CN117497315A - Anisotropic rare earth permanent magnet powder and preparation method thereof - Google Patents
Anisotropic rare earth permanent magnet powder and preparation method thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 47
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 45
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000006247 magnetic powder Substances 0.000 claims abstract description 59
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 42
- 239000010959 steel Substances 0.000 claims abstract description 42
- 238000005098 hot rolling Methods 0.000 claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000004806 packaging method and process Methods 0.000 claims abstract description 6
- 238000011049 filling Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 28
- 238000005516 engineering process Methods 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 10
- 238000010791 quenching Methods 0.000 claims description 8
- 230000000171 quenching effect Effects 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 5
- 238000005056 compaction Methods 0.000 claims description 4
- 230000006698 induction Effects 0.000 claims description 4
- 239000000155 melt Substances 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 238000000713 high-energy ball milling Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 239000000696 magnetic material Substances 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 13
- 229910001172 neodymium magnet Inorganic materials 0.000 description 13
- 238000005096 rolling process Methods 0.000 description 12
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 10
- 238000005520 cutting process Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000003723 Smelting Methods 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000003754 machining Methods 0.000 description 3
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 3
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 3
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
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- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- KPLQYGBQNPPQGA-UHFFFAOYSA-N cobalt samarium Chemical compound [Co].[Sm] KPLQYGBQNPPQGA-UHFFFAOYSA-N 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
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- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Classifications
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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
- H01F41/0266—Moulding; Pressing
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—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
- H01F1/04—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 metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
- H01F1/0556—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together pressed
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—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
- H01F1/04—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 metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0576—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together pressed, e.g. hot working
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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
- H01F41/0273—Imparting anisotropy
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- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The invention relates to the technical field of magnetic materials, in particular to anisotropic rare earth permanent magnet powder and a preparation method thereof. The preparation method comprises the following steps: filling amorphous or nanocrystalline magnetic powder into a steel sleeve and compacting to prepare steel sleeve packaging magnetic powder; then hot rolling the steel sleeve encapsulated magnetic powder to prepare a hot rolled magnet; then the hot-rolled magnet is made into rare earth permanent magnet powder; wherein, the grain size of the nanocrystalline magnetic powder is smaller than 20 nanometers. The preparation method can realize the manufacture of anisotropic permanent magnet powder in large batch, improves the production efficiency, is suitable for various magnetic powder compositions, and the prepared magnetic powder has the characteristics of high magnetic energy product and high coercivity, and has wide application range and high application value. In addition, the preparation method can reduce energy consumption and production cost.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to anisotropic rare earth permanent magnet powder and a preparation method thereof.
Background
The rare earth permanent magnetic material has the strongest magnetic performance and the widest application path, and especially plays an irreplaceable important role in new energy industry. Along with the progress and development of society, the demands of people for rare earth permanent magnet materials are more and more vigorous, and the application prospect of the rare earth permanent magnet materials is wider. In view of the situation, global researchers put more force into the development and application of novel rare earth permanent magnet materials so as to better meet the use demands of the rare earth permanent magnet materials.
The rare earth permanent magnet materials can be divided into two main categories according to the manufacturing technology of the rare earth permanent magnet materials. The first is a sintered rare earth permanent magnet material, typical representatives of which are sintered neodymium iron boron permanent magnets and sintered samarium cobalt permanent magnets. The sintered rare earth permanent magnetic material is a compact sintered body with the density close to the intrinsic theoretical density of the material, and has higher magnetic energy product. However, the magnet is generally a blank of a simple sintered shape, and then formed by relatively complex machining to produce a magnet of a desired shape. Machining processes can form 20-50wt.% of machining scrap, depending on the final shape and size of the magnet. The second type is a bonded rare earth permanent magnet material, typically a bonded neodymium iron boron permanent magnet. The bonded magnet is prepared by firstly preparing magnetic powder with better magnetic property, then mixing the magnetic powder with an adhesive and then forming, wherein the main forming process comprises compression molding and injection molding. The manufacturing process of bonded magnets determines that such magnets can achieve near net shape formation and therefore do not require complex post-processing and do not form significant amounts of processing waste. However, bonded magnets have far lower magnetic properties than sintered magnets because of the incorporation of binders and the isotropic non-oriented products that are the mainstream products of today.
The raw materials for manufacturing the bonded magnet at present are mainly neodymium iron boron thin belts prepared by a melt rapid quenching technology, and the thin belts have good comprehensive magnetic properties, form a series of brands through years of development and realize wide application. Unfortunately, such magnetic powders are magnetically isotropic and therefore do not allow maximization of the intrinsic magnetic properties of the material. Therefore, the development of the magnetic anisotropic rare earth permanent magnet powder material is a necessary path for further improving the magnetic performance of the bonded rare earth permanent magnet material and expanding the application range of the bonded rare earth permanent magnet material.
Heretofore, there are mainly two methods for preparing anisotropic neodymium iron boron magnetic powder. The first is the hydrogenation-disproportionation-dehydrogenation-recombination process (HDDR process for short). Chinese patent CN1154124C discloses a method for preparing micron-sized anisotropic neodymium iron boron magnetic powder by adopting HDDR method, and the obtained powderThe maximum magnetic energy product of the magnetic powder reaches 358kJ/m 3 . Another method is to prepare an anisotropic neodymium iron boron magnet by hot pressing-hot upsetting and then break the anisotropic neodymium iron boron magnet into anisotropic magnetic powder. For example, chinese patent CN103151161a discloses the preparation of isotropic magnets from hot pressed neodymium-iron-boron rapid quenching powder, followed by thermal deformation to obtain anisotropic neodymium-iron-boron magnets, and finally crushing to obtain anisotropic neodymium-iron-boron magnetic powder.
The anisotropic NdFeB magnetic powder with good magnetic property can be obtained by the method, but the two methods have the same short plate, i.e. the large-batch preparation of the magnetic powder is difficult to realize. In particular, the latter method has lower pulverizing efficiency. This limitation in yield also greatly limits the wide application of anisotropic neodymium iron boron magnetic powder.
Therefore, a new technology is needed to solve the above problems, and a preparation method of anisotropic permanent magnet powder is provided, which is easy to prepare in large scale, suitable for various magnetic powder compositions, and good in magnetic performance.
Disclosure of Invention
First, the invention provides a preparation method of anisotropic rare earth permanent magnet powder, which comprises the following steps:
filling amorphous or nanocrystalline magnetic powder into a steel sleeve and compacting to prepare steel sleeve packaging magnetic powder;
then hot rolling the steel sleeve encapsulated magnetic powder to prepare a hot rolled magnet;
then the hot-rolled magnet is made into rare earth permanent magnet powder;
wherein, the grain size of the nanocrystalline magnetic powder is smaller than 20 nanometers.
According to the invention, when the nanocrystalline magnetic powder is selected as a raw material, the hot-rolled magnet with high magnetic energy product and high coercivity can be prepared by controlling the grain size of the nanocrystalline magnetic powder to be smaller than 20 nanometers and combining hot rolling treatment, so that the anisotropic rare earth permanent magnet powder with high magnetic energy product and high coercivity is prepared.
Preferably, after the compacting, vacuumizing and packaging are carried out, so as to obtain the steel bushing packaged magnetic powder.
The packaging treatment is to weld and seal the steel sleeve. The purpose is to ensure that the compacted powder does not contact air during subsequent hot rolling.
Preferably, the vacuum degree of the vacuuming is below 0.01 Pa;
and/or, after the compaction, the density of the powder is not less than 6g/cm 3 。
The vacuum pumping process can adopt a mechanical pump, a diffusion pump or a molecular pump and other vacuum devices. And welding a vacuum steel tube at one end of the steel sleeve, and then sealing the vacuum steel tube to meet the vacuum requirement.
More preferably, the density of the powder after compaction is 6.3-7.2 g/cm 3 。
The powder density is more favorable for obtaining the hot-rolled magnet with better performance after hot rolling.
The compaction process is carried out at room temperature at a pressure of 1-5 GPa, preferably at a pressure hold of 10-30 minutes.
Preferably, the release agent is coated on the inner wall of the steel sleeve before the amorphous or nanocrystalline magnetic powder is packed into the steel sleeve and compacted.
Preferably, the mold release agent includes, but is not limited to, molybdenum disulfide, boron nitride.
Preferably, the steel bushing encapsulated magnetic powder is placed at 500-700 ℃ for heat preservation and then hot-rolled; preferably, after the hot rolling is completed, the reduction of the steel jacket is more than 95%.
When the grain size of the nanocrystalline magnetic powder is smaller than 20 nanometers, the rolling reduction of the steel sleeve after hot rolling is controlled to be larger than 95%, and the magnetic property of the prepared hot rolled magnet is better, so that the magnetic property of the finally prepared anisotropic rare earth permanent magnet powder is better.
Preferably, in the hot rolling process, the linear velocity of the rolls is controlled to be 0.05 to 0.1 m/s; more preferably 0.05 to 0.06 m/s.
The invention further discovers that the magnetic performance of the anisotropic rare earth permanent magnet powder with the same component is better under the condition of lower hot roll speed.
Preferably, the incubation time is 5 to 15 minutes.
The hot rolling process is to push the steel sleeve from one end of the roller to the other end of the roller for forming. The process may employ single pass or multiple pass rolling. The hot rolling process is carried out in air.
Preferably, after the hot rolling, the steel sleeve is cut to produce a hot rolled magnet.
The cutting may be performed using a microtome or a laser cutter, or the like.
Preferably, the cutting is wire cutting.
The shape of the steel sleeve in the invention can be a cube, a cuboid, a cylinder or a cylinder with other sections, and the size is not particularly limited, so that the yield of magnetic powder is planned to be obtained and the size which can be processed by a rolling mill for subsequent hot rolling is limited.
Preferably, the hot rolled magnet is mechanically crushed, the particle size of the mechanically crushed powder is below 425 microns, and then the mechanically crushed powder is subjected to ball milling treatment to obtain the rare earth permanent magnet powder with the average particle size of 10-150 microns.
Preferably, the amorphous or nanocrystalline magnetic powder has the following composition (mass percent):
RE x Fe 100-x-y-z M y B z wherein RE is at least one of Nd, pr, dy, ho, gd, tb, la, ce, Y and M is at least one of Co, al, cu, ga, nb, ti, zr, hf; x, y, z satisfy the following relationship: x is more than or equal to 28 and less than or equal to 32,0.5, y is more than or equal to 3, and z is more than or equal to 0.8 and less than or equal to 1.0;
or the amorphous or nanocrystalline magnetic powder comprises the following components:
RE x Co 100-x-y M y wherein RE is at least one of Sm, pr, gd, ce, Y and M is at least one of Fe, mn, cu, nb, zr, hf; x and y satisfy the following relationship: x is more than or equal to 25 and less than or equal to 35,0.3, y is more than or equal to 5.
Preferably, the rare earth permanent magnet master alloy is prepared by adopting an induction smelting or arc smelting technology, and then the amorphous or nanocrystalline magnetic powder is prepared from the rare earth permanent magnet master alloy by adopting a melt rapid quenching or high-energy ball milling technology.
In some embodiments, the source of the amorphous or nanocrystalline magnetic powder is a commercially available quick-quench powder, such as a series of magnetic powders available from the company migku's (Tianjin) company MQU.
Those skilled in the art can further combine the above preferred embodiments to arrive at other preferred embodiments.
Further, the present invention provides an anisotropic rare earth permanent magnet powder produced by the production method in any one of the above embodiments.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method can realize the manufacture of anisotropic permanent magnet powder in large batch, improves the production efficiency, is suitable for various magnetic powder compositions, and the prepared magnetic powder has the characteristics of high magnetic energy product and high coercivity, and has wide application range and high application value. In addition, the preparation method can reduce energy consumption and production cost.
Drawings
Fig. 1 is a microstructure photograph of the anisotropic rare earth permanent magnet powder of example 1.
Fig. 2 is a microstructure photograph of the anisotropic rare earth permanent magnet powder of example 2.
Fig. 3 is an X-ray diffraction pattern of the anisotropic rare earth permanent magnet powder of example 1.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The examples are not intended to identify the particular technology or conditions, and are either conventional or are carried out according to the technology or conditions described in the literature in this field or are carried out according to the product specifications. The reagents and instruments used, etc. are not identified to the manufacturer and are conventional products available for purchase by regular vendors.
Example 1
The embodiment provides a preparation method of anisotropic rare earth permanent magnet powder, which comprises the following steps:
vacuum induction smelting technology is adopted to prepare Nd as nominal component 29.9 Fe 62.6 Cu 0.9 Ga 0.6 B 1.0 (wt.%) then preparing it into nano-crystal magnetic powder with crystal grain size of 10 nm by melt quick quenching technique. The magnetic powder is filled into a steel sleeve with the inner wall uniformly coated with molybdenum disulfide and compacted, and the density of the compacted powder is 6.3 g/cm < 3 >. The steel sleeve is welded and sealed after vacuumizing, and the internal vacuum degree is 0.005Pa. The sealing steel sleeve is subjected to heat preservation at 500 ℃ for 5 minutes and then hot rolled, the linear speed of a roller in the rolling process is 0.05 m/s, and the rolling reduction of the steel sleeve after rolling is completed reaches 96%. After hot rolling, wire cutting is carried out on the steel sleeve to obtain a thermal deformation block-shaped magnet, and the magnet is firstly coarsely crushed to the maximum particle diameter d by adopting a mechanical crushing method<425 micrometers, and then further finely crushing by ball milling, and finally obtaining the rare earth permanent magnet powder product, wherein the average particle size of the rare earth permanent magnet powder product is 120 micrometers.
Example 2
The embodiment provides a preparation method of anisotropic rare earth permanent magnet powder, which comprises the following steps:
vacuum arc melting technology is adopted to prepare Sm with nominal composition 13.7 Pr 19.2 Co 67.1 (wt.%) and then preparing it into amorphous magnetic powder by adopting high-energy ball milling technology. Filling magnetic powder into a steel sleeve with inner wall uniformly coated with boron nitride, compacting, and compacting to obtain powder with a density of 7.2g/cm 3 . The steel sleeve is welded and sealed after vacuumizing, and the internal vacuum degree is 0.008Pa. The sealing steel sleeve is subjected to heat preservation at 700 ℃ for 15 minutes and then hot rolled, the linear speed of a roller in the rolling process is 0.1 m/s, and the rolling reduction of the steel sleeve after rolling is completed reaches 96%. After hot rolling, wire cutting is carried out on the steel sleeve to obtain a thermal deformation block-shaped magnet, and the magnet is firstly coarsely crushed to the maximum particle diameter d by adopting a mechanical crushing method<425 micrometers, and then further finely crushing by ball milling, and finally obtaining the rare earth permanent magnet powder product with the average particle size of 80 micrometers.
Example 3
The embodiment provides a preparation method of anisotropic rare earth permanent magnet powder, which comprises the following steps:
vacuum induction smelting technology is adopted to prepare Nd as nominal component 29.9 Fe 62.6 Cu 0.9 Ga 0.6 B 1.0 (wt.%) then preparing it into nano-crystal magnetic powder with crystal grain size of 10 nm by melt quick quenching technique. The magnetic powder is filled into a steel sleeve with the inner wall uniformly coated with molybdenum disulfide and compacted, and the density of the compacted powder is 6.3 g/cm < 3 >. The steel sleeve is welded and sealed after vacuumizing, and the internal vacuum degree is 0.005Pa. The sealing steel sleeve is subjected to heat preservation at 500 ℃ for 5 minutes and then hot rolled, the linear speed of a roller in the rolling process is 0.1 m/s, and the rolling reduction of the steel sleeve after rolling is completed reaches 96%. After hot rolling, wire cutting is carried out on the steel sleeve to obtain a thermal deformation block-shaped magnet, and the magnet is firstly coarsely crushed to the maximum particle diameter d by adopting a mechanical crushing method<425 micrometers, and then further finely crushing by ball milling, and finally obtaining the rare earth permanent magnet powder product, wherein the average particle size of the rare earth permanent magnet powder product is 120 micrometers.
Comparative example
This comparative example provides a method for preparing rare earth permanent magnet powder, the steps only differ from example 1:
the melt rapid quenching technology is adopted to prepare the nanocrystalline magnetic powder, and the grain size of the magnetic powder is 50 nanometers.
Test examples
The magnetic properties of the rare earth permanent magnet powders prepared in the above examples and comparative examples were tested. The specific method is as follows:
the prepared magnetic powder is weighed (mass is 30 mg), and the magnetic powder and 3g of AB glue are evenly mixed and then placed in a static magnetic field (2 Tesla) for solidification. After the solidified sample is magnetized along the direction parallel to the static magnetic field, the hysteresis loop of the solidified sample is tested by using a vibrating sample magnetometer, and key magnetic parameters such as magnetic energy and coercive force are obtained.
The test results are shown in Table 1.
TABLE 1
| Project | Magnetic energy product/MGOe | coercivity/kOe |
| Example 1 | 26.5 | 14.5 |
| Example 2 | 18.7 | 19.3 |
| Example 3 | 24.7 | 14.6 |
| Comparative example | 22.1 | 8.8 |
The result shows that the anisotropic magnetic powder prepared by the preparation method has good magnetic performance. In addition, the neodymium iron boron magnetic powder with the same components has better magnetic performance under the condition of lower hot roller speed. When the initial grain size of the sample is large (comparative example), the magnetic properties of the magnetic powder are significantly reduced under the same process conditions.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for preparing anisotropic rare earth permanent magnet powder, comprising the steps of:
filling amorphous or nanocrystalline magnetic powder into a steel sleeve and compacting to prepare steel sleeve packaging magnetic powder;
then hot rolling the steel sleeve encapsulated magnetic powder to prepare a hot rolled magnet;
then the hot-rolled magnet is made into rare earth permanent magnet powder;
wherein, the grain size of the nanocrystalline magnetic powder is smaller than 20 nanometers.
2. The method according to claim 1, wherein after the compacting, vacuum-pumping and packaging are performed to obtain steel-jacketed magnetic powder.
3. The production method according to claim 2, wherein the degree of vacuum of the evacuated air is 0.01Pa or less;
and/or, after the compaction, the density of the powder is not less than 6g/cm 3 。
4. The method of claim 1, wherein the release agent is applied to the inner wall of the steel jacket prior to compacting the amorphous or nanocrystalline magnetic powder in the steel jacket.
5. The method according to claim 1, wherein the hot rolling is performed after the steel bushing-packed magnetic powder is placed at 500 to 700 ℃ for heat preservation;
preferably, after the hot rolling is completed, the reduction of the steel jacket is more than 95%.
6. The method of claim 1, wherein after the hot rolling, the steel sleeve is cut to produce a hot rolled magnet.
7. The method according to claim 1, wherein the hot-rolled magnet is mechanically pulverized to have a powder particle diameter of 425 μm or less, and the mechanically pulverized powder is ball-milled to obtain rare earth permanent magnet powder having an average particle diameter of 10 to 150 μm.
8. The method according to claim 1, wherein the composition of the amorphous or nanocrystalline magnetic powder is:
RE x Fe 100-x-y-z M y B z wherein RE is at least one of Nd, pr, dy, ho, gd, tb, la, ce, Y and M is at least one of Co, al, cu, ga, nb, ti, zr, hf; x, y, z satisfy the following relationship: x is more than or equal to 28 and less than or equal to 32,0.5, y is more than or equal to 3, and z is more than or equal to 0.8 and less than or equal to 1.0;
or the amorphous or nanocrystalline magnetic powder comprises the following components:
RE x Co 100-x-y M y wherein RE is at least one of Sm, pr, gd, ce, Y and M is at least one of Fe, mn, cu, nb, zr, hf; x and y satisfy the following relationship: x is more than or equal to 25 and less than or equal to 35,0.3, y is more than or equal to 5.
9. The preparation method according to claim 8, wherein the rare earth permanent magnet master alloy is prepared by an induction melting or arc melting technology, and then the amorphous or nanocrystalline magnetic powder is prepared by a melt rapid quenching or high-energy ball milling technology.
10. Anisotropic rare earth permanent magnet powder, characterized in that it is produced by the production method according to any one of claims 1 to 9.
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