CN113421764A - Preparation method of permanent magnet with high toughness and high coercivity - Google Patents
Preparation method of permanent magnet with high toughness and high coercivity Download PDFInfo
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- CN113421764A CN113421764A CN202110748910.8A CN202110748910A CN113421764A CN 113421764 A CN113421764 A CN 113421764A CN 202110748910 A CN202110748910 A CN 202110748910A CN 113421764 A CN113421764 A CN 113421764A
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- 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
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- 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
- H01F41/026—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 protecting methods against environmental influences, e.g. oxygen, by surface treatment
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- 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
- H01F41/0293—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 diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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- Engineering & Computer Science (AREA)
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- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The invention discloses a preparation method of a permanent magnet with high toughness and high coercivity, and belongs to the technical field of magnetic materials. The preparation method comprises the following steps: preparing a Fe-Co-Ni-based high-entropy alloy cast ingot by adopting electric arc melting, and then adding a certain amount of nickel-based hard alloy particles with the mark GH4037 into the high-entropy alloy cast ingot in an atomization process to obtain mixed powder; the mixed powder is accelerated by using high-speed argon gas flow, then the surface layer of the samarium cobalt magnet is impacted, a microcrack region appears on the surface of the samarium cobalt magnet, meanwhile, the mixed powder is effectively filled in the microcrack region, and then, first-stage and second-stage tempering heat treatment under the protection of argon is carried out, so that the samarium cobalt permanent magnet with high toughness and high coercivity is obtained. The method has simple process and easy operation, and is beneficial to the application of the high-toughness samarium-cobalt 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 permanent magnet with high toughness and high coercivity.
Background
In recent years, with the gradual improvement of the magnetic performance of samarium cobalt permanent magnetic materials, especially the rapid improvement of the coercive force (H cj>1600 kA/m), new growth points required are continuously emerging, such as high-tech aspects of hybrid electric vehicles, wind power generation, national defense and military industry and the like, and the application of the high-coercivity samarium-cobalt rare earth permanent magnet material and the engine device is the guarantee of the propulsion power of the airship and the normal operation of a lifesaving system on the seven-China airship for realizing the great dream of Chinese space walking. However, in the practical application process, the defects of the samarium cobalt permanent magnet material are obvious, such as poor plasticity and toughness, difficult machining, shock and vibration resistance and the likeFurther expansion of the application range is severely restricted. The high-entropy alloy has a plurality of composition elements, so that various unique effects such as a high-entropy effect, a lattice distortion effect, a delayed diffusion effect, a cocktail effect and the like are endowed to the high-entropy alloy, and meanwhile, the mechanical properties of the high-entropy alloy are most extensively and deeply researched at present. High entropy alloys tend to have very high strength and hardness due to the solid solution strengthening effect and strong lattice distortion effect of the atoms within the alloy.
Therefore, the high-entropy alloy with better toughness and soft magnetic property is added, and the interior of the high-entropy alloy has lattice distortion, so that the pinning effect can be achieved, and the toughness and the mechanical property of the magnet are improved. Meanwhile, the atomized mixed powder of the high-entropy alloy and the nickel-based hard alloy impacts the surface of the samarium-cobalt magnet, so that a microcrack region appears on the surface of the samarium-cobalt magnet, the microcrack region is effectively filled with the mixed powder, the contact area between a diffusion object and the magnet is further increased, the diffusion efficiency is improved, and the samarium-cobalt permanent magnet with high toughness and high coercivity is obtained through primary and secondary tempering heat treatment under the protection of argon.
Disclosure of Invention
In view of the problems in the prior art, the present invention aims to provide a method for preparing a permanent magnet with high toughness and high coercivity.
The preparation method of the permanent magnet with high toughness and high coercivity comprises the following steps:
(1) preparing Fe-Co-Ni-based high-entropy alloy cast ingots by adopting electric arc melting;
(2) carrying out atomization treatment on the Fe-Co-Ni-based high-entropy alloy cast ingot obtained in the step (1) in vacuum, adding a certain amount of nickel-based hard alloy particles with the mark of GH4037 in the atomization process, wherein the average particle size of the nickel-based hard alloy is 20-500 mu m, and the mass ratio of the nickel-based hard alloy to the high-entropy alloy cast ingot is 0.01-0.1: 1, atomizing at 900-1600 ℃, for 3-10 h and under 5-20 MPa to obtain mixed powder;
(3) and (3) removing an oxide film on the surface of the samarium cobalt magnet, firstly accelerating the mixed powder obtained in the step (2) by using high-speed argon gas flow, then impacting the surface layer of the samarium cobalt magnet, wherein the impacting time of the high-speed gas flow is 15-45 min, so that a microcrack region appears on the surface of the samarium cobalt magnet, meanwhile, the mixed powder is effectively filled in the microcrack region, and then carrying out primary and secondary tempering heat treatment under the protection of argon gas, so that the samarium cobalt permanent magnet with high toughness and high coercivity is obtained.
Further, the Fe-Co-Ni-based high-entropy alloy in the step (1) is FeCoNiCr0.2Si0.2，FeCoNiAl1.25Cr, FeCoNiAlSi and/or FeCoNiPdCu alloy.
Further, the flow speed of the high-speed argon gas flow in the step (3) is 20-50 m/s; the temperature of the primary tempering heat treatment is 700-1000 ℃, the heating rate is 2-40 ℃/min, the heat preservation time is 1-25 h, and then the primary tempering heat treatment is rapidly cooled to the room temperature; the temperature of the secondary tempering heat treatment is 200-650 ℃, the heating rate is 2-40 ℃/min, the heat preservation time is 1-25 h, and then the temperature is rapidly cooled to the room temperature.
Compared with the prior art, the invention has the following advantages and beneficial effects: the method comprises the steps of atomizing Fe-Co-Ni-based high-entropy alloy and nickel-based hard alloy particles to prepare mixed powder, then effectively utilizing lattice distortion in the high-entropy alloy and a microcrack region of the samarium-cobalt magnet after the samarium-cobalt magnet is impacted, impacting the mixed powder on the surface of the samarium-cobalt magnet by adopting high-speed argon gas flow, enabling the surface of the samarium-cobalt magnet to have the microcrack region by controlling the flow rate of the gas flow, effectively filling the mixed powder in the microcrack region, further improving the contact area between a diffuser and the magnet, improving the diffusion efficiency, and obtaining the samarium-cobalt permanent magnet with high toughness and high coercivity through primary and secondary tempering heat treatment under the protection of argon gas.
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited to only the following examples.
Example 1
(1) Preparation of FeCoNiCr by arc melting0.2Si0.2High-entropy alloy ingot casting;
(2) obtained in step (1)FeCoNiCr (R)0.2Si0.2Atomizing the high-entropy alloy cast ingot in vacuum, adding nickel-based hard alloy particles with the mark GH4037 in the atomizing process, wherein the average particle size of the nickel-based hard alloy is 50 microns, and the mass ratio of the nickel-based hard alloy to the high-entropy alloy cast ingot is 0.02: 1, atomizing at 900 ℃ for 3 h under 5 MPa to obtain mixed powder;
(3) removing an oxide film on the surface of the samarium cobalt magnet, firstly accelerating the mixed powder obtained in the step (2) by using high-speed argon gas flow with the flow rate of 20 m/s, then impacting the surface layer of the samarium cobalt magnet, wherein the impact time of the high-speed gas flow is 15 min, so that a microcrack region appears on the surface of the samarium cobalt magnet, meanwhile, the mixed powder is effectively filled in the microcrack region, and then carrying out primary and secondary tempering heat treatment under the protection of argon, wherein the temperature of the primary tempering heat treatment is 700 ℃, the temperature rise rate is 40 ℃/min, the heat preservation time is 5 h, and then rapidly cooling to room temperature; the temperature of the secondary tempering heat treatment is 200 ℃, the heating rate is 40 ℃/min, the heat preservation time is 5 h, and then the secondary tempering heat treatment is rapidly cooled to the room temperature, so that the samarium cobalt permanent magnet with high toughness and high coercivity is obtained.
Comparative example 1
Removing an oxide film on the surface of a samarium cobalt magnet, coating the surface with the mixed powder obtained in the step (2) in the example 1, then carrying out primary and secondary tempering heat treatment under the protection of argon, wherein the temperature of the primary tempering heat treatment is 700 ℃, the heating rate is 40 ℃/min, the heat preservation time is 5 h, and then carrying out quenching to room temperature; the temperature of the secondary tempering heat treatment is 200 ℃, the heating rate is 40 ℃/min, the heat preservation time is 5 h, and then the magnet is obtained after the temperature is rapidly cooled to the room temperature.
Example 2
(1) FeCoNiAl prepared by arc melting1.25Cr high-entropy alloy ingot casting;
(2) for FeCoNiAl obtained in the step (1)1.25Carrying out atomization treatment on the Cr high-entropy alloy cast ingot in vacuum, adding nickel-based hard alloy particles with the mark GH4037 in the atomization process, wherein the average particle size of the nickel-based hard alloy is 200 mu m, and the mass ratio of the nickel-based hard alloy to the high-entropy alloy cast ingot is 0.06: 1, the atomization temperature is 1Atomizing for 6 h at 300 ℃, and atomizing at 10 MPa to obtain mixed powder;
(3) removing an oxide film on the surface of the samarium cobalt magnet, firstly accelerating the mixed powder obtained in the step (2) by using high-speed argon gas flow with the flow rate of 35 m/s, then impacting the surface layer of the samarium cobalt magnet, wherein the impact time of the high-speed gas flow is 30 min, so that a microcrack region appears on the surface of the samarium cobalt magnet, meanwhile, the mixed powder is effectively filled in the microcrack region, and then carrying out primary and secondary tempering heat treatment under the protection of argon, wherein the temperature of the primary tempering heat treatment is 800 ℃, the temperature rise rate is 20 ℃/min, the heat preservation time is 15 h, and then rapidly cooling to room temperature; the temperature of the secondary tempering heat treatment is 400 ℃, the heating rate is 20 ℃/min, the heat preservation time is 15 h, and then the secondary tempering heat treatment is rapidly cooled to the room temperature, so that the samarium-cobalt permanent magnet with high toughness and high coercivity is obtained.
Comparative example 2
Removing an oxide film on the surface of a samarium cobalt magnet, coating the surface with the mixed powder obtained in the step (2) in the example 2, then carrying out primary and secondary tempering heat treatment under the protection of argon, wherein the temperature of the primary tempering heat treatment is 800 ℃, the heating rate is 20 ℃/min, the heat preservation time is 15 h, and then carrying out quenching to room temperature; the temperature of the secondary tempering heat treatment is 400 ℃, the heating rate is 20 ℃/min, the heat preservation time is 15 h, and then the magnet is obtained after the temperature is rapidly cooled to the room temperature.
Example 3
(1) Preparing a FeCoNiAlSi high-entropy alloy ingot by adopting electric arc melting;
(2) carrying out atomization treatment on the FeCoNiAlSi high-entropy alloy ingot obtained in the step (1) in vacuum, adding nickel-based hard alloy particles with the mark of GH4037 in the atomization process, wherein the average particle size of the nickel-based hard alloy is 400 mu m, and the mass ratio of the nickel-based hard alloy to the high-entropy alloy ingot is 0.1: 1, atomizing at 1500 ℃ for 10 h under 18 MPa to obtain mixed powder;
(3) removing an oxide film on the surface of the samarium cobalt magnet, firstly accelerating the mixed powder obtained in the step (2) by using high-speed argon gas flow with the flow rate of 50 m/s, then impacting the surface layer of the samarium cobalt magnet, wherein the impact time of the high-speed gas flow is 45 min, so that a microcrack region appears on the surface of the samarium cobalt magnet, meanwhile, the mixed powder is effectively filled in the microcrack region, and then carrying out primary tempering heat treatment and secondary tempering heat treatment under the protection of argon, wherein the temperature of the primary tempering heat treatment is 1000 ℃, the heating rate is 5 ℃/min, the heat preservation time is 25 h, and then rapidly cooling to room temperature; the temperature of the secondary tempering heat treatment is 650 ℃, the heating rate is 5 ℃/min, the heat preservation time is 25 h, and then the secondary tempering heat treatment is rapidly cooled to room temperature, so that the samarium cobalt permanent magnet with high toughness and high coercivity is obtained.
Comparative example 3
Removing an oxide film on the surface of the samarium cobalt magnet, coating the mixed powder obtained in the step (2) in the example 3 on the surface, then carrying out primary and secondary tempering heat treatment under the protection of argon, wherein the temperature of the primary tempering heat treatment is 1000 ℃, the heating rate is 5 ℃/min, the heat preservation time is 25 h, and then carrying out quenching to room temperature; the temperature of the secondary tempering heat treatment is 650 ℃, the heating rate is 5 ℃/min, the heat preservation time is 25 h, and then the magnet is obtained after the secondary tempering heat treatment is quenched to room temperature.
The samples prepared in the above examples and comparative examples were subjected to magnetic and mechanical property tests, and the comparative results are shown in table 1.
The present invention is further illustrated by the following examples, which are intended to facilitate the understanding of the reader, but are not intended to limit the scope of the present invention to such examples, and any technical extensions or remnants of the present invention may be protected by the present invention.
TABLE 1
Claims (3)
1. A method for preparing a permanent magnet with high toughness and high coercivity is characterized by comprising the following steps:
(1) preparing Fe-Co-Ni-based high-entropy alloy cast ingots by adopting electric arc melting;
(2) carrying out atomization treatment on the Fe-Co-Ni-based high-entropy alloy cast ingot obtained in the step (1) in vacuum, adding a certain amount of nickel-based hard alloy particles with the mark of GH4037 in the atomization process, wherein the average particle size of the nickel-based hard alloy is 20-500 mu m, and the mass ratio of the nickel-based hard alloy to the high-entropy alloy cast ingot is 0.01-0.1: 1, atomizing at 900-1600 ℃, for 3-10 h and under 5-20 MPa to obtain mixed powder;
(3) and (3) removing an oxide film on the surface of the samarium cobalt magnet, firstly accelerating the mixed powder obtained in the step (2) by using high-speed argon gas flow, then impacting the surface layer of the samarium cobalt magnet, wherein the impacting time of the high-speed gas flow is 15-45 min, so that a microcrack region appears on the surface of the samarium cobalt magnet, meanwhile, the mixed powder is effectively filled in the microcrack region, and then carrying out primary and secondary tempering heat treatment under the protection of argon gas, so that the samarium cobalt permanent magnet with high toughness and high coercivity is obtained.
2. A method for producing a high-toughness and high-coercive force permanent magnet according to claim 1, characterized in that: the Fe-Co-Ni-based high-entropy alloy in the step (1) is FeCoNiCr0.2Si0.2，FeCoNiAl1.25Cr, FeCoNiAlSi and/or FeCoNiPdCu alloy.
3. A method for producing a high-toughness and high-coercive force permanent magnet according to claim 1, characterized in that: the flow velocity of the high-speed argon gas flow in the step (3) is 20-50 m/s; the temperature of the primary tempering heat treatment is 700-1000 ℃, the heating rate is 2-40 ℃/min, the heat preservation time is 1-25 h, and then the primary tempering heat treatment is rapidly cooled to the room temperature; the temperature of the secondary tempering heat treatment is 200-650 ℃, the heating rate is 2-40 ℃/min, the heat preservation time is 1-25 h, and then the temperature is rapidly cooled to the room temperature.
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