CN117105654A - Permanent magnetic strontium ferrite magnetic powder and preparation method and application thereof - Google Patents
Permanent magnetic strontium ferrite magnetic powder and preparation method and application thereof Download PDFInfo
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- CN117105654A CN117105654A CN202311065175.6A CN202311065175A CN117105654A CN 117105654 A CN117105654 A CN 117105654A CN 202311065175 A CN202311065175 A CN 202311065175A CN 117105654 A CN117105654 A CN 117105654A
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- strontium ferrite
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- 239000006247 magnetic powder Substances 0.000 title claims abstract description 84
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 77
- 229910052712 strontium Inorganic materials 0.000 title claims abstract description 76
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 20
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 47
- 238000000498 ball milling Methods 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 21
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 4
- 238000007493 shaping process Methods 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 4
- 230000002349 favourable effect Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 24
- 239000002002 slurry Substances 0.000 description 17
- 239000012071 phase Substances 0.000 description 8
- 238000002156 mixing Methods 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000002270 dispersing agent Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 229960004494 calcium gluconate Drugs 0.000 description 4
- 239000004227 calcium gluconate Substances 0.000 description 4
- 235000013927 calcium gluconate Nutrition 0.000 description 4
- 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 4
- 230000007423 decrease Effects 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 230000005389 magnetism Effects 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 229910000018 strontium carbonate Inorganic materials 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 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
- 230000000996 additive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
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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
- C04B35/2608—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
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- 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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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- 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
- H01F1/032—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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- 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
- 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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- 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
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- 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
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention provides permanent magnetic strontium ferrite magnetic powder, a preparation method and application thereof, wherein the chemical formula of the permanent magnetic strontium ferrite magnetic powder is as follows: sr (Sr) 1‑x La x Fe 12‑y Al y O 19 Wherein x is more than 0 and less than or equal to 0.3, and y is more than 0 and less than or equal to 0.4. The invention carries out co-doping by introducing La and Al with specific contents, under the synergistic effect of the La and the Al, the intrinsic magnetic property of the magnetic powder can be improved, the remanence of the magnetic powder is reduced, the coercive force is improved, and the magnetic powder can be formed subsequentlyThe forming process brings a good foundation. Meanwhile, the cost can be controlled by adopting La and Al for co-doping, so that the cost is lower. The permanent magnet prepared based on the method has higher Hcj and squareness, and is favorable for fully utilizing the performance of products.
Description
Technical Field
The invention belongs to the technical field of permanent magnetic materials, relates to permanent magnetic strontium ferrite magnetic powder and a preparation method and application thereof, and particularly relates to M-type high-performance permanent magnetic strontium ferrite magnetic powder and a preparation method and application thereof.
Background
The application of rare earth permanent magnetic ferrite relates to various fields of social life. The ferrite has the characteristics of high performance and low cost, and becomes the permanent magnet material with the highest yield and the widest application range. In recent years, with the rapid development of new energy technology in which the drive section in electric vehicles in new energy includes various types of motors, a series of demands for new magnets are made for miniaturization, weight saving and high performance.
Most of the permanent magnetic ferrites at present are strontium ferrites with M-shaped magnetoplumbite structures, and the ferrites are prepared from iron oxide red and strontium carbonate by a solid phase reaction method. However, the magnetic performance of the existing strontium ferrite is difficult to meet the requirements of people on high-performance magnetic materials, and still has an improved space.
The permanent magnetic ferrite magnetic powder can have a certain influence on the performance of the final magnet, and in order to further improve the final magnetic performance, researchers properly adjust the magnetic powder, and the magnetic powder performance is generally reflected on parameters such as saturated magnetization Ms, residual magnetism Mr, coercive force Hc and the like. It is found that substitution of La, co and other elements can greatly improve the magnetic performance of the strontium ferrite material. CN105439551a discloses a high magnetic energy product La-Co-doped strontium ferrite and a preparation method thereof, and specific embodiments thereof are as follows: by SrCO 3 And Fe (Fe) 2 O 3 As raw material, lanthanum oxide La 2 O 3 And cobalt oxide CoO as doping agent, mixing (0.5-0.9) (5.75-5.95) (0.05-0.25) (0.1-0.5), ball milling, drying, crushing, calcining in a muffle furnace, heating to 950-1200 deg.C at 10-20 deg.C/min, and maintaining for two hours to obtain La-Co Co-doped strontium ferrite magnetic material powder.
And, through corresponding production, la-Co substitution can significantly improve magnetic properties, and has been successfully applied commercially. However, the addition of rare earth elements and noble metals adds cost and some complications.
Therefore, it is desirable to provide a solution that can reduce the cost of the strontium ferrite material and can improve its magnetic properties.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide permanent magnetic strontium ferrite magnetic powder and a preparation method and application thereof. According to the permanent magnetic strontium ferrite magnetic powder, la and Al with specific contents are introduced for co-doping, under the synergistic effect of the La and the Al, the intrinsic magnetic property of the magnetic powder can be improved, the residual magnetism of the magnetic powder is reduced, the coercive force is improved, and a good foundation can be brought for a subsequent forming process. Meanwhile, the cost can be controlled by adopting La and Al for co-doping, so that the cost is lower.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a permanent magnetic strontium ferrite powder having the chemical formula: sr (Sr) 1-x La x Fe 12-y Al y O 19 Where 0 < x.ltoreq.0.3 (e.g., may be 0.01, 0.02, 0.03, 0.05, 0.07, 0.1, 0.12, 0.15, 0.17, 0.2, 0.22, 0.25, 0.27, or 0.3, etc.), 0 < y.ltoreq.0.4 (e.g., may be 0.01, 0.02, 0.03, 0.05, 0.07, 0.1, 0.12, 0.15, 0.17, 0.2, 0.22, 0.25, 0.27, 0.3, 0.32, 0.35, 0.37, or 0.4, etc.).
The invention provides a permanent magnetic strontium ferrite magnetic powder, which is co-doped by introducing La and Al with specific contents, and under the synergistic effect of the La and the Al, the intrinsic magnetic property of the magnetic powder can be improved, so that the residual magnetism of the magnetic powder is reduced, the coercive force is improved, and a good foundation can be brought for a subsequent forming process. Meanwhile, the cost can be controlled by adopting La and Al for co-doping, so that the cost is lower. The permanent magnet prepared based on the method has higher Hcj and squareness, and is favorable for fully utilizing the performance of products.
Preferably, the Sr 1-x La x Fe 12-y Al y O 19 In the above, x/y is in the range of 0.25 to 3.0, and may be, for example, 0.25, 0.3, 0.35, 0.5, 1, 1.5, 2, 2.5, or 3.0.
Preferably, the D50 particle size of the permanent magnetic strontium ferrite magnetic powder is 0.56-2.14. Mu.m, for example, 0.56. Mu.m, 0.58. Mu.m, 0.6. Mu.m, 0.7. Mu.m, 0.8. Mu.m, 0.9. Mu.m, 1.2. Mu.m, 1.5. Mu.m, 1.7. Mu.m, 2.1. Mu.m, 2.14. Mu.m, etc.
In a second aspect, the present invention provides a method for preparing the permanent magnetic strontium ferrite magnetic powder according to the first aspect, the method comprising:
(1) According to Sr 1-x La x Fe 12-y Al y O 19 Wherein x is more than 0 and less than or equal to 0.3, and y is more than 0 and less than or equal to 0.4;
(2) And ball-milling the raw materials and roasting to obtain the permanent magnetic strontium ferrite magnetic powder.
Preferably, the feedstock includes an iron source, a strontium source, a lanthanum source, and an aluminum source.
Preferably, the iron source comprises Fe 2 O 3 。
Preferably, the strontium source comprises SrCO 3 。
Preferably, the lanthanum source comprises La 2 O 3 。
Preferably, the aluminum source comprises Al 2 O 3 。
Preferably in Fe 2 O 3 、SrCO 3 、La 2 O 3 And Al 2 O 3 Is 100% of the total mass of Fe 2 O 3 Is 83.04-87.02% by mass of SrCO 3 Is 10.72 to 11.13 mass percent of La 2 O 3 The mass percentage of Al is 1.48-4.34 percent 2 O 3 The mass percentage of (2) is 0.46-2.30%. Wherein Fe is 2 O 3 For example, 83.04%, 83.05%, 83.1%, 83.5%, 84%, 84.5%, 85%, 85.5%, 86%, 86.5% or 87% by mass; srCO 3 For example, the mass percentage of (a) may be 10.72%, 10.8%, 10.9%, 11% or 11.1%; la (La) 2 O 3 For example, 1.48%, 1.5%, 1.52%, 1.58%, 1.6%, 2%, 2.2%, 2.5%, 3%, 3.2%, 3.5%, 4% or 4.2% by mass; al (Al) 2 O 3 For example, the mass percentage of (a) may be 0.46%, 0.5%, 0.53%, 0.7%, 1%, 1.5%, 2% or 2.1%.
Preferably, the purity of the raw material is 97% or more. Illustratively, iron oxide red (Fe 2 O 3 ) Is 99% pure, aluminum oxide (Al) 2 O 3 ) Has a purity of 99.99%, lanthanum oxide (La 2 O 3 ) Has a purity of 99.9%, strontium carbonate (SrCO 3 ) The purity of (2) was 97%.
Preferably, the ball milling in the step (2) is wet ball milling, and the reagent used in the wet ball milling comprises water, wherein the mass ratio of the water to the raw materials is (1.5-2): 1, for example, 1.5:1, 1.6:1, 1.7:1, 1.8:1 or 1.9:1, etc.
Preferably, the ball ratio of the ball milling in the step (2) is 1 (12-16), and can be 1:12, 1:14 or 1:16, for example. Wherein the ball ratio refers to the mass ratio of raw materials to ball grinding balls.
Preferably, the time of ball milling in the step (2) is 2-4h, for example, 2h, 2.5h, 3h, 3.5h or 4h, and the like, preferably 2-3h.
Preferably, in the step (2), between the ball milling and the calcination, the steps of drying and pulverizing are sequentially performed, and the drying temperature is 90-120 ℃, for example, 90 ℃, 95 ℃, 100 ℃, 105 ℃, 110 ℃, 115 ℃, 120 ℃, or the like.
Preferably, the temperature of the calcination in the step (2) is 1200-1270deg.C, and may be 1200-1210 deg.C, 1220 deg.C, 1230 deg.C, 1240 deg.C, 1250 deg.C, 1260 deg.C or 1270deg.C, for example.
Preferably, the roasting time in the step (2) is 0.5-2h, for example, 0.5h, 1h, 1.5h or 2h, etc.
As a preferable technical scheme of the invention, the preparation method specifically comprises the following steps:
(a) According to Sr 1-x La x Fe 12-y Al y O 19 Is of the formula (I)Ratio of Fe 2 O 3 、SrCO 3 、La 2 O 3 And Al 2 O 3 Wherein x is more than 0 and less than or equal to 0.3, y is more than 0 and less than or equal to 0.4, and then Fe is added 2 O 3 、SrCO 3 、La 2 O 3 、Al 2 O 3 Ball milling for 2-4h together with water, drying the ball milled product at 90-120 ℃, and crushing the dried product;
(b) Roasting the crushed product at 1200-1270 ℃ in air atmosphere to obtain the permanent magnetic strontium ferrite magnetic powder.
Optionally, the comminuting is performed using a pulverizer. The roasting is performed by adopting a box-type electric heating furnace.
In a third aspect, the present invention provides a permanent magnet made from the permanent magnet strontium ferrite magnetic powder of the first aspect.
In a fourth aspect, the present invention provides a method for preparing a permanent magnet according to the third aspect, the method comprising:
ball milling permanent magnetic strontium ferrite magnetic powder, and obtaining a green magnet after orientation shaping;
and (II) sintering the green magnet to obtain the permanent magnet.
Preferably, the ball milling in the step (I) is wet ball milling, and the reagents adopted by the wet ball milling comprise water and additives, wherein the mass ratio of the water to the permanent magnetic strontium ferrite magnetic powder is (1.2-1.8): 1, for example, 1.2:1, 1.3:1, 1.4:1, 1.5:1, 1.6:1, 1.7:1 or 1.8:1, etc.
The kind of the additive is not particularly limited, and examples thereof include organic dispersants, srCO 3 、CaCO 3 Or SiO 2 And the like, and the organic dispersant may be, for example, calcium gluconate, sorbitol, or the like.
Preferably, the ball ratio of the ball milling in the step (I) is 1 (12-16), and can be 1:12, 1:14 or 1:16, for example. Wherein the ball ratio is the mass ratio of the permanent magnetic strontium ferrite magnetic powder to the ball grinding balls.
Preferably, the ball milling time in the step (I) is 16-20h, for example, 16h, 17h, 18h, 19h or 20h, etc.
Preferably, in the step (I), the D50 particle size of the permanent magnetic strontium ferrite magnetic powder after ball milling is 0.4-2 μm, for example, 0.4 μm, 0.5 μm, 0.6 μm, 0.7 μm, 0.8 μm, 1 μm, 1.2 μm, 1.5 μm, 1.7 μm or 2 μm, preferably 0.6-0.96 μm.
Preferably, in step (i), after the ball milling, filtration sedimentation is performed, and then the filtration sedimentation product is subjected to orientation setting.
Preferably, the humidity of the filtered and settled product is 30-40%, for example 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39% or 40% etc.
Preferably, the orientation set of step (i) is a wet orientation set.
Preferably, the molding pressure of the orientation molding in the step (I) is 4-6Mpa, for example, 4Mpa, 5Mpa or 6Mpa, and the magnetic field strength of the orientation molding is 1.2-1.5T, for example, 1.2T, 1.3T, 1.4T or 1.5T, and the like.
Preferably, the sintering temperature in step (II) is 1180-1220 ℃, and may be 1180 ℃, 1185 ℃, 1190 ℃, 1195 ℃, 1200 ℃, 1205 ℃, 1210 ℃, 1215 ℃ or the like.
Preferably, the sintering time in step (II) is 0.5-1.5h, for example, 0.5h, 0.7h, 1h, 1.2h, 1.5h, etc.
The numerical ranges recited herein include not only the above-listed point values, but also any point values between the above-listed numerical ranges that are not listed, and are limited in space and for the sake of brevity, the present invention is not intended to be exhaustive of the specific point values that the stated ranges include.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a compound with the chemical formula of Sr 1-x La x Fe 12-y Al y O 19 The high-performance permanent magnetic strontium ferrite magnetic powder is co-doped by introducing La and Al with specific contents, and under the synergistic effect of the La and the Al, the intrinsic magnetic property of the magnetic powder can be improved, so that the residual magnetic powder of the magnetic powderThe magnetic property is reduced, the coercivity is improved, and a good foundation can be brought for the subsequent forming process. Meanwhile, the cost can be controlled by adopting La and Al for co-doping, so that the cost is lower. The permanent magnet prepared based on the method has higher Hcj and squareness, and is favorable for fully utilizing the performance of products.
Drawings
Fig. 1 is a flow chart of a process for preparing a permanent magnet prepared in example 1 of the present invention.
Fig. 2 is an XRD pattern of the permanent magnet powder provided in examples 1 to 4 of the present invention.
Fig. 3 is an XRD pattern of the permanent magnet powder provided in examples 5 to 8 of the present invention.
Fig. 4 is an XRD pattern of the permanent magnet powder provided in examples 9 to 12 of the present invention.
Fig. 5 is a graph showing Hcj changes of the permanent magnet provided in examples 1 to 12 and comparative example 1 of the present invention.
Fig. 6 is a graph showing the change in remanence Br of the permanent magnet provided in examples 1 to 12 and comparative example 1 of the present invention.
Fig. 7 is an SEM image of the permanent magnetic strontium ferrite magnetic powder prepared in examples 9 to 12 of the present invention.
Fig. 8 is an SEM image of the slurry obtained after the permanent magnetic strontium ferrite magnetic powder of examples 9-12 of the present invention was subjected to wet ball milling for 16 hours.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments.
Example 1
The embodiment provides a permanent magnetic strontium ferrite magnetic powder, the chemical formula of which is Sr 1- x La x Fe 12-y Al y O 19 ，x＝0.1，y＝0.1，x/y＝1；
Wherein the D50 particle size of the permanent magnetic strontium ferrite magnetic powder is 0.8-1.5 mu m.
The embodiment also provides a preparation method of the permanent magnetic strontium ferrite magnetic powder, which comprises the following steps:
(1) According to Sr 1-x La x Fe 12-y Al y O 19 Is converted intoStoichiometric arrangement of Fe 2 O 3 、SrCO 3 、La 2 O 3 And Al 2 O 3 (Fe 2 O 3 、SrCO 3 、La 2 O 3 And Al 2 O 3 97% purity) and then Fe 2 O 3 、SrCO 3 、La 2 O 3 、Al 2 O 3 Mixing the slurry with water by planetary ball milling for 2 hours, drying the ball milled product at 90 ℃ after the slurry is obtained, and crushing the dried product;
wherein water is mixed with raw materials (including Fe 2 O 3 、SrCO 3 、La 2 O 3 And Al 2 O 3 ) The mass ratio of (2) to (1);
(2) Roasting the crushed product at 1250 ℃ for 2 hours in an air atmosphere to obtain the permanent magnetic strontium ferrite magnetic powder.
The embodiment also provides a permanent magnet, which is prepared from the permanent magnet strontium ferrite magnetic powder, and the specific preparation method comprises the following steps:
300g of the permanent magnetic strontium ferrite magnetic powder, 0.5wt% of organic dispersant (namely calcium gluconate) and 0.5wt% of SrCO 3 、1.5wt％CaCO 3 、0.5wt％SiO 2 Mixing with 500g of water, performing wet ball milling for 16 hours to obtain slurry with the D50 particle size of 0.86 mu m, filtering and settling the slurry to ensure that the humidity of the slurry reaches 30%, and performing wet orientation setting on the filtered and settled product under the conditions of a magnetic field of 1.5T and a pressure of 6Mpa to prepare a green magnet with the diameter of 22mm and the height of 15 mm;
wherein the mass ratio of water to the permanent magnetic strontium ferrite magnetic powder is 1.67:1;
and (II) sintering the green magnet at 1200 ℃ for 0.5h to obtain the permanent magnet.
Fig. 1 shows a flow chart of a process for preparing a permanent magnet according to the present embodiment.
Examples 2 to 4
Examples 2 to 4 differ from example 1 in that examples 2 to 4 provide permanent magnet strontium ferrite magnetic powders having y of 0.2, 0.3 and 0.4, respectively.
The remaining preparation methods and parameters remain the same as in example 1.
Fig. 2 shows XRD patterns of the permanent magnet powder provided in examples 1 to 4, from which the phase purity ratios of the magnet powder when x=0.1, y=0.1, 0.2, 0.3 and 0.4 can be known.
Example 5
The embodiment provides a permanent magnetic strontium ferrite magnetic powder, the chemical formula of which is Sr 1- x La x Fe 12-y Al y O 19 ，x＝0.2，y＝0.1，x/y＝2；
Wherein the D50 particle size of the permanent magnetic strontium ferrite magnetic powder is 0.8-1.5 mu m.
The embodiment also provides a preparation method of the permanent magnetic strontium ferrite magnetic powder, which comprises the following steps:
(1) According to Sr 1-x La x Fe 12-y Al y O 19 Stoichiometric ratio of Fe 2 O 3 、SrCO 3 、La 2 O 3 And Al 2 O 3 (Fe 2 O 3 、SrCO 3 、La 2 O 3 And Al 2 O 3 97% purity) and then Fe 2 O 3 、SrCO 3 、La 2 O 3 、Al 2 O 3 Mixing the slurry with water by planetary ball milling for 2 hours, drying the ball milled product at 120 ℃ after the slurry is obtained, and crushing the dried product;
wherein water is mixed with raw materials (including Fe 2 O 3 、SrCO 3 、La 2 O 3 And Al 2 O 3 ) The mass ratio of (2) is 1.5:1;
(2) Roasting the crushed product at 1250 ℃ for 2 hours in an air atmosphere to obtain the permanent magnetic strontium ferrite magnetic powder.
The embodiment also provides a permanent magnet, which is prepared from the permanent magnet strontium ferrite magnetic powder, and the specific preparation method comprises the following steps:
300g of the permanent magnetic strontium ferrite magnetic powder,0.5wt% of organic dispersant (namely calcium gluconate) and 0.3wt% of SrCO 3 、1.5wt％CaCO 3 、0.5wt％SiO 2 Mixing with 500g of water, performing wet ball milling for 16 hours to obtain slurry with the D50 particle size of 0.90 mu m, filtering and settling the slurry to enable the humidity of the slurry to reach 40%, and performing wet orientation setting on the filtered and settled product under the conditions of a magnetic field of 1.5T and a pressure of 6Mpa to prepare a green magnet with the diameter of 22mm and the height of 15 mm;
wherein the mass ratio of water to the permanent magnetic strontium ferrite magnetic powder is 1.67:1;
and (II) sintering the green magnet at 1200 ℃ for 0.5h to obtain the permanent magnet.
Examples 6 to 8
Examples 6-8 differ from example 5 in that examples 6-8 provide permanent magnet strontium ferrite magnetic powders with y of 0.2, 0.3 and 0.4, respectively.
The remaining preparation methods and parameters remain the same as in example 5.
Fig. 3 shows XRD patterns of the permanent magnet powder provided in examples 5 to 8, from which it can be seen that when x=0.2, y=0.1, 0.2, 0.3 and 0.4 are phase purity ratios of the magnet powder.
Example 9
The embodiment provides a permanent magnetic strontium ferrite magnetic powder, the chemical formula of which is Sr 1- x La x Fe 12-y Al y O 19 ，x＝0.3，y＝0.1，x/y＝3；
Wherein the D50 particle size of the permanent magnetic strontium ferrite magnetic powder is 1.34 mu m.
The embodiment also provides a preparation method of the permanent magnetic strontium ferrite magnetic powder, which comprises the following steps:
(1) According to Sr 1-x La x Fe 12-y Al y O 19 Stoichiometric ratio of Fe 2 O 3 、SrCO 3 、La 2 O 3 And Al 2 O 3 (Fe 2 O 3 、SrCO 3 、La 2 O 3 And Al 2 O 3 Is 97% pure),then Fe is added 2 O 3 、SrCO 3 、La 2 O 3 、Al 2 O 3 Mixing the slurry with water by planetary ball milling for 2 hours, drying the ball milled product at 110 ℃ after the slurry is obtained, and crushing the dried product;
wherein water is mixed with raw materials (including Fe 2 O 3 、SrCO 3 、La 2 O 3 And Al 2 O 3 ) The mass ratio of (2) to (1);
(2) Roasting the crushed product at 1250 ℃ for 2 hours in an air atmosphere to obtain the permanent magnetic strontium ferrite magnetic powder.
The embodiment also provides a permanent magnet, which is prepared from the permanent magnet strontium ferrite magnetic powder, and the specific preparation method comprises the following steps:
300g of the permanent magnetic strontium ferrite magnetic powder, 0.5wt% of organic dispersant (namely calcium gluconate) and 1.5wt% of CaCO 3 、0.5wt％SiO 2 Mixing with 500g of water, performing wet ball milling for 16 hours to obtain slurry with the D50 particle size of 0.82 mu m, filtering and settling the slurry to ensure that the humidity of the slurry reaches 35%, and performing wet orientation setting on the filtered and settled product under the conditions of a magnetic field of 1.5T and a pressure of 6Mpa to prepare a green magnet with the diameter of 22mm and the height of 15 mm;
wherein the mass ratio of water to the permanent magnetic strontium ferrite magnetic powder is 1.67:1;
and (II) sintering the green magnet at 1200 ℃ for 0.5h to obtain the permanent magnet.
Examples 10 to 12
Examples 10 to 12 differ from example 9 in that examples 10 to 12 provide permanent magnet strontium ferrite magnetic powders having y of 0.2, 0.3 and 0.4, respectively.
The remaining preparation methods and parameters remain the same as in example 9.
Fig. 4 shows XRD patterns of the permanent magnet powder provided in examples 9 to 12, from which it can be seen that when x=0.3, y=0.1, 0.2, 0.3 and 0.4 are phase purity ratios of the magnetic powder.
Fig. 7 shows SEM images of the permanent magnetic strontium ferrite magnetic powder prepared in examples 9 to 12, and it can be seen from the figures that when x=0.3, y=0.1, 0.2, 0.3 and 0.4, the magnetic powder has a particle size morphology at a pre-sintering temperature of 1250 ℃.
Fig. 8 shows SEM images of the slurries obtained after wet ball milling of the permanent magnet strontium ferrite magnetic powder of examples 9-12 for 16 hours, and it can be seen from the figures that when x=0.3, y=0.1, 0.2, 0.3 and 0.4, the magnetic powder undergoes secondary ball milling for 16 hours.
Example 13
This example differs from example 1 in that the firing temperature in step (2) is 1100 ℃.
The remaining preparation methods and parameters remain the same as in example 1.
Example 14
This example differs from example 1 in that the firing temperature in step (2) is 1300 ℃.
The remaining preparation methods and parameters remain the same as in example 1.
Comparative example 1
The comparative example is different from example 1 in that the permanent magnet strontium ferrite magnetic powder provided in the comparative example does not contain La and Al, and x and y are both 0, i.e. La is not added in step (1) 2 O 3 And Al 2 O 3 。
The remaining preparation methods and parameters remain the same as in example 1.
Fig. 5 shows graphs of Hcj changes of the permanent magnet provided in examples 1 to 12 and comparative example 1, and it can be seen from the graphs that the trend of Hcj changes with changes in x and y.
Fig. 6 shows graphs of the change in remanence Br of the permanent magnet provided in examples 1 to 12 and comparative example 1, from which it can be seen that the degree of change in Br is changed with the change in x and y.
Comparative example 2
The comparative example is different from example 1 in that the permanent magnet strontium ferrite magnetic powder provided in the comparative example does not contain La and x is 0, i.e. La is not added in step (1) 2 O 3 。
The remaining preparation methods and parameters remain the same as in example 1.
Comparative example 3
The comparative example is different from example 1 in that the permanent magnet strontium ferrite magnetic powder provided in the comparative example does not contain Al, and y is 0, i.e., al is not added in step (1) 2 O 3 。
The remaining preparation methods and parameters remain the same as in example 1.
Comparative example 4
This comparative example differs from example 1 in that the permanent magnet strontium ferrite magnetic powder provided in this comparative example has x of 0.5.
The remaining preparation methods and parameters remain the same as in example 1.
Comparative example 5
This comparative example is different from example 1 in that the y in the permanent magnet strontium ferrite magnetic powder provided in this comparative example is 0.8.
The remaining preparation methods and parameters remain the same as in example 1.
Performance testing
The permanent magnet powder and the permanent magnet prepared in examples 1 to 14 and comparative examples 1 to 5 were tested.
Test conditions:
(1) Polishing two ends of a magnet to be flat, and taking the value of a second quadrant when the maximum field in a BH tester is 1.5T under the condition of room temperature to obtain the maximum magnetic energy product (BH) max;
the intercept of the y axis of the loop is remanence Br, the intercept of the x axis is intrinsic coercive force Hcj, wherein H k Hcj represents the rectangularity of the test sample.
(2) XRD testing is carried out on different magnetic powder to obtain phase purity.
The test results are shown in Table 1.
TABLE 1
Analysis:
as is clear from the data results of examples 1 to 4, the permanent magnet prepared by the invention has M phase purity of about 90%, when lanthanum is fixed and aluminum is gradually increased, the obtained sample has Br falling range of 7.1 to 11.8%, but Hcj is increased by 67.0 to 99.7%, and the intrinsic magnetic property of the magnetic powder is changed based on element doping, so that the residual magnetism is reduced and the coercive force is improved.
As is clear from the data of examples 5 to 8, the permanent magnet prepared by the invention has M phase purity of 95% or more, and when lanthanum is fixed and aluminum is gradually increased, the obtained sample has Br falling range of 2.3 to 14.1%, but Hcj is increased by 57.3 to 92.7%, and the intrinsic magnetic properties of the magnetic powder are changed based on element doping, so that the remanence is reduced and the coercive force is improved.
As can be seen from the data of examples 9-12, the permanent magnet prepared according to the present invention has M phase purity of 98% or more, and when lanthanum is fixed to gradually increase aluminum, the Hcj of the obtained sample increases up to 61.1%, and Br thereof increases up to 7.9%. It is known that there are many ways to raise coercivity of magnetic powder, while remanence is difficult to raise, and it mainly depends on intrinsic and technological parameters, and this has the same effect as La-Co series samples, but well controls cost, and the main reason is that Co-doping effect of lanthanum and aluminum changes intrinsic magnetic properties of magnetic powder, so as to cause magnet property change.
From the data of examples 1 and 13 to 14, it is understood that if the temperature of the firing in step (2) is too low, the magnet density and the phase purity are lowered, resulting in a decrease in magnetic properties; if the temperature of the firing in step (2) is too high, the magnet is overdriven, resulting in a decrease in magnetic properties.
From the data of example 1 and comparative example 1, it is evident that the co-doping without adding La and Al does not improve the magnet performance, and the coercive force is reduced.
From the data of example 1 and comparative examples 2 to 3, it is understood that doping with only La or Al causes the deterioration of magnetic properties due to the non-uniformity of particles and the increase of impurity phases.
As is clear from the data of example 1 and comparative example 4, when the doping ratio of La is too high, the phase temperature increases, and the coercive force decreases sharply.
As is clear from the data of example 1 and comparative example 5, if the doping ratio of Al is too high, the impurity phase ratio increases, and the magnetic properties decrease.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.
Claims (10)
1. The permanent magnetic strontium ferrite magnetic powder is characterized by comprising the following chemical formula: sr (Sr) 1- x La x Fe 12-y Al y O 19 Wherein x is more than 0 and less than or equal to 0.3, and y is more than 0 and less than or equal to 0.4.
2. A permanent magnet strontium ferrite magnetic powder as defined in claim 1, wherein the Sr 1-x La x Fe 12-y Al y O 19 Wherein x/y ranges from 0.25 to 3.0;
preferably, the D50 particle size of the permanent magnetic strontium ferrite magnetic powder is 0.56-2.14 mu m.
3. A method of producing the permanent magnetic strontium ferrite powder as defined in claim 1 or 2, comprising:
(1) According to Sr 1-x La x Fe 12-y Al y O 19 Wherein x is more than 0 and less than or equal to 0.3, and y is more than 0 and less than or equal to 0.4;
(2) And ball-milling the raw materials and roasting to obtain the permanent magnetic strontium ferrite magnetic powder.
4. A method of preparing permanent magnet strontium ferrite magnetic powder according to claim 3, wherein the raw materials comprise an iron source, a strontium source, a lanthanum source and an aluminum source;
preferably, the iron source comprises Fe 2 O 3 ；
Preferably, the strontium source comprises SrCO 3 ；
Preferably, the lanthanum source comprises La 2 O 3 ；
Preferably, the aluminum source comprises Al 2 O 3 ；
Preferably, the purity of the raw material is 97% or more.
5. The method for preparing permanent magnet strontium ferrite magnetic powder according to claim 3 or 4, wherein the ball milling in the step (2) is wet ball milling, the reagent used for the wet ball milling comprises water, and the mass ratio of the water to the raw materials is (1.5-2): 1;
preferably, the ball milling in step (2) is carried out for a period of time ranging from 2 to 4 hours, preferably from 2 to 3 hours;
preferably, in the step (2), between the ball milling and the roasting, the steps of drying and crushing are sequentially carried out, and the drying temperature is 90-120 ℃;
preferably, the roasting temperature in the step (2) is 1200-1270 ℃;
preferably, the roasting time in the step (2) is 0.5-2h.
6. A method for preparing permanent magnet strontium ferrite magnetic powder according to any of claims 3-5, wherein the preparation method specifically comprises:
(a) According to Sr 1-x La x Fe 12-y Al y O 19 Stoichiometric ratio of Fe 2 O 3 、SrCO 3 、La 2 O 3 And Al 2 O 3 Wherein x is more than 0 and less than or equal to 0.3, y is more than 0 and less than or equal to 0.4, and then Fe is added 2 O 3 、SrCO 3 、La 2 O 3 、Al 2 O 3 Ball milling for 2-4h together with water, drying the ball milled product at 90-120 ℃, and crushing the dried product;
(b) Roasting the crushed product at 1200-1270 ℃ in air atmosphere to obtain the permanent magnetic strontium ferrite magnetic powder.
7. A permanent magnet, characterized in that it is produced from the permanent-magnet strontium ferrite magnetic powder as claimed in claim 1 or 2.
8. A method of producing a permanent magnet according to claim 7, comprising:
ball milling permanent magnetic strontium ferrite magnetic powder, and obtaining a green magnet after orientation shaping;
and (II) sintering the green magnet to obtain the permanent magnet.
9. The method for preparing a permanent magnet according to claim 8, wherein the ball milling in the step (i) is wet ball milling, the reagents used in the wet ball milling comprise water and additives, and the mass ratio of the water to the permanent magnet strontium ferrite magnetic powder is (1.2-1.8): 1;
preferably, the ball milling time in the step (I) is 16-20 hours;
preferably, in the step (I), the D50 particle size of the permanent magnetic strontium ferrite magnetic powder after ball milling is 0.4-2 mu m, preferably 0.6-0.96 mu m;
preferably, in the step (I), after the ball milling, filtration sedimentation is carried out, and then orientation setting is carried out on the product of filtration sedimentation;
preferably, the humidity of the filtered and settled product is 30-40%;
preferably, the orientation setting in step (i) is a wet orientation setting;
preferably, the forming pressure of the orientation shaping in the step (I) is 4-6Mpa, and the magnetic field strength of the orientation shaping is 1.2-1.5T.
10. The method of producing a permanent magnet according to claim 8 or 9, wherein the sintering temperature in step (ii) is 1180 to 1220 ℃;
preferably, the sintering time in step (II) is 0.5-1.5h.
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