CN109659108B - NdFeB material prepared by HDDR and preparation method thereof - Google Patents

NdFeB material prepared by HDDR and preparation method thereof Download PDF

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CN109659108B
CN109659108B CN201811556533.2A CN201811556533A CN109659108B CN 109659108 B CN109659108 B CN 109659108B CN 201811556533 A CN201811556533 A CN 201811556533A CN 109659108 B CN109659108 B CN 109659108B
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hddr
iron boron
neodymium iron
metal
temperature
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CN109659108A (en
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刘荣明
刘冬
熊君
张康
周小文
刘辉
王倩
贾立颖
李炳山
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Bgrimm Technology Co ltd
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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
    • H01F1/0573—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 obtained by reduction or by hydrogen decrepitation or embrittlement
    • 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

Abstract

The invention relates to the technical field of neodymium iron boron materialsIn particular to a neodymium iron boron material prepared by HDDR and a preparation method thereof. The method comprises the following steps: in at% by Nd13Fe(75‑Y)CoYB6.4ZrXZn(5.6‑X)According to the proportion, metal neodymium, iron, ferroboron, electrolytic cobalt, metal zirconium and metal zinc are mixed, melted under the protection of argon, cast to obtain an alloy ingot, and the alloy ingot is crushed to prepare a rapid hardening casting sheet; under the protection of argon, the rapid-hardening casting sheet is subjected to heat treatment at the temperature of 900-1000 ℃ for 1-2 h; after the heat treatment, carrying out HDDR treatment on the rapid-hardening casting sheet to obtain a neodymium iron boron material; wherein, X is 1.5-3.2, Y is 14-15. According to the invention, through adjusting appropriate raw materials and process conditions of various steps of HDDR, a long-time homogenization heat treatment is not required in advance, the neodymium iron boron material with excellent performance can be obtained, and the production efficiency is improved.

Description

NdFeB material prepared by HDDR and preparation method thereof
Technical Field
The invention relates to the technical field of neodymium iron boron materials, in particular to a neodymium iron boron material prepared by HDDR and a preparation method thereof.
Background
The Hydrogenation-disproportionation-dehydrogenation-Recombination (HDDR) process is a practical method for preparing anisotropic neodymium iron boron magnetic powder. The use of the HDDR process converts coarse grains of the original master alloy into a large number of sub-micron fine grains of about 0.3 μm average grain size, which is close to Nd in size2Fe14B-phase single magnetic domain size and aligned uniformly along the easy magnetization axis direction of the original master alloy crystal grains, so that the magnetic powder particles exhibit high outward appearanceAnisotropy is observed.
However, in the conventional HDDR process, the HDDR process needs to be performed after about 24 heat treatments at 1100-1200 ℃, which consumes a lot of time and energy.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a method for preparing a neodymium iron boron material by HDDR, the method for preparing the neodymium iron boron material can obtain the neodymium iron boron material with excellent performance by adjusting appropriate raw materials and process conditions of various steps of HDDR without long-time homogenization heat treatment in advance, and the production efficiency is improved.
The second purpose of the invention is to provide the HDDR neodymium iron boron material prepared by the method for preparing the neodymium iron boron material by HDDR.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
a method for preparing a neodymium iron boron material by HDDR comprises the following steps:
(a) in at% by Nd13Fe(75-Y)CoYB6.4ZrXZn(5.6-X)According to the proportion, metal neodymium, iron, ferroboron, electrolytic cobalt, metal zirconium and metal zinc are mixed, melted under the protection of argon, and cast to obtain an alloy ingot; crushing the alloy cast ingot to prepare a rapid hardening cast piece;
(b) under the protection of argon, the rapid-hardening casting sheet is subjected to heat treatment at the temperature of 900-1000 ℃ for 1-2 h;
(c) after the heat treatment, carrying out HDDR treatment on the rapid-hardening casting sheet to obtain a neodymium iron boron material;
wherein, X is 1.5-3.2, Y is 14-15.
According to the invention, the proportion of neodymium iron boron raw materials is adjusted, specific amounts of zirconium and zinc are doped in the neodymium iron boron raw materials, a Zr-rich phase exists in the materials due to the addition of zirconium, a certain amount of Zr is dissolved in an Nd-rich phase and a B-rich phase and mainly distributed in an intercrystalline region, part of Zr enters the main phase, the main phase is stabilized, the disproportionation and decomposition of the main phase are inhibited, the undecomposed main phase particles become grains with the preferred nucleation and growth of the main phase grains in the dehydrogenation and recombination process, and the recombined grains are oriented and arranged, so that the magnetic performance is improved; the zinc is added to form a binary or ternary phase with Nd and Fe to form a nonmagnetic grain boundary phase, so that the main phase is magnetically decoupled, the coercivity is improved, the growth of main phase grains is inhibited, and the easily corroded Nd-rich phase is partially replaced, so that the corrosion resistance is improved.
The synergistic addition of zirconium and zinc can ensure that the vigor of preferred nucleation and growth is kept in the dehydrogenation and recombination process, and the orientation arrangement of the recombined crystal grains is promoted, so that the magnetic performance is improved; meanwhile, the growth of main phase crystal grains is inhibited, and the coercive force and remanence are improved. And, the neodymium iron boron material has an excellent curie temperature.
Meanwhile, the rapid-hardening casting piece is used as a raw material, so that the alloy is in a supercooled state, the precipitation of α -Fe is fundamentally inhibited, α -Fe can be eliminated to the maximum extent, and the rapid-hardening casting piece is fine in crystal grains and uniform in structure.
The addition of zirconium and zinc is proved by the inventor through a large number of experiments, the magnetic performance of the neodymium iron boron can be optimized at the addition, if the addition of zirconium or zinc is too small, the performance cannot be realized, and if the addition of zinc is too large, the negative effect is achieved, for example, if excessive zinc is added, the excessive zinc is locally dissolved in the main phase to replace Fe, so that the saturation magnetization of the main phase is reduced; or excessive zirconium addition may produce non-magnetic boride phases in grain boundaries or grains, leading to a decrease in the volume fraction of the main phase, and the like.
The addition amount of the zirconium and the zinc is in the range, the addition amount of the zirconium and the zinc is 1.5 to 3.2 percent in terms of at percent, and the addition amount of the Zn is 2.4 to 4.1 percent; as in the different examples, Zr may be added in an amount of 1.5, 1.6, 1.7, 1.8, 1.9, 2.0, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, 3.0, 3.1, 3.2, etc., and correspondingly Zn may be added in an amount of 4.1, 4.0, 3.9, 3.8, 3.7, 3.6, 3.5, 3.4, 3.3, 3.2, 3.1, 3.0, 2.9, 2.8, 2.7, 2.6, 2.5, 2.4, etc.
Preferably, in said step (a), in at%, by Nd13Fe(60.2-60.8)Co(14.2-14.8)B6.4Zr(2.1-2.9)Zn(2.7-3.5)The proportion of the metal is neodymium, iron, ferroboron, electrolytic cobalt, metal zirconium and metal zinc.
It is preferable thatIn said step (a), in at% by Nd13Fe60.5Co14.5B6.4Zr2.6Zn3The proportion of the metal is neodymium, iron, ferroboron, electrolytic cobalt, metal zirconium and metal zinc.
Preferably, in the step (b), the temperature is raised to 900-1000 ℃ at a temperature raising rate of 50-60 ℃/min for heat treatment for 1-2h under the protection of argon.
According to the invention, through raw material regulation and control, a rapid-hardening casting sheet without α -Fe is adopted, and zinc and zirconium are doped in a matching manner, so that long-time heat preservation homogenization treatment is not needed, the magnetic performance is improved from the aspect of composition, the process cost is saved, and the efficiency is improved.
Preferably, the method for HDDR treatment includes the following steps:
(c1) after heat treatment, the rapid-hardening casting sheet absorbs hydrogen and is crushed, the rapid-hardening casting sheet is heated to 700-750 ℃ under the vacuum condition, hydrogen with 0.1-0.2MPa is introduced, and the hydrogen is absorbed and disproportionated for 2-3 h;
(c2) reducing the hydrogen partial pressure to 0.01-0.02MPa, and maintaining the hydrogen partial pressure for 0.5-1h at the temperature of 850 ℃;
(c3) cooling to 750--2Pa dehydrogenating for 1-2h, filling argon, and cooling to room temperature to obtain the neodymium iron boron material.
Preferably, in the step (c2), the temperature is raised to 800-850 ℃ at a speed of 1-20 ℃/min.
Preferably, in the step (c2), the hydrogen partial pressure is reduced to 0.01-0.02MPa, the temperature is raised to 800 ℃ at 5-8 ℃, and then the temperature is raised to 850 ℃ at 15-20 ℃/min, and the temperature is maintained for 0.5-1 h.
Preferably, the neodymium iron boron material is ultrasonically dispersed in a solution containing a silane coupling agent for coupling pretreatment, dried, mixed with epoxy resin and an auxiliary agent, applied with an oriented magnetic field, pressed, molded and cured.
Preferably, the dosage of the silane coupling agent is 1-2% of the mass of the neodymium iron boron material.
Preferably, the epoxy resin includes one or more of bisphenol a type epoxy resin, phenol formaldehyde type epoxy resin, o-phenol formaldehyde type polyepoxy resin, resorcinol type epoxy resin, tetraphenol ethane type epoxy resin and W-6C epoxy resin glue.
Preferably, the adjuvant comprises a curing agent. More preferably, the curing agent comprises one or more of aliphatic amine, alicyclic amine, aromatic amine, polyamide, tertiary amine and dicyandiamide curing agents.
Preferably, the curing condition is curing at 170-180 ℃ for 1-2 h.
The invention also provides the neodymium iron boron material prepared by the method for preparing the neodymium iron boron material by adopting the HDDR. The neodymium iron boron material has excellent magnetic property.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the method for preparing the neodymium iron boron material by HDDR, the neodymium iron boron material with excellent performance can be obtained by adjusting appropriate raw materials and process conditions of all steps of HDDR without carrying out homogenization heat treatment for a long time in advance, and the production efficiency is improved;
(2) meanwhile, a rapid hardening casting sheet is adopted as the raw material, so that the alloy is in a supercooled state, the precipitation of α -Fe is fundamentally inhibited, α -Fe can be eliminated to the greatest extent, and the neodymium iron boron material has fine crystal grains and uniform structure;
(3) the neodymium iron boron material prepared by the preparation method has excellent magnetic property.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following detailed description, but those skilled in the art will understand that the following described examples are some, not all, of the examples of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The partial reagent information related to the invention is as follows:
metal neodymium: the purity is 99 percent;
industrial pure iron: the purity is 99.9%;
b, iron and boron: boron content of 22% and iron content of 78%;
electrolyzing cobalt with the purity of 99.8 percent;
metal zirconium: the purity is 99.9%;
metal zinc: the purity is 99.9%.
Example 1
The embodiment provides a method for preparing a neodymium iron boron material by HDDR, which comprises the following steps:
(1) in at% by Nd13Fe60.5Co14.5B6.4Zr2.6Zn3The alloy ingot is prepared by the steps of proportioning metal neodymium, iron, ferroboron, electrolytic cobalt, metal zirconium and metal zinc, uniformly mixing, putting into a vacuum induction furnace, smelting under the protection of argon, and casting to obtain an alloy ingot; then crushing the alloy cast ingot, carrying out induction heating melting in a quartz tube of a rapid-hardening casting sheet preparation device under a vacuum condition, casting the alloy cast ingot on a copper roller with a roller surface linear speed of 5m/s and high-speed rotation under the action of 0.08MPa of injection pressure to form a rapid-hardening casting sheet with the thickness of about 0.25mm, and crushing the rapid-hardening casting sheet into a sheet with the length of 1-5 mm;
(2) heating the rapid-hardening casting sheet obtained in the step (1) to 950 ℃ at a heating rate of 55 ℃/min under the protection of argon, and carrying out heating treatment for 1.5 h;
(3) after the heat treatment in the step (2), performing HDDR treatment, specifically:
(31) sanding the rapidly solidified casting sheet after heat treatment to remove a surface oxide layer, and carrying out hydrogen absorption treatment for 2h at the hydrogen pressure of 0.3MPa and the temperature of 200 ℃; then placing the mixture in an HDDR furnace, heating the mixture to 750 ℃ under a vacuum condition, introducing 0.15MPa hydrogen, and preserving heat and pressure for 2.5 hours to finish the hydrogen absorption disproportionation process;
(32) reducing the hydrogen partial pressure to 0.015MPa, raising the temperature to 800 ℃ at the temperature rise rate of 5 ℃/min, raising the temperature to 850 ℃ at the temperature rise rate of 15 ℃/min, and preserving the heat and the pressure for 30 min;
(33) cooling to 750 deg.C, and vacuumizing to less than or equal to 10 deg.C-2Pa dehydrogenation is carried out for 2h, argon is filled, and the neodymium iron boron material is obtained after cooling to room temperature.
Example 2
This example refers to the preparation of example 1, with the only difference that: in at% by Nd13Fe60.2Co14.8B6.4Zr2.1Zn3.5The proportion of the metal is neodymium, iron, ferroboron, electrolytic cobalt, metal zirconium and metal zinc.
Example 3
This example refers to the preparation of example 1, with the only difference that: in at% by Nd13Fe60.8Co14.2B6.4Zr2.9Zn2.7The proportion of the metal is neodymium, iron, ferroboron, electrolytic cobalt, metal zirconium and metal zinc.
Example 4
This example refers to the preparation of example 1, with the only difference that: in at% by Nd13Fe60Co15B6.4Zr1.5Zn4.1The proportion of the metal is neodymium, iron, ferroboron, electrolytic cobalt, metal zirconium and metal zinc.
Example 5
This example refers to the preparation of example 1, with the only difference that: in at% by Nd13Fe61Co14B6.4Zr3.2Zn2.4The proportion of the metal is neodymium, iron, ferroboron, electrolytic cobalt, metal zirconium and metal zinc.
Example 6
This example refers to the preparation of example 1, with the only difference that: in the step (3), the HDDR processing includes:
(31) sanding the rapidly solidified casting sheet after heat treatment to remove a surface oxide layer, and carrying out hydrogen absorption treatment for 2h at the hydrogen pressure of 0.3MPa and the temperature of 200 ℃; then placing the mixture in an HDDR furnace, heating the mixture to 750 ℃ under a vacuum condition, introducing 0.15MPa hydrogen, and preserving heat and pressure for 2.5 hours to finish the hydrogen absorption disproportionation process;
(32) reducing the hydrogen partial pressure to 0.015MPa, raising the temperature to 850 ℃ at the heating rate of 5 ℃/min, and keeping the temperature and the pressure for 30 min;
(33) cooling to 750 deg.C, and vacuumizing to less than or equal to 10 deg.C-2Pa dehydrogenation is carried out for 2h, argon is filled, and the neodymium iron boron material is obtained after cooling to room temperature.
Example 7
This example refers to the preparation of example 1, with the only difference that: in the step (3), the HDDR processing includes:
(31) sanding the rapidly solidified casting sheet after heat treatment to remove a surface oxide layer, and carrying out hydrogen absorption treatment for 2h at the hydrogen pressure of 0.3MPa and the temperature of 200 ℃; then placing the mixture in an HDDR furnace, heating the mixture to 750 ℃ under a vacuum condition, introducing 0.15MPa hydrogen, and preserving heat and pressure for 2.5 hours to finish the hydrogen absorption disproportionation process;
(32) reducing the hydrogen partial pressure to 0.015MPa, raising the temperature to 800 ℃ at a temperature rise rate of 15 ℃/min, raising the temperature to 850 ℃ at a temperature rise rate of 5 ℃/min, and preserving heat and pressure for 30 min;
(33) cooling to 750 deg.C, and vacuumizing to less than or equal to 10 deg.C-2Pa dehydrogenation is carried out for 2h, argon is filled, and the neodymium iron boron material is obtained after cooling to room temperature.
Example 8
This example refers to the preparation of example 1, with the only difference that: in the step (2), the rapid-hardening casting sheet obtained in the step (1) is heated to 950 ℃ at a heating rate of 30 ℃/min under the protection of argon, and is subjected to heating treatment for 1.5 h.
Example 9
The method for preparing the neodymium iron boron material by HDDR described in this embodiment adopts the neodymium iron boron material prepared in embodiments 1 to 8, and bonds the neodymium iron boron material with epoxy resin and the like, and takes embodiment 1 as an example to specifically describe the following steps:
placing the neodymium iron boron material prepared in the embodiment 1 in an acetone solution containing a silane coupling agent (KH570) for coupling treatment in an ultrasonic dispersion mode, wherein the mass of the silane coupling agent is 2% of that of the neodymium iron boron material, uniformly mixing and dispersing, and collecting and drying the material;
100g of neodymium iron boron material subjected to coupling treatment, 3g of bisphenol A epoxy resin and 0.2g of dicyandiamide curing agent are mixed, after uniform mixing, a 2.5T oriented magnetic field is applied, after orientation is completed, compression molding is carried out under the pressure of 1000MPa, and then curing is carried out for 2h at 180 ℃ to obtain the magnet prepared from the neodymium iron boron material.
Comparative example 1
Comparative example 1 the preparation process of example 1 was referenced, with the following differences: in at% by Nd13Fe70Co5B6.4Zr4Zn1.6The proportion of the metal is neodymium, iron, ferroboron, electrolytic cobalt, metal zirconium and metal zinc.
Comparative example 2
Comparative example 2 the preparation process of example 1 was referenced, with the following differences: in at% by Nd13Fe60.5Co14.5B6.4Zr5.6The proportion of the alloy is that metal neodymium, iron, ferroboron, electrolytic cobalt and metal zirconium are mixed.
Comparative example 3
Comparative example 3 the preparation process of example 1 was referenced, with the following differences: in at% by Nd13Fe60.5Co14.5B6.4Zn5.6The proportion of the alloy is that metal neodymium, iron, ferroboron, electrolytic cobalt and metal zinc are mixed.
Comparative example 4
Comparative example 4 the preparation process of example 1 was referenced, with the following differences: in at% by Nd13Fe60.5Co14.5B6.4Zr4Zn1.6The proportion of the metal is neodymium, iron, ferroboron, electrolytic cobalt, metal zirconium and metal zinc.
Experimental example 1
In order to illustrate the performance of the neodymium iron boron material prepared in each embodiment and comparative example of the invention in a comparative way, the neodymium iron boron material prepared in each embodiment and comparative example is prepared by referring to the preparation method of embodiment 9, a magnet is prepared and is saturated and magnetized by a 5.5T pulse magnetic field, and referring to GB/T3217-.
TABLE 1 magnetic Performance test results for different Nd-Fe-B materials
Figure BDA0001912070620000091
Figure BDA0001912070620000101
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (14)

1. A method for preparing a neodymium iron boron material by HDDR is characterized by comprising the following steps:
(a) in at% by Nd13Fe(75-Y)CoYB6.4ZrXZn(5.6-X)According to the proportion, metal neodymium, iron, ferroboron, electrolytic cobalt, metal zirconium and metal zinc are mixed, melted under the protection of argon, and cast to obtain an alloy ingot; crushing the alloy cast ingot to prepare a rapid hardening cast piece;
(b) under the protection of argon, the rapid-hardening casting sheet is subjected to heat treatment at the temperature of 900-1000 ℃ for 1-2 h;
(c) after the heat treatment, carrying out HDDR treatment on the rapid-hardening casting sheet to obtain a neodymium iron boron material;
wherein, X is 1.5-3.2, Y is 14-15.
2. The method for preparing NdFeB Material by HDDR of claim 1, wherein in step (a), at% Nd13Fe(60.2-60.8)Co(14.2-14.8)B6.4Zr(2.1-2.9)Zn(2.7-3.5)The proportion of the metal is neodymium, iron, ferroboron, electrolytic cobalt, metal zirconium and metal zinc.
3. The method for preparing NdFeB Material by HDDR of claim 1, wherein in step (a), at% Nd13Fe60.5Co14.5B6.4Zr2.6Zn3The proportion of the metal is neodymium, iron, ferroboron, electrolytic cobalt, metal zirconium and metal zinc.
4. The method for preparing NdFeB material by HDDR as claimed in claim 1, wherein in step (b), the temperature is raised to 900-1000 ℃ at a temperature raising rate of 50-60 ℃/min for 1-2h under the protection of argon.
5. The method of HDDR preparation of ndfeb material as claimed in claim 1 wherein the method of HDDR treatment comprises the steps of:
(c1) after heat treatment, the rapid-hardening casting sheet absorbs hydrogen and is crushed, the rapid-hardening casting sheet is heated to 700-750 ℃ under the vacuum condition, hydrogen with 0.1-0.2MPa is introduced, and the hydrogen is absorbed and disproportionated for 2-3 h;
(c2) reducing the hydrogen partial pressure to 0.01-0.02MPa, and maintaining the hydrogen partial pressure for 0.5-1h at the temperature of 850 ℃;
(c3) cooling to 750--2Pa dehydrogenating for 1-2h, filling argon, and cooling to room temperature to obtain the neodymium iron boron material.
6. The method for preparing NdFeB material by HDDR as claimed in claim 5, wherein in the step (c2), the temperature is raised to 800-850 ℃ at 1-20 ℃/min.
7. The method for preparing NdFeB Material by HDDR of claim 6, wherein in the step (c2), the partial pressure of hydrogen is reduced to 0.01-0.02MPa, and after the temperature is raised to 800 ℃ at 5-8 ℃/min, the temperature is raised to 850 ℃ at 15-20 ℃/min, and the temperature is maintained for 0.5-1 h.
8. The method for preparing NdFeB materials by HDDR according to claim 1, wherein the NdFeB materials are ultrasonically dispersed in a solution containing silane coupling agent for coupling pretreatment, dried, mixed with epoxy resin and auxiliary agent, applied with an orientation magnetic field, pressed, molded and cured.
9. The method for preparing NdFeB materials by HDDR of claim 8, wherein the amount of silane coupling agent is 1-2% of the mass of NdFeB material.
10. The method of HDDR preparation of neodymium iron boron materials of claim 8, wherein the epoxy resin comprises one or more of bisphenol a type epoxy resin, phenol formaldehyde type epoxy resin, ortho phenol formaldehyde type polyepoxy resin, resorcinol type epoxy resin, tetraphenol ethane type epoxy resin and W-6C epoxy glue.
11. The method for preparing neodymium iron boron materials by HDDR of claim 8, wherein the additive includes a curing agent.
12. The HDDR method of producing a neodymium iron boron material of claim 11, wherein the curing agent comprises one or more of aliphatic amine, alicyclic amine, aromatic amine, polyamide, tertiary amine and dicyandiamide curing agents.
13. The method for preparing NdFeB materials by HDDR as claimed in claim 12, wherein the curing condition is 170 ℃ and 180 ℃ for 1-2 h.
14. The neodymium iron boron material prepared by the method for preparing neodymium iron boron material by HDDR as claimed in any one of claims 1-13.
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