CN117727549A - Preparation method of high-performance nanocrystalline composite magnetic powder - Google Patents
Preparation method of high-performance nanocrystalline composite magnetic powder Download PDFInfo
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- CN117727549A CN117727549A CN202410044022.1A CN202410044022A CN117727549A CN 117727549 A CN117727549 A CN 117727549A CN 202410044022 A CN202410044022 A CN 202410044022A CN 117727549 A CN117727549 A CN 117727549A
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- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 239000006247 magnetic powder Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 27
- 238000005121 nitriding Methods 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000010791 quenching Methods 0.000 claims abstract description 17
- 230000000171 quenching effect Effects 0.000 claims abstract description 17
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 8
- 239000000956 alloy Substances 0.000 claims description 26
- 229910045601 alloy Inorganic materials 0.000 claims description 26
- 239000000843 powder Substances 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000000696 magnetic material Substances 0.000 abstract description 3
- 239000000155 melt Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 5
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 3
- 229910001172 neodymium magnet Inorganic materials 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
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Abstract
The invention discloses a preparation method of high-performance nanocrystalline composite magnetic powder, and belongs to the technical field of magnetic materials. The preparation method comprises the following steps: the method prepares Sm with nominal components respectively by a melt rapid quenching method 2 Fe 17 And Nd 1 Fe 12 Is then quenched in N 2 High energy ball milling in gas shielded process, followed byAnd mixing according to a certain proportion, and performing primary and secondary nitriding aging treatment under the assistance of a low magnetic field to finally obtain the high-performance SmFeN/NdFeN nanocrystalline composite magnetic powder. The invention has simple process and easy operation, and is beneficial to the application of the high-performance composite magnetic powder in more permanent magnetic 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 high-performance nanocrystalline composite magnetic powder.
Background
The rare earth permanent magnetic material is an alloy formed by rare earth Nd, sm, pr and other elements and some transition metal elements, and is prepared by a specific process to form a special material with permanent magnetic performance, and is widely applied to motors, generators, nuclear magnetic resonance imagers, microwave communication technologies, meters and other devices and equipment needing permanent magnetic fields. Meanwhile, since the advent of SmFeN permanent magnet materials, people attach importance to the excellent magnetic performance and good temperature stability, and the SmFeN permanent magnet materials are the only permanent magnet which can surpass NdFeB in performance, and become one of research hot spots of rare earth permanent magnet materials at home and abroad. Further, recent studies have revealed that NdFe having a 1:12 type crystal structure 12 The N permanent magnet has lower requirement on the addition amount of rare earth elements than the Nd-Fe-B permanent magnet, and has higher Curie temperature, thus being expected to become a new generation permanent magnet material.
Therefore, the melt rapid quenching method of the invention respectively prepares Sm with nominal composition 2 Fe 17 And Nd 1 Fe 12 Is then quenched in N 2 And (3) performing high-energy ball milling in gas protection, mixing according to a certain proportion, and performing primary and secondary nitriding aging treatment under the assistance of a low magnetic field to obtain the high-performance SmFeN/NdFeN nanocrystalline composite magnetic powder.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a preparation method of high-performance nanocrystalline composite magnetic powder.
The preparation method of the high-performance nanocrystalline composite magnetic powder comprises the following steps:
(1) Preparing Sm with nominal components by melt rapid quenching method 2 Fe 17 And Nd 1 Fe 12 The rotating speed of the copper roller is 20-40 m/s;
(2) Sm obtained in the step (1) 2 Fe 17 And Nd 1 Fe 12 The alloy rapid quenching belts of (2) are respectively in N 2 Performing high-energy ball milling in gas protection for 5-10 h to obtain Sm with average particle size less than 200 nm 2 Fe 17 Alloy powderNd 1 Fe 12 Alloy powder;
(3) Sm obtained in the step (2) 2 Fe 17 Alloy powder and Nd 1 Fe 12 Mixing alloy powder according to the mass ratio of 1:0.1-1, and adding the mixture into N 2 And performing primary and secondary nitriding aging treatment under the assistance of a low magnetic field in the gas protection to obtain the high-performance SmFeN/NdFeN nanocrystalline composite magnetic powder.
Further, the temperature of the primary nitriding aging treatment and the secondary nitriding aging treatment under the assistance of the low magnetic field in the step (3) is 600-800 ℃, the heating rate is 1-5 ℃/min, the heat preservation time is 3-9 h, the magnetic field strength is 1000-3000 Oe, and then the primary nitriding aging treatment is quenched to room temperature; the temperature of the secondary nitriding aging treatment is 300-500 ℃, the heating rate is 1-5 ℃/min, the heat preservation time is 1-6 h, the magnetic field strength is 1000-3000 Oe, and then the secondary nitriding aging treatment is quenched to room temperature.
Compared with the prior art, the invention has the following advantages and beneficial effects: the method prepares Sm with nominal components respectively by a melt rapid quenching method 2 Fe 17 And Nd 1 Fe 12 Is then quenched in N 2 And (3) performing high-energy ball milling in gas protection, mixing according to a certain proportion, and performing primary and secondary nitriding aging treatment under the assistance of a low magnetic field to obtain the high-performance SmFeN/NdFeN nanocrystalline composite magnetic powder. The invention has simple process and easy operation, and is beneficial to the application of the high-performance composite magnetic powder in more permanent magnetic devices so as to meet the market demand.
Description of the embodiments
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) Preparing Sm with nominal components by melt rapid quenching method 2 Fe 17 And Nd 1 Fe 12 The rotation speed of the copper roller is respectively 20 m/s and 40 m/s;
(2) Sm obtained in the step (1) 2 Fe 17 And Nd 1 Fe 12 The alloy rapid quenching belts of (2) are respectively in N 2 Performing high-energy ball milling in gas protection for 5 h and 10 h respectively to obtain Sm with average particle diameter less than 200 nm 2 Fe 17 Alloy powder and Nd 1 Fe 12 Alloy powder;
(3) Sm obtained in the step (2) 2 Fe 17 Alloy powder and Nd 1 Fe 12 Mixing alloy powder according to the mass ratio of 1:0.3, and adding the mixture into N 2 Performing primary and secondary nitriding aging treatment under the assistance of a low magnetic field in gas protection, wherein the temperature of the primary nitriding aging treatment under the assistance of the low magnetic field is 600 ℃, the heating rate is 1 ℃/min, the heat preservation time is 3 h, the magnetic field strength is 1000 Oe, and then quenching to room temperature; the temperature of the secondary nitriding aging treatment is 500 ℃, the heating rate is 5 ℃/min, the heat preservation time is 6 h, the magnetic field strength is 3000 Oe, and then the secondary nitriding aging treatment is quenched to room temperature, so that the high-performance SmFeN/NdFeN nanocrystalline composite magnetic powder is obtained.
The high-performance nanocrystalline composite magnetic powder prepared by the method has the coercivity of 12.2 kOe, the remanence of 0.95T and the magnetic energy product of 10.2 MGOe through magnetic property test.
Example 2
(1) Preparing Sm with nominal components by melt rapid quenching method 2 Fe 17 And Nd 1 Fe 12 The rotation speed of the copper roller is 35 m/s and 30 m/s respectively;
(2) Sm obtained in the step (1) 2 Fe 17 And Nd 1 Fe 12 The alloy rapid quenching belts of (2) are respectively in N 2 Performing high-energy ball milling in gas protection for 8 h and 7 h respectively to obtain Sm with average particle diameter less than 200 nm 2 Fe 17 Alloy powder and Nd 1 Fe 12 Alloy powder;
(3) Sm obtained in the step (2) 2 Fe 17 Alloy powder and Nd 1 Fe 12 Mixing alloy powder according to the mass ratio of 1:0.7, and adding the mixture into N 2 Performing primary and secondary nitriding aging treatment under the assistance of a low magnetic field in gas protection, wherein the temperature of the primary nitriding aging treatment under the assistance of the low magnetic field is 700 ℃, the heating rate is 3 ℃/min, the heat preservation time is 6 h, and the magnetic field is the same as that of the primary nitriding aging treatment under the assistance of the low magnetic fieldStrength 2000 Oe, followed by quenching to room temperature; the temperature of the secondary nitriding aging treatment is 400 ℃, the heating rate is 3 ℃/min, the heat preservation time is 3 h, the magnetic field strength is 2000 Oe, and then the secondary nitriding aging treatment is quenched to room temperature, so that the high-performance SmFeN/NdFeN nanocrystalline composite magnetic powder is obtained.
The high-performance nanocrystalline composite magnetic powder prepared by the method has the coercivity of 13.9 kOe, the remanence of 1.02T and the magnetic energy product of 11.8 MGOe through magnetic property test.
Example 3
(1) Preparing Sm with nominal components by melt rapid quenching method 2 Fe 17 And Nd 1 Fe 12 The rotation speed of the copper roller is respectively 40 m/s and 20 m/s;
(2) Sm obtained in the step (1) 2 Fe 17 And Nd 1 Fe 12 The alloy rapid quenching belts of (2) are respectively in N 2 Performing high-energy ball milling in gas protection for 10 h and 5 h respectively to obtain Sm with average particle diameter less than 200 nm 2 Fe 17 Alloy powder and Nd 1 Fe 12 Alloy powder;
(3) Sm obtained in the step (2) 2 Fe 17 Alloy powder and Nd 1 Fe 12 Mixing alloy powder according to the mass ratio of 1:1, and adding the mixture into N 2 Performing primary and secondary nitriding aging treatment under the assistance of a low magnetic field in gas protection, wherein the temperature of the primary nitriding aging treatment under the assistance of the low magnetic field is 800 ℃, the heating rate is 5 ℃/min, the heat preservation time is 9 h, the magnetic field strength is 3000 Oe, and then quenching to room temperature; the temperature of the secondary nitriding aging treatment is 300 ℃, the heating rate is 1 ℃/min, the heat preservation time is 1 h, the magnetic field strength is 1000 Oe, and then the secondary nitriding aging treatment is quenched to room temperature, so that the high-performance SmFeN/NdFeN nanocrystalline composite magnetic powder is obtained.
The high-performance nanocrystalline composite magnetic powder prepared by the method has the coercivity of 14.5 kOe, the remanence of 1.09T and the magnetic energy product of 12.7 MGOe through magnetic property test.
Claims (2)
1. The preparation method of the high-performance nanocrystalline composite magnetic powder is characterized by comprising the following steps:
(1) Preparing Sm with nominal components by melt rapid quenching method 2 Fe 17 And Nd 1 Fe 12 The rotating speed of the copper roller is 20-40 m/s;
(2) Sm obtained in the step (1) 2 Fe 17 And Nd 1 Fe 12 The alloy rapid quenching belts of (2) are respectively in N 2 Performing high-energy ball milling in gas protection for 5-10 h to obtain Sm with average particle size less than 200 nm 2 Fe 17 Alloy powder and Nd 1 Fe 12 Alloy powder;
(3) Sm obtained in the step (2) 2 Fe 17 Alloy powder and Nd 1 Fe 12 Mixing alloy powder according to the mass ratio of 1:0.1-1, and adding the mixture into N 2 And performing primary and secondary nitriding aging treatment under the assistance of a low magnetic field in the gas protection to obtain the high-performance SmFeN/NdFeN nanocrystalline composite magnetic powder.
2. The method for preparing high-performance nanocrystalline composite magnetic powder according to claim 1, wherein: the temperature of the primary nitriding aging treatment and the secondary nitriding aging treatment under the assistance of the low magnetic field in the step (3) is 600-800 ℃, the heating rate is 1-5 ℃/min, the heat preservation time is 3-9 h, the magnetic field strength is 1000-3000 Oe, and then quenching is carried out to room temperature; the temperature of the secondary nitriding aging treatment is 300-500 ℃, the heating rate is 1-5 ℃/min, the heat preservation time is 1-6 h, the magnetic field strength is 1000-3000 Oe, and then the secondary nitriding aging treatment is quenched to room temperature.
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