CN118197785A - Preparation method of fully dense anisotropic composite magnet - Google Patents
Preparation method of fully dense anisotropic composite magnet Download PDFInfo
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- CN118197785A CN118197785A CN202410370393.9A CN202410370393A CN118197785A CN 118197785 A CN118197785 A CN 118197785A CN 202410370393 A CN202410370393 A CN 202410370393A CN 118197785 A CN118197785 A CN 118197785A
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- anisotropic composite
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- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 59
- 239000000956 alloy Substances 0.000 claims abstract description 59
- 238000010438 heat treatment Methods 0.000 claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 18
- 238000000137 annealing Methods 0.000 claims abstract description 16
- 238000005324 grain boundary diffusion Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000010791 quenching Methods 0.000 claims abstract description 11
- 230000000171 quenching effect Effects 0.000 claims abstract description 11
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 10
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000155 melt Substances 0.000 claims abstract description 5
- 239000010949 copper Substances 0.000 claims description 31
- 238000004321 preservation Methods 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 230000006698 induction Effects 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000000696 magnetic material Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 3
- 229910000905 alloy phase Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- H01F41/0273—Imparting anisotropy
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a preparation method of a fully dense anisotropic composite magnet, and belongs to the technical field of magnetic materials. The preparation method comprises the following steps: the method comprises the steps of respectively preparing Sm (Fe, TM) 12 and Sm (Fe, TM) 7 alloy thin strips by a melt rapid quenching method, preparing low-melting-point Dy 20Tb30Cu25Co25 alloy powder by a high-energy ball milling technology, mixing Sm (Fe, TM) 12 alloy, sm (Fe, TM) 7 alloy and Dy 20Tb30Cu25Co25 alloy powder according to a proportion, performing spark plasma sintering, performing primary grain boundary diffusion heat treatment under a subsequent magnetic field, and performing secondary annealing heat treatment, and finally obtaining the fully compact anisotropic composite magnet. The invention has simple process and easy operation, and is beneficial to the application of the high-performance anisotropic composite magnet in more permanent magnet devices so as to meet the market demand.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a preparation method of a fully dense anisotropic composite magnet.
Background
As an important functional material, magnetic materials play an extremely important role in modern society. In particular, the production and development application degree of the permanent magnet material is one of the marks of economic development of modern countries. The SmFe 12 alloy is found in the 1980 s, and because the ThMn 12 type alloy phase is a metastable phase, the intrinsic magnetic parameters of the alloy phase are not measured, and meanwhile, the impact of the RE 2Fe14 B permanent magnet material is not paid enough attention, so that the SmFe 12 alloy also greatly delays the practical process. Meanwhile, smCo 7 type alloys have high magnetocrystalline anisotropy field, high Curie temperature and high temperature stability and are attracting attention. However, due to unstable structure of SmCo 7, it is difficult to prepare single-phase alloy, and the process of rapid quenching of melt, isothermal tempering, chemical auxiliary high-energy ball milling, ultra-high pressure thermal deformation and the like is generally adopted to make crystal grains nano and obtain certain magnetic anisotropy.
The invention adopts a melt rapid quenching method to prepare Sm (Fe, TM) 12 and Sm (Fe, TM) 7 alloy thin strips respectively, prepares low-melting-point Dy 20Tb30Cu25Co25 alloy powder by a high-energy ball milling technology, and then mixes Sm (Fe, TM) 12 alloy, sm (Fe, TM) 7 alloy and Dy 20Tb30Cu25Co25 alloy powder according to a proportion, and then carries out spark plasma sintering, and a first-stage grain boundary diffusion heat treatment and a second-stage annealing heat treatment under a subsequent magnetic field to finally obtain the full-compact anisotropic composite magnet.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a preparation method of a fully dense anisotropic composite magnet.
The preparation method of the fully dense anisotropic composite magnet comprises the following steps:
(1) Preparing alloy thin strips with nominal components of Sm (Fe, TM) 12 and Sm (Fe, TM) 7 respectively by adopting a melt rapid quenching method, wherein the rotating speed of a copper roller is 10-30 m/s, and the TM is one or more of Ti, zr, si, co;
(2) Preparing a Dy 20Tb30Cu25Co25 alloy cast ingot with a low melting point according to atomic percent by adopting a high vacuum induction melting technology, crushing the Dy 20Tb30Cu25Co25 alloy cast ingot to Dy 20Tb30Cu25Co25 alloy powder with an average granularity of 3-9 mu m by adopting a high-energy ball milling technology, wherein the ball milling time is 1-6 hours;
(3) Mixing the Sm (Fe, TM) 12 and Sm (Fe, TM) 7 alloy thin strips obtained in the step (1) with Dy 20Tb30Cu25Co25 alloy powder obtained in the step (2) according to a certain mass ratio, and then placing the mixture into a hard alloy die for spark plasma sintering to obtain a fully compact block-shaped composite magnet;
(4) And (3) performing primary grain boundary diffusion heat treatment and secondary annealing heat treatment on the block-shaped composite magnet obtained in the step (3) under a magnetic field to finally obtain the full-compact anisotropic composite magnet.
Further, the mass ratio of the Sm (Fe, TM) 12 alloy thin strip, the Sm (Fe, TM) 7 alloy thin strip and Dy 20Tb30Cu25Co25 alloy powder in the step (3) is 1: 0.5-1: 0.01 to 0.03; the specific technological parameters of the spark plasma sintering are as follows: the sintering temperature is 650-900 ℃, the pressure is 400-600 MPa, and the sintering heat preservation time is 10-30 min.
Further, the temperature of the primary grain boundary diffusion heat treatment under the magnetic field in the step (4) is 800-950 ℃, the temperature rising rate is 1-5 ℃/min, the heat preservation time is 5-10 h, the magnetic field strength is 2-3T, and then the primary grain boundary diffusion heat treatment is quenched to room temperature; the temperature of the secondary annealing heat treatment under the magnetic field is 400-600 ℃, the heating rate is 1-5 ℃/min, the heat preservation time is 1-3 h, the magnetic field strength is 0.5-1T, and then the secondary annealing heat treatment is quenched to the room temperature.
Compared with the prior art, the invention has the following advantages and beneficial effects: the invention adopts a melt rapid quenching method to prepare Sm (Fe, TM) 12 and Sm (Fe, TM) 7 alloy thin strips respectively, prepares low-melting-point Dy 20Tb30Cu25Co25 alloy powder by a high-energy ball milling technology, then mixes Sm (Fe, TM) 12 alloy, sm (Fe, TM) 7 alloy and Dy 20Tb30Cu25Co25 alloy powder according to a proportion, and then carries out spark plasma sintering, and then carries out primary grain boundary diffusion heat treatment and secondary annealing heat treatment under a magnetic field to finally obtain the fully compact anisotropic composite magnet. The invention has simple process and easy operation, and is beneficial to the application of the high-performance anisotropic composite magnet in more permanent magnet devices so as to meet the market demand.
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited to the following examples.
Example 1
(1) The nominal components Sm (Fe 0.8Ti0.2)12 and Sm (alloy thin strip of Fe 0.7Zr0.3)7, copper roller rotating speed is 10 m/s;
(2) Preparing a Dy 20Tb30Cu25Co25 alloy cast ingot with a low melting point according to atomic percent by adopting a high vacuum induction melting technology, and crushing the Dy 20Tb30Cu25Co25 alloy cast ingot into Dy 20Tb30Cu25Co25 alloy powder with an average granularity of 9 mu m by adopting a high-energy ball milling technology, wherein the ball milling time is 2 h;
(3) Mixing the Sm (Fe 0.8Ti0.2)12 and Sm (Fe 0.7Zr0.3)7 alloy thin strip and Dy 20Tb30Cu25Co25 alloy powder obtained in the step (2) according to the mass ratio of 1:0.5:0.01), placing the mixture into a hard alloy die for spark plasma sintering at the sintering temperature of 650 ℃, the pressure of 400 MPa and the sintering heat preservation time of 10min to obtain a fully compact block-shaped composite magnet;
(4) Carrying out primary grain boundary diffusion heat treatment and secondary annealing heat treatment on the block-shaped composite magnet obtained in the step (3) under a magnetic field, wherein the temperature of the primary grain boundary diffusion heat treatment under the magnetic field is 800 ℃, the heating rate is 5 ℃/min, the heat preservation time is 10h, the magnetic field strength is 2T, and then quenching to room temperature; the temperature of the secondary annealing heat treatment under the magnetic field is 600 ℃, the heating rate is 1 ℃/min, the heat preservation time is 1h, the magnetic field strength is 1T, and then the secondary annealing heat treatment is quenched to room temperature, so that the full-compact anisotropic composite magnet is finally obtained.
The magnetic property test shows that the coercive force of the fully dense anisotropic composite magnet prepared by the invention is 15.3 kOe, and the magnetic energy product is 21.5 MGOe.
Example 2
(1) The nominal components Sm (Fe 0.9Zr0.1)12 and Sm (alloy thin strip of Fe 0.8Si0.2)7, copper roller rotating speed is 20 m/s;
(2) Preparing a Dy 20Tb30Cu25Co25 alloy cast ingot with a low melting point according to atomic percent by adopting a high vacuum induction melting technology, and crushing the Dy 20Tb30Cu25Co25 alloy cast ingot into Dy 20Tb30Cu25Co25 alloy powder with an average granularity of 6 mu m by adopting a high-energy ball milling technology, wherein the ball milling time is 4 h;
(3) Mixing Sm (Fe 0.9Zr0.1)12 and Sm (Fe 0.8Si0.2)7 alloy thin strip and Dy 20Tb30Cu25Co25 alloy powder obtained in the step (2) according to the mass ratio of 1:0.8:0.02), placing the mixture into a hard alloy die, and performing spark plasma sintering at 750 ℃ under the pressure of 500 MPa for 20min to obtain a fully compact block-shaped composite magnet;
(4) Carrying out primary grain boundary diffusion heat treatment and secondary annealing heat treatment on the block-shaped composite magnet obtained in the step (3) under a magnetic field, wherein the temperature of the primary grain boundary diffusion heat treatment under the magnetic field is 870 ℃, the heating rate is 3 ℃/min, the heat preservation time is 8 h, the magnetic field strength is 2T, and then quenching to room temperature; the temperature of the secondary annealing heat treatment under the magnetic field is 500 ℃, the heating rate is 3 ℃/min, the heat preservation time is 2 h, the magnetic field strength is 0.5T, and then the fully compact anisotropic composite magnet is obtained after quenching to room temperature.
The magnetic property test shows that the coercive force of the fully dense anisotropic composite magnet prepared by the invention is 17.1 kOe, and the magnetic energy product is 23.2 MGOe.
Example 3
(1) The nominal components Sm (Fe 0.7Si0.3)12 and Sm (alloy thin strip of Fe 0.9Co0.1)7, copper roller rotating speed is 30 m/s;
(2) Preparing a Dy 20Tb30Cu25Co25 alloy cast ingot with a low melting point according to atomic percent by adopting a high vacuum induction melting technology, and crushing the Dy 20Tb30Cu25Co25 alloy cast ingot into Dy 20Tb30Cu25Co25 alloy powder with an average granularity of 3 mu m by adopting a high-energy ball milling technology, wherein the ball milling time is 6 h;
(3) Mixing Sm (Fe 0.7Si0.3)12 and Sm (Fe 0.9Co0.1)7 alloy thin strip and Dy 20Tb30Cu25Co25 alloy powder obtained in the step (2) according to the mass ratio of 1:1:0.03), placing the mixture into a hard alloy die, and performing spark plasma sintering at 900 ℃ under the conditions of pressure of 600 MPa and sintering heat preservation time of 30min to obtain a fully compact block-shaped composite magnet;
(4) Carrying out primary grain boundary diffusion heat treatment and secondary annealing heat treatment on the block-shaped composite magnet obtained in the step (3) under a magnetic field, wherein the temperature of the primary grain boundary diffusion heat treatment under the magnetic field is 950 ℃, the heating rate is 1 ℃/min, the heat preservation time is 5h, the magnetic field strength is 3T, and then quenching to room temperature; the temperature of the secondary annealing heat treatment under the magnetic field is 400 ℃, the heating rate is 5 ℃/min, the heat preservation time is 3h, the magnetic field strength is 0.5T, and then the fully compact anisotropic composite magnet is obtained after quenching to room temperature.
The magnetic property test shows that the coercive force of the fully dense anisotropic composite magnet prepared by the invention is 18.5 kOe, and the magnetic energy product is 25.1 MGOe.
Claims (3)
1. The preparation method of the fully dense anisotropic composite magnet is characterized by comprising the following steps of:
(1) Preparing alloy thin strips with nominal components of Sm (Fe, TM) 12 and Sm (Fe, TM) 7 respectively by adopting a melt rapid quenching method, wherein the rotating speed of a copper roller is 10-30 m/s, and the TM is one or more of Ti, zr, si, co;
(2) Preparing a Dy 20Tb30Cu25Co25 alloy cast ingot with a low melting point according to atomic percent by adopting a high vacuum induction melting technology, crushing the Dy 20Tb30Cu25Co25 alloy cast ingot to Dy 20Tb30Cu25Co25 alloy powder with an average granularity of 3-9 mu m by adopting a high-energy ball milling technology, wherein the ball milling time is 1-6 hours;
(3) Mixing the Sm (Fe, TM) 12 and Sm (Fe, TM) 7 alloy thin strips obtained in the step (1) with Dy 20Tb30Cu25Co25 alloy powder obtained in the step (2) according to a certain mass ratio, and then placing the mixture into a hard alloy die for spark plasma sintering to obtain a fully compact block-shaped composite magnet;
(4) And (3) performing primary grain boundary diffusion heat treatment and secondary annealing heat treatment on the block-shaped composite magnet obtained in the step (3) under a magnetic field to finally obtain the full-compact anisotropic composite magnet.
2. The method for preparing the fully dense anisotropic composite magnet according to claim 1, wherein the method comprises the following steps: the mass ratio of the Sm (Fe, TM) 12 alloy thin strip, the Sm (Fe, TM) 7 alloy thin strip and Dy 20Tb30Cu25Co25 alloy powder in the step (3) is 1: 0.5-1: 0.01 to 0.03; the specific technological parameters of the spark plasma sintering are as follows: the sintering temperature is 650-900 ℃, the pressure is 400-600 MPa, and the sintering heat preservation time is 10-30 min.
3. The method for preparing the fully dense anisotropic composite magnet according to claim 1, wherein the method comprises the following steps: the temperature of the primary grain boundary diffusion heat treatment under the magnetic field in the step (4) is 800-950 ℃, the heating rate is 1-5 ℃/min, the heat preservation time is 5-10 h, the magnetic field strength is 2-3T, and then the primary grain boundary diffusion heat treatment is quenched to room temperature; the temperature of the secondary annealing heat treatment under the magnetic field is 400-600 ℃, the heating rate is 1-5 ℃/min, the heat preservation time is 1-3 h, the magnetic field strength is 0.5-1T, and then the secondary annealing heat treatment is quenched to the room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410370393.9A CN118197785A (en) | 2024-03-29 | 2024-03-29 | Preparation method of fully dense anisotropic composite magnet |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202410370393.9A CN118197785A (en) | 2024-03-29 | 2024-03-29 | Preparation method of fully dense anisotropic composite magnet |
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| CN118197785A true CN118197785A (en) | 2024-06-14 |
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| CN202410370393.9A Pending CN118197785A (en) | 2024-03-29 | 2024-03-29 | Preparation method of fully dense anisotropic composite magnet |
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