares the residual magnetic flux density (Br) for significantly improving magnet, and maintains higher coercivity (Hcj), and magnet is comprehensive
Performance is closed to make moderate progress；
(2) preparation method of a kind of hexagonal sintered permanent ferrite magnet of the invention, can under same magnetic properties
To reduce the consumption of noble metal cobalt, there is higher cost performance on production cost；
(3) a kind of preparation method of hexagonal sintered permanent ferrite magnet of the invention, secondary addition alkali metal chlorine
Compound, can reduce double sintering radial contraction ratio, be more beneficial for production, help to reduce production cost, improve production efficiency；
(4) preparation method of a kind of hexagonal sintered permanent ferrite magnet of the invention, acquisition it is high performance sintered
The Br of Permanent magnetic ferrite is higher than 4350Gs, and Hcj is higher than 4500Oe, and rectangular degree Hk/Hcj is higher than 0.92, magnet combination property
It is obviously improved.
Brief description of the drawings
Fig. 1 is a kind of flow chart of the preparation method of hexagonal sintered permanent ferrite magnet of the present invention.
Embodiment
To further appreciate that present disclosure, with reference to accompanying drawing, the present invention is described in detail.
With reference to embodiment, the invention will be further described.
Research on high performance sintered Permanent magnetic ferrite is long-standing, and research finds to use and taken by adding lanthanum cobalt
Magnetic property is favorably improved for permanent-magnet ferrite, and trivalent lanthanum ion and divalent cobalt ion are theoretical when keeping ion valence mumber balance
Upper lanthanum ion molal quantity and cobalt ions molal quantity should be equal, but found in actual production it is above-mentioned in the case of cobalt ions can produce substantially
Stacking fault phenomenon, cause magnetic property to decline, particularly squareness ratio Hk/Hcj is relatively low, magnet combination property is not good enough, research hair
Now by improve the molal quantity of lanthanum ion can reduce cobalt ions produce stacking fault, especially when lanthanum ion molal quantity reach cobalt from
The stacking fault that cobalt ions is produced at 1.2-1.5 times of sub- molal quantity can be eliminated substantially, but facts have proved under such a state
Its magnetic field performance of permanent-magnet ferrite still suffers from many deficiencies, and performance still needs to optimization, further researchs and analyses discovery due to now forever
The ion combination valency of magnetic ferrites is difficult to reach balance, causes magnetic field performance to be still weak, and how to realize chemical valence tends to be flat
Weighing apparatus and the all-win situation of elimination stacking fault are the problems that technical staff needs to overcome.
A kind of hexagonal sintered permanent ferrite magnet of the present invention, its composition formula A2+ 1-x-yB1+ yLa3+ xFe3+ n- zCo2+ zO2- 19Represent, A is at least one of divalent alkaline-earth metal calcium, strontium, barium, B be in monovalence alkali metal lithium, sodium, potassium extremely
Few one kind, x, y, z, n are the adding proportion of each element, and wherein x is 0.24-0.45, and y is 0.03-0.10, and z is 0.20-0.33, n
For 10.0-12.0, and 1.1z≤x≤1.8z, y+z≤x.The magnet that the present invention is provided has higher remanent magnetization, interior
Coercivity and squareness ratio Hk/Hcj are reported, magnetic property is substantially optimized, and realizes above-mentioned all-win situation.
The present invention participates in the substitution of lanthanum cobalt jointly by adding monovalence alkali metal, makes its mutual coordinated, monovalence alkali metal
It is engaged complementary common substitution divalent alkaline-earth metal with lanthanum ion, and cobalt ions remains unchanged substitution iron ion, and by each substitution
The accurate control of element, also avoids the serious unbalance of chemical valence while avoiding and producing cobalt ions stacking fault, and combines life
The strict cooperation control of production. art, is obviously improved the magnetic property of final magnet.Said with reference to specific embodiment
It is bright.
Embodiment 1
A kind of hexagonal sintered permanent ferrite magnet of the present embodiment, its composition formula A2+ 1-x-yB1+ yLa3+ xFe3+ n- zCo2+ zO2- 19Represent, A be divalent alkaline-earth metal calcium, strontium, the mixing of barium, B be monovalence alkali metal lithium, sodium, the mixing of potassium, x, y, z,
N is the adding proportion of each element, and wherein x is 0.24-0.45, and y is 0.03-0.10, and z is 0.20-0.33, and n is 10.0-12.0,
And 1.1z≤x≤1.8z, y+z≤x.As shown in figure 1, its preparation method comprises the following steps：
Step 1: dispensing is mixed：By A2+ 1-x-yB1+ yLa3+ xFe3+ n-zCo2+ zO2- 19Composition formula weigh and calculate containing required
The material powder of element, raw material is uniformly mixed 1 hour by wet process, and mixed mixed material particle mean size reaches
0.6um, reactivity more preferably, ensures that energy pre-burning is abundant in follow-up burn-in process, it is to avoid the generation ferritic content of hexagonal crystalline phase
It is too low；The granule size of raw material mixed once carries out influenceing great for subsequent reactions, and Slurry Granularity is excessive easily to cause pre-burning
Insufficient, undersized can then cause the decline of secondary ball milling characteristic again, and (the granularity crystallization of mixed once determines that whole crystal grain is big
Small, secondary ball milling is then that solid phase reaction, particle infiltration occur for crystal grain to be opened)；It should be noted that A is divalent alkaline-earth metal
Calcium, strontium, the mixing of barium, B are monovalence alkali metal lithium, sodium, the mixing of potassium, and x, y, z, n are the adding proportion of each element, and x is 0.24-
0.45, y is 0.03-0.10, and z is 0.20-0.33, and n is 10.0-12.0, and 1.1z≤x≤1.8z, y+z≤x；
Specific material powder is iron oxide (Fe2O3) powder (purity >=99.0wt%, the original mean particle of particle：
0.7~1.0um), calcium carbonate (CaCO3) powder (purity >=98.5wt%, the original mean particle of particle：2.0~5.0um),
Strontium carbonate (SrCO3) powder (purity >=98.5wt%, the original mean particle of particle：1.0~2.0um), barium carbonate (BaCO3)
Powder (purity >=98.5wt%, the original mean particle of particle：1.0~2.0um), lanthana (La2O3) powder (purity >=
99.0wt%, particle original mean particle：2.0~5.0um), cobalt oxide (Co2O3) powder (purity >=99.0wt%, particle
Original mean particle：2.0~5.0um), lithium carbonate (Li2CO3) powder (purity >=99.0wt%, the original average grain of particle
Degree：2.0~5.0um), sodium carbonate (Na2CO3) powder (purity >=99.0wt%, the original mean particle of particle：2.0~
5.0um), potassium carbonate (K2CO3) powder (purity >=99.0wt%, the original mean particle of particle：2.0~5.0um)；Also add
Once additive silica, boric acid, alkali metal (lithium, sodium, potassium) chloride and alkaline-earth metal (barium, strontium, calcium) chloride, have
Body adds 0.05wt% SiO2Powder (purity >=98.0wt%, the original mean particle of particle：1.0um), 0.05wt%
H3BO3Powder (purity >=99.0wt%), 0.10wt% alkali metal chloride, 0.10wt% alkaline earth metal chloride.
Step 2: pre-burning：By the mixed material in step one, pre-burning obtains Preburning material particle, calcined temperature control in atmosphere
System is at 1150 DEG C, and soaking time is 1 hour；
Step 3: coarse crushing：It is 3.0um that Preburning material particle in step 2 is carried out into dry type ball mill grinding to particle mean size
Coarse powder, obtain pre-burning feed powder；
Step 4: ball milling：Secondary additive is added in weight proportion mode into above-mentioned Preburning material powder, by gained mixture
Thicker 0.7 μm is reached using the particle mean size of wet ball-milling mode continuously grinding to particle；Due to the addition of monovalence alkali metal
So that reactivity is higher, reaction is more easy to, therefore ball milling granularity is appropriate partially thick so that processing cost is reduced, and processing is easier to grasp
Make；
Specifically, 500 grams of the coarse powder material that step 3 is obtained is weighed, 0.30wt% CaCO is added3, 0.1wt% SiO2、
0.1wt% Al2O3, 0.1wt% Cr2O3, 0.05wt% H3BO3, 0.05wt% La2O3, 0.1wt% alkali metal chlorine
Compound (lithium chloride, sodium chloride, the mixing of potassium chloride), 0.1wt% alkaline earth metal chloride (barium chloride, strontium chloride, calcium chloride
Mixing), wherein the particle mean size of each compound powder is not more than 2.0um, also add 0.20wt% calcium gluconae, sorb
The mixing of sugar alcohol, ascorbic acid, then 700 milliliters of water is added, case of wet attrition is carried out, particle mean size 0.7um ferrite is obtained
Slurry；
Step 5: shaping：The slurry dewatering processing that step 4 is obtained, can be taken off using centrifugation or press filtration mode
Water, pulp density is in 60wt%, then in applied field strengths 700kA/m parallel magnetic field, with briquetting pressure 0.4ton/
cm3Shaping is compressed, gained formed body is a diameter of 40mm, height 15mm cylinder；
Step 6: sintering：Formed body is heat-treated with 100-500 DEG C of temperature, moisture and organic dispersing agent is removed,
Then it is 120 DEG C/h with programming rate to be heated up, with 1200 DEG C of temperature sintered heat insulatings 1 hour in oxidizing atmosphere, obtains
Sintered permanent magnet.
The present embodiment makes itself and lanthanum cobalt phase coordinated, permanent magnet is participated in jointly by a certain proportion of monovalence alkali metal
Ferrite magnet inner ion replaces, while cobalt ions stacking fault problem is cancelled, and reduces chemical valence inside magnet and seriously loses
Weigh phenomenon, internal chemical valence is tended to balance, and is adjusted to tackling each manufacturing procedure, the high-performance for obtaining final sintering
The Br of sintered permanent ferrite magnet is higher than 4350Gs, and Hcj is higher than 4500Oe, and rectangular degree Hk/Hcj is higher than 0.92, and magnet is integrated
Performance is obviously improved.
Embodiment 2
A kind of hexagonal sintered permanent ferrite magnet of the present embodiment, its composition formula A2+ 1-x-yB1+ yLa3+ xFe3+ n- zCo2+ zO2- 19Represent, A is divalent alkaline-earth metal calcium, B is monovalence alkali metal lithium, and x, y, z, n are the adding proportion of each element, wherein
X is 0.24-0.45, and y is 0.03-0.10, and z is 0.20-0.33, and n is 10.0-12.0, and 1.1z≤x≤1.8z, y+z≤x.Its
The basic be the same as Example 1 of preparation method, except that, the feed proportioning and processing method of the present embodiment slightly have difference, specifically such as
Under：
Material powder is iron oxide (Fe in step one2O3) powder, calcium carbonate (CaCO3) powder, lanthana (La2O3) powder
End, cobalt oxide (Co2O3) powder, lithium carbonate (Li2CO3) powder；Also add once additive as follows：0.5wt% SiO2Powder
End, 0.2wt% H3BO3Powder, 0.5wt% lithium chloride, 0.5wt% calcium chloride.Above-mentioned dispensing is equal by wet process
Even mixing 3 hours, mixed mixed material particle mean size reaches 1.2um.
Calcined temperature control is at 1250 DEG C in step 2, and soaking time is 3 hours；
Preburning material particle carries out dry type ball mill grinding to the coarse powder that particle mean size is 5.0um in step 3；
Secondary additive is added into obtained coarse powder and dispersant is as follows in step 4：
Add 1.5wt% CaCO3, 0.5wt% SiO2, 1.5wt% Al2O3, 1.5wt% Cr2O3, 0.2wt%
H3BO3, 0.5wt% La2O3, 0.4wt% lithium chloride, 0.5wt% calcium chloride；1.0wt% calcium gluconae.Will
The particle mean size of mixture wet ball-milling to particle reaches 1.1 μm.
Concentration is 65wt% after slurry dewatering in step 5, and forming magnetic field intensity is 800kA/m.
Sintering temperature is 1250 DEG C in step 6, is incubated 3.0 hours.
Embodiment 3
A kind of hexagonal sintered permanent ferrite magnet of the present embodiment, its composition formula A2+ 1-x-yB1+ yLa3+ xFe3+ n- zCo2+ zO2- 19Represent, A is divalent alkaline-earth metal strontium, B is monovalence alkali metallic sodium, and x, y, z, n are the adding proportion of each element, wherein
X is 0.24-0.45, and y is 0.03-0.10, and z is 0.20-0.33, and n is 10.0-12.0, and 1.1z≤x≤1.8z, y+z≤x.Its
The basic be the same as Example 1 of preparation method, except that, the feed proportioning and processing method of the present embodiment slightly have difference, specifically such as
Under：
Material powder is iron oxide (Fe in step one2O3) powder, strontium carbonate (SrCO3) powder, lanthana (La2O3) powder
End, cobalt oxide (Co2O3) powder, sodium carbonate (Na2CO3) powder, also add once additive as follows：0.3wt% chlorination
The strontium chloride of sodium, 0.3wt%.Above-mentioned dispensing is uniformly mixed 2 hours by wet process, the average grain of mixed mixed material
Degree reaches 0.9um.
Calcined temperature control is at 1180 DEG C in step 2, and soaking time is 2 hours；
Preburning material particle carries out dry type ball mill grinding to the coarse powder that particle mean size is 4.0um in step 3；
Secondary additive is added into obtained coarse powder and dispersant is as follows in step 4：
Add 0.2wt% sodium chloride, 0.3wt% strontium chloride；0.6wt% D-sorbite.By mixture wet type ball
The particle mean size for being milled to particle reaches 0.9 μm.
Concentration is 63wt% after slurry dewatering in step 5, and forming magnetic field intensity is 900kA/m.
Sintering temperature is 1230 DEG C in step 6, is incubated 2.0 hours.
Embodiment 4
A kind of hexagonal sintered permanent ferrite magnet of the present embodiment, its composition formula A2+ 1-x-yB1+ yLa3+ xFe3+ n- zCo2+ zO2- 19Represent, A is divalent alkaline-earth metal barium, B is monoacidic base metallic potassium, and x, y, z, n are the adding proportion of each element, wherein
X is 0.24-0.45, and y is 0.03-0.10, and z is 0.20-0.33, and n is 10.0-12.0, and 1.1z≤x≤1.8z, y+z≤x.Its
The basic be the same as Example 1 of preparation method, except that, the feed proportioning and processing method of the present embodiment slightly have difference, specifically such as
Under：
Material powder is iron oxide (Fe in step one2O3) powder, barium carbonate (BaCO3) powder, lanthana (La2O3) powder
End, cobalt oxide (Co2O3) powder, potassium carbonate (K2CO3) powder, also add once additive as follows：0.1wt% boric acid,
0.3wt% potassium chloride, 0.3wt% barium chloride.Above-mentioned dispensing is uniformly mixed 2 hours by wet process, it is mixed
Mixed material particle mean size reaches 0.8um.
Calcined temperature control is at 1200 DEG C in step 2, and soaking time is 3 hours；
Preburning material particle carries out dry type ball mill grinding to the coarse powder that particle mean size is 3.0um in step 3；
Secondary additive is added into obtained coarse powder and dispersant is as follows in step 4：
Add 1.5wt% CaCO3The SiO of powder, 0.3wt%2Powder, 0.2wt% potassium chloride, 0.3wt% chlorination
Barium；1.0wt% ascorbic acid.The particle mean size of said mixture wet ball-milling to particle is reached 1.1 μm.
Concentration is 60wt% after slurry dewatering in step 5, and forming magnetic field intensity is 600kA/m.
Sintering temperature is 1200 DEG C in step 6, is incubated 1.8 hours.
Embodiment 5
A kind of hexagonal sintered permanent ferrite magnet of the present embodiment, its composition formula A2+ 1-x-yB1+ yLa3+ xFe3+ n- zCo2+ zO2- 19Represent, A is divalent alkaline-earth metal calcium, strontium, B is monovalence alkali metal lithium, sodium, and x, y, z, n are the addition ratio of each element
Example, wherein x is 0.24-0.45, and y is 0.03-0.10, and z is 0.20-0.33, and n is 10.0-12.0, and 1.1z≤x≤1.8z, y+
z≤x.The basic be the same as Example 1 of its preparation method, except that, the feed proportioning and processing method of the present embodiment slightly have difference,
It is specific as follows：
Material powder is iron oxide (Fe in step one2O3) powder, calcium carbonate (CaCO3) powder, strontium carbonate (SrCO3) powder
End, lanthana (La2O3) powder, cobalt oxide (Co2O3) powder, lithium carbonate (Li2CO3) powder, sodium carbonate (Na2CO3) powder, also
Once additive is as follows for addition：0.3wt% lithium chloride is mixed with sodium chloride, 0.3wt% calcium chloride and strontium chloride are mixed.
Above-mentioned dispensing is uniformly mixed 2 hours by wet process, mixed mixed material particle mean size reaches 0.8um.
Calcined temperature control is at 1200 DEG C in step 2, and soaking time is 3 hours；
Preburning material particle carries out dry type ball mill grinding to the coarse powder that particle mean size is 3.0um in step 3；
Secondary additive is added into obtained coarse powder and dispersant is as follows in step 4：
Add 0.3wt% SiO2Powder, 0.2wt% lithium chloride and sodium chloride, 0.3wt% calcium chloride and chlorination
Strontium；The mixing of 1.0wt% calcium gluconae, D-sorbite.
Concentration is 61wt% after slurry dewatering in step 5, and forming magnetic field intensity is 650kA/m.
Sintering temperature is 1220 DEG C in step 6, is incubated 1.5 hours.
Embodiment 6
A kind of hexagonal sintered permanent ferrite magnet of the present embodiment, its composition formula A2+ 1-x-yB1+ yLa3+ xFe3+ n- zCo2+ zO2- 19Represent, A is divalent alkaline-earth metal calcium, barium, B is monovalence alkali metal lithium, potassium, and x, y, z, n are the addition ratio of each element
Example, wherein x is 0.24-0.45, and y is 0.03-0.10, and z is 0.20-0.33, and n is 10.0-12.0, and 1.1z≤x≤1.8z, y+
z≤x.The basic be the same as Example 1 of its preparation method, except that, the feed proportioning and processing method of the present embodiment slightly have difference,
It is specific as follows：
Material powder is iron oxide (Fe in step one2O3) powder, calcium carbonate (CaCO3) powder, barium carbonate (BaCO3) powder
End, lanthana (La2O3) powder, cobalt oxide (Co2O3) powder, lithium carbonate (Li2CO3) powder, potassium carbonate (K2CO3) powder, also add
It is as follows added with an additive：0.3wt% lithium chloride and potassium chloride, 0.3wt% calcium chloride and barium chloride.
Secondary additive is added into obtained coarse powder and dispersant is as follows in step 4：
Add 0.2wt% lithium chloride and potassium chloride, 0.3wt% calcium chloride and barium chloride；1.0wt% gluconic acid
Calcium and ascorbic acid.
Embodiment 7
A kind of hexagonal sintered permanent ferrite magnet of the present embodiment, its composition formula A2+ 1-x-yB1+ yLa3+ xFe3+ n- zCo2+ zO2- 19Represent, A is divalent alkaline-earth metal strontium, barium, B is monovalence alkali metallic sodium, potassium, and x, y, z, n are the addition ratio of each element
Example, wherein x is 0.24-0.45, and y is 0.03-0.10, and z is 0.20-0.33, and n is 10.0-12.0, and 1.1z≤x≤1.8z, y+
z≤x.The basic be the same as Example 1 of its preparation method, except that, the feed proportioning and processing method of the present embodiment slightly have difference,
It is specific as follows：
Material powder is iron oxide (Fe in step one2O3) powder, strontium carbonate (SrCO3) powder, barium carbonate (BaCO3) powder
End, lanthana (La2O3) powder, cobalt oxide (Co2O3) powder, sodium carbonate (Na2CO3) powder, potassium carbonate (K2CO3) powder, also add
It is as follows added with an additive：0.3wt% sodium chloride and potassium chloride, 0.3wt% strontium chloride and barium chloride.
Secondary additive is added into obtained coarse powder and dispersant is as follows in step 4：
Add 0.2wt% sodium chloride and potassium chloride, 0.3wt% strontium chloride and barium chloride；1.0wt% sorbose
Alcohol, ascorbic acid.
Similarly, for dispensing selection and the control of preparation technology still has multiple combinations mode, and this is no longer going to repeat them.
Part ferrimagnet sample composition prepared by above example is analyzed, expression combined type is determined
Cas1Srs2Bas3Liy1Nay2Ky3Lax0FemCo2+ zO2- 19In s1, s2, s3, x0, m, y1, y2, y3, z, m measure is using titration
Method, s1, s2, s3, x0, y1, y2, y3, z measure uses x-ray fluorescence analysis, and measures the magnetic with magnetism testing instrument
Institute in residual magnetic flux density (Br), HCJ (Hcj) and the rectangular degree (Hk/Hcj) of body sample, measurement result such as table 1
Show, and the measurement result of the comparative sample of the part ferrimagnet processed using traditional preparation method is then as shown in table 2.
Table 1
Table 2
It can be seen from the above results by add monovalence alkali metal lithium, sodium, potassium carbonate, magnetic can be significantly improved
Every magnetic property of body, its overall performance makes moderate progress, and especially rectangular degree performance is substantially better than prior art, in certain limit
The addition of interior monovalence alkali metal increases to the HCJ of magnet, remanent magnetism performance, and it combines addition more to the whole of magnet
Body has been adjusted.With reference to the preparation technology of the present embodiment, the consumption of noble metal cobalt can be reduced under same magnetic properties, in production
There is higher cost performance in cost；And by secondary addition alkali metal chloride, can effectively reduce double sintering radial contraction
Than being more beneficial for production, helping to reduce production cost, improve production efficiency.
Schematical above that the present invention and embodiments thereof are described, the description does not have restricted, institute in accompanying drawing
What is shown is also one of embodiments of the present invention, and actual structure is not limited thereto.So, if the common skill of this area
Art personnel are enlightened by it, without departing from the spirit of the invention, are designed and the technical scheme without creative
Similar frame mode and embodiment, all should belong to protection scope of the present invention.
Claims (10)
1. a kind of hexagonal sintered permanent ferrite magnet, it is characterised in that：Its composition formula A2+ 1-x-yB1+ yLa3+ xFe3+ n-
zCo2+ zO2- 19Represent, A is at least one of divalent alkaline-earth metal calcium, strontium, barium, B be in monovalence alkali metal lithium, sodium, potassium extremely
Few one kind, x, y, z, n are the adding proportion of each element, and wherein x is 0.24-0.45, and y is 0.03-0.10, and z is 0.20-0.33, n
For 10.0-12.0, and 1.1z≤x≤1.8z, y+z≤x.
2. a kind of preparation method of hexagonal sintered permanent ferrite magnet, it is characterised in that comprise the following steps：
Step 1: dispensing is mixed：By A2+ 1-x-yB1+ yLa3+ xFe3+ n-zCo2+ zO2- 19Composition formula weigh and calculate containing required element
Material powder, raw material is well mixed by wet process, and incorporation time is 1-3 hours, the average grain of mixed mixed material
Spend for 0.6-1.2um, wherein A is at least one of divalent alkaline-earth metal calcium, strontium, barium, during B is monovalence alkali metal lithium, sodium, potassium
At least one, x, y, z, n be each element adding proportion, x is 0.24-0.45, and y is 0.03-0.10, and z is 0.20-0.33, n
For 10.0-12.0, and 1.1z≤x≤1.8z, y+z≤x；
Step 2: pre-burning：By the mixed material in step one, pre-burning obtains Preburning material particle in atmosphere, and calcined temperature is
1150-1250 DEG C, soaking time is 1-3 hours；
Step 3: coarse crushing：It is 3-5um that Preburning material particle in step 2 is carried out into dry type ball mill grinding to particle mean size, is obtained
To pre-burning feed powder；
Step 4: ball milling：Secondary additive is added in weight proportion mode into above-mentioned Preburning material powder, gained mixture is used
The particle mean size of wet ball-milling mode continuously grinding to particle reaches 0.7-1.1 μm；
Step 5: shaping：The slurry dewatering processing that step 4 is obtained, then carries out pressing under magnetic field；
Step 6: sintering：Formed body in step 5 is sintered in oxidizing atmosphere.
3. a kind of preparation method of hexagonal sintered permanent ferrite magnet according to claim 2, it is characterised in that：
A in step one is divalent alkaline-earth metal calcium, strontium, the mixing of barium, and B is monovalence alkali metal lithium, sodium, the mixing of potassium.
4. a kind of preparation method of hexagonal sintered permanent ferrite magnet according to Claims 2 or 3, its feature exists
In：Material powder in step one includes calcium carbonate powder, strontium carbonate powder, barium carbonate powder, lithium carbonate powder, carbonic acid sodium powder
End, potassium carbonate powder, lanthanum oxide powder, cobalt oxide powder and croci.
5. a kind of preparation method of hexagonal sintered permanent ferrite magnet according to claim 2, it is characterised in that：
Dewater treatment is adjusted to pulp density in 60-65wt% in step 5, and forming magnetic field intensity is not less than 500kA/m.
6. a kind of preparation method of hexagonal sintered permanent ferrite magnet according to claim 2, it is characterised in that：
Sintering temperature is 1200-1250 DEG C in step 6, is incubated 1.0-3.0 hours.
7. a kind of preparation method of hexagonal sintered permanent ferrite magnet according to claim 2, it is characterised in that：
In the mixing of step one dispensing, in addition to additive silica, boric acid, alkali metal chloride and alkaline earth metal chloride
One kind is mixed, and its adding proportion is：Silica 0.05-0.5wt%, boric acid 0.05-0.2wt%, alkali metal chloride
0.10-0.5wt%, alkaline earth metal chloride 0.10-0.50wt%, wherein alkali metal are at least one of lithium, sodium, potassium, alkali
Earth metal is at least one of barium, strontium, calcium.
8. a kind of preparation method of hexagonal sintered permanent ferrite magnet according to claim 2, it is characterised in that：
Secondary additive includes CaCO in step 43Powder, SiO2Powder, Al2O3Powder, Cr2O3Powder, H3BO3Powder, La2O3Powder
At least one of end, alkali metal chloride powder and alkaline earth metal chloride powder, wherein the average grain of each compound powder
Degree is not more than 2.0um, and wherein alkali metal is at least one of lithium, sodium, potassium, and alkaline-earth metal is at least one in barium, strontium, calcium
Kind.
9. a kind of preparation method of hexagonal sintered permanent ferrite magnet according to claim 8, it is characterised in that：
The adding proportion of each secondary additive is：CaCO3：0.3~1.5wt%, SiO2：0.1~0.5wt%, Al2O3：0.1~
1.5wt%, Cr2O3：0.1~1.5wt%, H3BO3：0.05~0.2wt%, La2O3：0.05~0.5wt%, alkali metal chlorination
Thing：0.1-0.4wt%, alkaline earth metal chloride：0.1-0.5wt%.
10. a kind of preparation method of hexagonal sintered permanent ferrite magnet according to any one of claim 2~9,
It is characterized in that：In step 4 ball milling process, a certain amount of dispersant need to be added, dispersant be calcium gluconae, D-sorbite,
One or more in ascorbic acid, addition is the 0.2-1.0wt% of total Ingredients Weight.
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Denomination of invention: A hexagonal crystalline sintered permanent magnet ferrite magnet and its preparation method Effective date of registration: 20230712 Granted publication date: 20180116 Pledgee: Anhui Ma'anshan Rural Commercial Bank Co.,Ltd. Pledgor: MAANSHAN XINYANG PERMANENT MAGNET Co.,Ltd. Registration number: Y2023980048114 |