CN108346508A - A kind of preparation method of nanocrystalline complex phase Nd-Fe-B permanent magnet texturing enhancing - Google Patents
A kind of preparation method of nanocrystalline complex phase Nd-Fe-B permanent magnet texturing enhancing Download PDFInfo
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- CN108346508A CN108346508A CN201710050591.7A CN201710050591A CN108346508A CN 108346508 A CN108346508 A CN 108346508A CN 201710050591 A CN201710050591 A CN 201710050591A CN 108346508 A CN108346508 A CN 108346508A
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- permanent magnet
- enhancing
- texturing
- complex phase
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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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- 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
- H01F41/0266—Moulding; Pressing
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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 present invention provides a kind of preparation methods of nanocrystalline complex phase Nd-Fe-B permanent magnet texturing enhancing.The NdFeB composite bodies obtained through hot-pressing processing are carried out thermal deformation field by this method with low rate at low temperature, obtain complete fine and close anisotropic NdFeB complex phase permanents block.Compared with traditional handicraft, deformation orientation, effectively can inhibit crystal grain to grow up at low temperature, the Grain-Boundary Phase that the thermal deformation of low rate progress simultaneously is conducive under low temperature is uniformly distributed, enhance hard magnetic phase texture, moreover it is possible to which the formation and extension for inhibiting crackle in deformation process improve densification and the magnetic property of block.
Description
Technical field
The present invention relates to technical field of magnetic materials, refer in particular to a kind of nanocrystalline complex phase Nd-Fe-B permanent magnet texturing increasing
Strong preparation method.
Background technology
1993, Skomski and Coey theoretically foretold that anisotropic nanocomposite permanent magnets have 120MGOe
Magnetic energy product, be far above the theoretical value 64MGOe of existing powder sintered NdFeB magnets, and content of rare earth is low, this makes it be expected to
As the permanent magnet material of next-generation high-performance, low cost.However, it is one huge experimentally to prepare this ideal nanostructure
Big challenge.
Hot-pressing thermal deformation technology is the effective means for preparing the single-phase NdFeB permanent magnets of complete fine and close anisotropy, it is generally recognized that
It is that Nd-rich phase promotes crystal grain rotation as grain boundary liquid phase, so that magnet is formed sheet crystal structure, to which the magnetocrystalline for obtaining strong is each
Anisotropy.In order to prepare the mutually compound heat distortion magnet of soft or hard magnetism, researchers use rich rare earth quenched powder and poor rare earth
Quenched powder mixes and the modes such as poor rare earth quenched powder and low-melting alloy mixing are attempted.
Microstructure shows the heat distortion magnet mixed for rich rare earth quenched powder and poor rare earth quenched powder, only rich dilute
Native liquid phase region forms hard magnetic phase texture, and poor rare earth region does not deform orientation substantially;For poor rare earth quenched powder and eutectic
The heat distortion magnet of point alloy mixing is used as the deformation orientation energy that Grain-Boundary Phase improves built-up magnet by introducing low-melting alloy
Power can be prepared with notable anisotropic full-compact nanometer crystalline substance complex phase permanent material.But traditional heat distortion temperature
It is higher, 700 DEG C or more are generally reached, flake crystalline overgrowth, lateral dimension is made to reach a few micrometers, considerably beyond soft or hard magnetic phase
Required spin-exchange-coupled size.In addition, traditional thermal deformation technique deformation time is short, low melting point Grain-Boundary Phase is unevenly distributed, meeting
Deteriorate the anisotropy of built-up magnet.
Invention content
Present situation in view of the above technology, the present invention is intended to provide a kind of nanocrystalline complex phase Nd-Fe-B permanent magnet texturing enhancing
Preparation method can not only realize that built-up magnet deforms, and can further enhance knitting for deformation magnet at a lower temperature
Structure ability.
To achieve the goals above, the present inventor uses hot pressing thermal deformation method, is found after many experiments exploratory development
It in thermal deformation process, is deformed using low temperature low speed, that is, control temperature can effectively inhibit crystal grain long at 550 DEG C~700 DEG C
Greatly, it is ensured that the exchange-coupling interaction soft, hard magnetic is alternate;It is deformed using low rate, that is, control is fast along the deformation of pressure direction
Rate v≤4um/s can promote the Grain-Boundary Phase under low temperature to be uniformly distributed, and not only be conducive to enhancing hard magnetic phase texture, moreover it is possible to inhibit low temperature
The formation and extension of crackle in deformation process, improve densification and the magnetic property of block.
That is, the technical scheme is that:A kind of preparation method of nanocrystalline complex phase Nd-Fe-B permanent magnet texturing enhancing,
Using hot pressing thermal deformation method, that is, include the hot pressing that the powder of neodymium iron boron two-phase composite permanent-magnetic material is pre-formed as to green body,
And the microcosmic texture of green body is turned to the thermal deformation process of anisotropy block, it is characterized in that:In thermal deformation process, edge is controlled
Rate of deformation v≤4um/s of pressure direction, control deformation temperature is 550 DEG C~700 DEG C.
The neodymium iron boron two-phase composite permanent-magnetic material is with intermetallic compound Re2Fe14Permanent-magnet material based on B,
Main component is rear earth element nd (Nd), iron (Fe), boron (B), and in order to obtain different performance, part neodymium can use dysprosium (Dy), praseodymium
(Pr) etc. other rare earth metals substitute.Also, anisotropy block made from the powder using the Nd-Fe-B permanent magnet material is packet
The Re of phase containing hard magnetic2Fe14The neodymium iron boron two-phase composite construction of B and soft magnetism phase α-Fe.
Preferably, in thermal deformation process, controlled at 550 DEG C~650 DEG C, further preferably 600 DEG C~650
℃。
Preferably, in thermal deformation process, control along the rate of deformation v of pressure direction be 0.02um/s≤v≤
4um/s, further preferably 0.5um/s≤v≤1um/s.
The thermal deformation device used in the thermal deformation process is unlimited, preferably vacuum induction thermal deformation device.
Thermal deformation field is carried out again preferably, the green body is put into the contour 304 stainless steel protections set of equal diameter.
Preferably, pre-incubation 10min~30min before thermal deformation.
Preferably, in thermal deformation process, it is evacuated to 10 first-4Pa is re-filled with a small amount of Ar gas as protective gas.
Preferably, the low-melting alloy phase containing rare earth element is adulterated in the neodymium iron boron two-phase composite permanent-magnetic material,
Grain-Boundary Phase is filled in the rare earth liquid phase of the thermal deformation process of the present invention, doping, promotes the orientation texture of Hard Magnetic crystal grain.As excellent
Choosing, the quality of the doped alloys account for the 1%~10% of neodymium iron boron two-phase composite permanent-magnetic material quality, further preferably 2%~
8%.
Compared with prior art, the present invention by the neodymium iron boron complex phase green body obtained through hot-pressing processing at low temperature with low rate
Thermal deformation field is carried out, the full densification Re of texture enhancing is obtained2Fe14B composite permanet magnet blocks.Compared to traditional handicraft, low
The lower deformation orientation of temperature, can effectively inhibit crystal grain to grow up, while the Grain-Boundary Phase that low rate progress thermal deformation is conducive under low temperature is uniform
Distribution enhances hard magnetic phase texture, moreover it is possible to which the formation and extension for inhibiting crackle in deformation process improve densification and the magnetism of block
Energy.
Description of the drawings
Fig. 1 is blocky permanent magnet made from embodiment 1 along the fracture pattern SEM pictures of pressure direction;
Fig. 2 is blocky permanent magnet made from comparative example along the fracture pattern SEM pictures of pressure direction;
Fig. 3 is embodiment 1, embodiment 2 and the demagnetizing curve of blocky permanent magnet at room temperature made from comparative example.
Specific implementation mode
The present invention will be further described with reference to the accompanying drawings and embodiments, it should be pointed out that embodiment described below
It is intended to be convenient for the understanding of the present invention, without playing any restriction effect.
Embodiment 1:
In the present embodiment, raw material is the poor rare earth two-phase magnetic powder of commercialization bought from Magnequench (Tianjin) Co., Ltd.
NdFeB (15-7), the raw material and low-melting alloy powder Nd70Cu30Mixing, the doping of the Nd-Cu alloy powders account for the raw material
The 8% of quality, obtains doped raw material.
The preparation method of the Nd-Cu alloy powders is as follows:
(1) Nd is made through vacuum induction melting according to NdCu alloying component dispensings70Cu30Alloy cast ingot;
(2) it is crushed the Nd under protection of argon gas70Cu30Alloy cast ingot, ground, sieving, it is below in 90um to obtain grain size
NdCu alloy powders;
Using the doped raw material, anisotropic Nd is prepared using hot pressing thermal deformation method2Fe14B complex phase permanent block materials,
It is specific as follows:
(1) hot pressing:The quantitative doped raw material is packed into sintered-carbide die, vacuum induction hot pressing thermal change is used
Shape dress is set, in vacuum 4 × 10-2Pa, pressure 215MPa, hot pressing is preforming under the conditions of 700 DEG C, obtains green body;
(2) thermal deformation process:The green body obtained in (1) is first put into 304 contour stainless steel capsules of equal diameter, then is put
Enter to preset in the sintered-carbide die of size;Incude hot pressing thermal deformation device using high vacuum, is evacuated to 10-4Pa, then fill
Enter a small amount of Ar as protective gas;Then control carries out heat along the rate of deformation v=1um/s of pressure direction under the conditions of 600 DEG C
Compressive strain obtains two-phase composite permanet magnet block materials to predetermined size.
Embodiment 2:
In the present embodiment, using with identical doped raw material in embodiment 1.
Using the doped raw material, anisotropic Nd is prepared using hot pressing thermal deformation method2Fe14B complex phase permanent block materials,
It is specific as follows:
(1) identical with (1) the step of embodiment 2;
(2) essentially identical with (2) the step of embodiment 2, it is unique the difference is that control is along pressure side under the conditions of 600 DEG C
To rate of deformation v=2um/s carry out hot compression deformation to the predetermined size, obtain two-phase composite permanet magnet block materials.
Comparative example:
In the present embodiment, using with identical doped raw material in embodiment 1.
Using the doped raw material, anisotropic Nd is prepared using hot pressing thermal deformation method2Fe14B complex phase permanent block materials,
It is specific as follows:
(1) identical with (1) the step of embodiment 2;
(2) essentially identical with (2) the step of embodiment 2, except that control is along pressure direction under the conditions of 600 DEG C
Rate of deformation v=8um/s carry out hot compression deformation to predetermined size, obtain two-phase composite permanet magnet block materials.
Fig. 1 and Fig. 2 is blocky permanent magnet made from above-described embodiment 1 and comparative example respectively along the fracture of pressure direction
Pattern SEM pictures.Compared with comparative example, compare Fig. 1 and Fig. 2, is shown in the texture of nanocrystal under deformation condition at a slow speed
Change is enhanced, and good orientation texture is formd.
Fig. 3 is that above-described embodiment 1, embodiment 2 and the demagnetization of blocky permanent magnet at room temperature made from comparative example are bent
Line, display control carry out the anisotropy that deformation at a slow speed enhances permanent magnet along pressure direction.
The following table 1 is the magnetic property of embodiment 1, embodiment 2 and blocky permanent magnet made from comparative example, display and comparison
Embodiment is compared, and the magnetic property of the blocky permanent magnet deformed at a slow speed is improved.
Table 1:
Hci(kOe) | Br(kG) | (BH)max(MGOe) | |
Embodiment 1 | 8.14 | 12.15 | 31.18 |
Embodiment 2 | 7.23 | 11.91 | 28.21 |
Comparative example | 7.03 | 11.18 | 24.63 |
Technical scheme of the present invention is described in detail in embodiment described above, it should be understood that described in having gone up only
For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in the spirit of this statement,
Supplement or similar fashion replacement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of nanocrystalline complex phase Nd-Fe-B permanent magnet texturing enhancing, using hot pressing thermal deformation method, that is, including
The powder of neodymium iron boron complex phase permanent material is pre-formed as to the hot pressing of green body, and the microcosmic texture of green body is turned to each to different
The thermal deformation process of property block, it is characterized in that:In thermal deformation process, rate of deformation v≤4um/ along pressure direction is controlled
S, controlled at 550 DEG C~700 DEG C.
2. the preparation method of nanocrystalline complex phase Nd-Fe-B permanent magnet texturing enhancing as described in claim 1, it is characterized in that:
In thermal deformation process, controlled at 550 DEG C~650 DEG C.
3. the preparation method of nanocrystalline complex phase Nd-Fe-B permanent magnet texturing enhancing as described in claim 1, it is characterized in that:
In thermal deformation process, controlled at 600 DEG C~650 DEG C.
4. the preparation method of nanocrystalline complex phase Nd-Fe-B permanent magnet texturing enhancing as described in claim 1, it is characterized in that:
In thermal deformation process, control is 0.02um/s≤v≤4um/s along the rate of deformation v of pressure direction.
5. the preparation method of nanocrystalline complex phase Nd-Fe-B permanent magnet texturing enhancing as claimed in claim 4, it is characterized in that:
In thermal deformation process, control is 0.5um/s≤v≤1um/s along the rate of deformation v of pressure direction.
6. the preparation method of nanocrystalline complex phase Nd-Fe-B permanent magnet texturing enhancing as described in claim 1, it is characterized in that:Heat
Pre-incubation 10min~30min before deformation.
7. the preparation method of nanocrystalline complex phase Nd-Fe-B permanent magnet texturing enhancing as described in claim 1, it is characterized in that:It will
The green body is put into the contour 304 stainless steel protections set of equal diameter and carries out thermal deformation field again.
8. the preparation method of nanocrystalline complex phase Nd-Fe-B permanent magnet texturing enhancing as described in claim 1, it is characterized in that:Institute
High vacuum induction heat deformation device is used in the thermal deformation process stated, and is evacuated to 10-4Pa is re-filled with a small amount of Ar gas as protection
Gas.
9. the system of the nanocrystalline complex phase Nd-Fe-B permanent magnet texturing enhancing as described in any claim in claim 1 to 8
Preparation Method, it is characterized in that:The low-melting alloy phase containing rare earth element is adulterated in the neodymium iron boron two-phase composite permanent-magnetic material.
10. the preparation method of nanocrystalline complex phase Nd-Fe-B permanent magnet texturing enhancing as claimed in claim 9, it is characterized in that:
The quality of the doped alloys accounts for the 1%~10% of neodymium iron boron two-phase composite permanent-magnetic material quality, and further preferably 2%~8%.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109473248A (en) * | 2018-11-21 | 2019-03-15 | 重庆科技学院 | A kind of NdCeFeB anisotropic permanent magnet and preparation method thereof |
CN111554504A (en) * | 2020-05-26 | 2020-08-18 | 北京大学 | Nano-scale textured rare earth permanent magnet material and preparation method thereof |
CN113996791A (en) * | 2021-09-27 | 2022-02-01 | 宁波金鸡强磁股份有限公司 | Manufacturing method of high-performance hot-pressing neodymium-iron-boron magnet ring |
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CN102982995A (en) * | 2012-12-17 | 2013-03-20 | 湖南航天工业总公司 | Microwave curing process of bonded NdFeB magnet |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109473248A (en) * | 2018-11-21 | 2019-03-15 | 重庆科技学院 | A kind of NdCeFeB anisotropic permanent magnet and preparation method thereof |
CN111554504A (en) * | 2020-05-26 | 2020-08-18 | 北京大学 | Nano-scale textured rare earth permanent magnet material and preparation method thereof |
CN113996791A (en) * | 2021-09-27 | 2022-02-01 | 宁波金鸡强磁股份有限公司 | Manufacturing method of high-performance hot-pressing neodymium-iron-boron magnet ring |
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