CN117153511A - High-performance sintered NdFeB magnet material and preparation method thereof - Google Patents

High-performance sintered NdFeB magnet material and preparation method thereof Download PDF

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CN117153511A
CN117153511A CN202311078740.2A CN202311078740A CN117153511A CN 117153511 A CN117153511 A CN 117153511A CN 202311078740 A CN202311078740 A CN 202311078740A CN 117153511 A CN117153511 A CN 117153511A
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alloy
powder
iron
neodymium
temperature
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赵浩峰
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Anhui Institute of Information Engineering
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Anhui Institute of Information Engineering
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys 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
    • H01F1/0575Alloys 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
    • H01F1/0577Alloys 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 sintered
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/02Apparatus 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
    • H01F41/0253Apparatus 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
    • H01F41/0293Apparatus 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)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)

Abstract

The application discloses a high-performance sintered NdFeB magnet material and a preparation method thereof, which relate to the field of permanent magnet materials and comprise the following steps: s1, mixing materials according to the mass ratio of the magnetic composite material alloy material neodymium iron boron powder, copper alloy powder and iron silicon powder of 1:0.05-0.10:0.03-0.09, and adding the materials into a three-dimensional mixer to mix to obtain powder; s2, filling the mixed powder into a forming die, wherein the temperature of the materials in the die and a die cavity is not more than 30 ℃; s3, orienting the mixed powder in a magnetic field press, wherein the strength of an oriented magnetic field applied by compression molding is 2.0T, the pressure is 150KN, and the pressure is maintained for 15S; s4, placing the molded blank into a sintering furnace under the protection of argon gas for sintering; and S5, carrying out tempering treatment twice on the sintered molded blank, and then carrying out aging treatment to obtain the high-performance sintered neodymium-iron-boron magnet material. The cyclone separation equipment has high separation efficiency, and the sintered neodymium-iron-boron magnet has high coercive force and high comprehensive magnetism.

Description

High-performance sintered NdFeB magnet material and preparation method thereof
Technical Field
The application mainly relates to the technical field of permanent magnet materials, in particular to a high-performance sintered NdFeB magnet material and a preparation method thereof.
Background
The sintered NdFeB permanent magnet material is a permanent magnet material based on an intermetallic compound ND2FE 14B.
Compared with other permanent magnetic materials, the sintered NdFeB permanent magnet has outstanding magnetic performance advantages. It has extremely high magnetic energy product, coercive force and energy density, and has good mechanical properties and easy processing. The excellent performances enable the sintered NdFeB permanent magnet to be widely applied in modern industry and electronic technology, and widely applied to the fields of electronics, electric machinery, medical equipment, toys, packaging, hardware machinery, aerospace and the like, and more common permanent magnet motors, speakers, magnetic separators, computer disk drives, magnetic resonance imaging equipment meters and the like.
The prior art CN201910765838.2 discloses a preparation method of a high-performance sintered NdFeB magnet, which comprises the following steps: (1) Preparing raw materials according to the composition components of the sintered NdFeB magnet to be finally obtained; (2) Raw materials are put into smelting equipment for alloy smelting, and a neodymium iron boron alloy sheet is obtained; (3) Carrying out hydrogen absorption crushing treatment on the neodymium iron boron alloy sheet, and carrying out half dehydrogenation after crushing to obtain neodymium iron boron coarse powder; (4) Carrying out air current grinding on the neodymium iron boron coarse powder at low temperature, and then carrying out secondary cyclone separation to obtain neodymium iron boron fine powder with uniform particle size distribution; (5) molding the neodymium iron boron fine powder at low temperature; and (6) finally, sintering and heat treatment are carried out to obtain the target product.
When the prior art separates coarse powder through a cyclone separator, the air inlet of the prior separator is directly communicated with a separating cylinder, and because the inside of the separator is not provided with a flow guiding structure, the internal air flow is easy to collide, the centrifugal force is small, and the separation efficiency is low; and the coercivity of the sintered NdFeB magnet in the prior art needs to be improved, and the comprehensive magnetic performance is not high.
Disclosure of Invention
Based on the above, the present application aims to provide a high-performance sintered neodymium-iron-boron magnet material and a preparation method thereof, so as to solve the technical problems set forth in the above background art.
In order to achieve the above purpose, the present application provides the following technical solutions:
the high-performance sintered neodymium-iron-boron magnet material is formed by combining and sintering neodymium-iron-boron powder, copper alloy powder and iron silicon powder, wherein the mass ratio of the neodymium-iron-boron powder to the copper alloy powder to the iron silicon powder is 1:0.05-0.10:0.03-0.09.
The technical scheme is that the neodymium iron boron powder is prepared by the following steps: the alloy is prepared from 99.5wt% of metal neodymium Nd, 99.5wt% of metal iron Fe, 99.5wt% of metal cerium Ce, 99.5wt% of metal nickel Ni, 99.5wt% of metal tin Sn, 80wt% of gadolinium Gd content gadolinium iron alloy and 22% of boron B content ferroboron alloy serving as raw materials according to the mass ratio Nd: gd: fe: ni: ce: sn: b=25-28: 4-6:60-65:1-3:3-6:0.3-0.6:1-3, and weighing the raw materials.
According to the technical scheme, the proportioned neodymium iron boron powder raw materials are put into smelting equipment to be subjected to alloy smelting, and a neodymium iron boron alloy sheet is obtained through rotation of a molybdenum roller; wherein the rotating speed of the molybdenum roller during alloy smelting is 1.3-1.7m/s, and the casting temperature is 1480-1530 ℃; carrying out normal dehydrogenation treatment on the powder in the hydrogen crushing process to obtain neodymium iron boron coarse powder, and controlling the hydrogen content in the neodymium iron boron coarse powder to be 940-980ppm; cooling the air flow grinding chamber, the carrier gas and the neodymium iron boron coarse powder, wherein the temperature of the air flow grinding chamber is 20 ℃, the temperature of the carrier gas is 15 ℃, the temperature of the neodymium iron boron coarse powder is 20-25 ℃, and the temperature of the grinding chamber and the temperature of the material are maintained to be less than or equal to 38 ℃ in the air flow grinding treatment process; and carrying out secondary cyclone separation on the material subjected to the air current grinding through cyclone separation equipment to obtain neodymium iron boron powder with the particle size distribution of 3.2-3.7 mu m.
According to the technical scheme, the cyclone separation equipment comprises a separation cylinder, the separation cylinder is in a cylindrical structure with a large top and a small bottom, a spiral air inlet pipe is connected to the outer wall of one side of the top of the separation cylinder in a penetrating mode, a guide cylinder penetrates through the top of the separation cylinder, and a spiral guide plate is connected to the outer circumferential wall of the guide cylinder in a spiral downward rotating mode.
According to the technical scheme, the top of the spiral guide plate is close to the airflow inlet of the spiral air inlet pipe and corresponds to the airflow direction of the spiral air inlet pipe.
The technical scheme is that the copper alloy powder is prepared by the following steps: taking waste materials of HMn62-3-3-1 alloy, putting the waste materials into a melting furnace for melting, adding other elements Zn, fe and P into the melting furnace, wherein the melting temperature is 1200-1280 ℃, and then casting the alloy ingot into alloy ingots, wherein the obtained alloy ingots comprise the following components: 61-63% of Cu, 0.5-1.3% of Fe, 0.2-0.6% of Pb, 2.2-3.8% of Si, 0.01-0.03% of P, less than 0.6% of Ni and the balance of zinc.
The technical scheme is that the alloy ingot is placed into an induction furnace crucible, a diameter of 1-2mm is arranged at a bottom hole of the crucible, when alloy in the crucible is melted, the alloy can flow out under the action of nitrogen pressure, the alloy is just contacted with a rotating molybdenum alloy rotating wheel arranged at the lower part of the bottom hole of the crucible to form a strip casting, the melting temperature is 650-690 ℃, the temperature is kept for 4-8min after melting, the nitrogen pressure is 1.0-1.3 atm, the linear speed of the edge of the molybdenum alloy rotating wheel is 24-26m/s, then the alloy strip is heated to 300-320 ℃ for 20-30 min, the alloy strip is taken out and placed into an environment of minus 50-60 ℃ directly, the temperature is kept for 20-30 min, and then the alloy strip is placed into a ball mill to be crushed into copper alloy powder with 20-30 microns of granularity for standby.
The technical scheme is that the preparation of the ferrosilicon powder comprises the following steps: melting pure iron scraps in an induction furnace, adding silicon during melting at 1650-1700 ℃, and casting into alloy ingots, wherein the obtained iron ingots comprise the following components: si is 0.4% -0.9% and the balance is Fe.
The technical scheme is that the alloy ingot is placed into a crucible of an induction furnace, a diameter of 1-2mm is arranged at a bottom hole of the crucible, when alloy in the crucible is melted, the alloy can flow out under the action of nitrogen pressure, the alloy is just contacted with a rotating molybdenum alloy rotating wheel arranged at the lower part of the bottom hole of the crucible to form a strip casting, the melting temperature is 1650-1690 ℃, the temperature is kept for 4-8min after melting, the nitrogen pressure is 1.0-1.2 atm, the linear speed of the edge of the molybdenum alloy rotating wheel is 22-24m/s, then an alloy strip is heated to 320-350 ℃ for 20-30 min, the alloy strip is taken out and then placed into an environment of minus 60-70 ℃ for 20-40 min, and the alloy strip is placed into a ball mill to be crushed into iron silicon powder with 20-30 microns of granularity for standby.
According to the technical scheme of the high-performance sintered NdFeB magnet material, the preparation method of the high-performance sintered NdFeB magnet is provided, and comprises the following steps:
s1, mixing materials according to the mass ratio of the magnetic composite material alloy material neodymium iron boron powder, copper alloy powder and iron silicon powder of 1:0.05-0.10:0.03-0.09, and adding the materials into a three-dimensional mixer to uniformly mix to obtain mixed powder;
s2, filling the mixed powder into a forming die, wherein the temperature of the materials in the die and a die cavity is not more than 30 ℃;
s3, orienting the mixed powder in a magnetic field press, performing compression molding, wherein the strength of an oriented magnetic field applied during compression molding is 2.0T, the pressure is 150KN, and the pressure is maintained for 15S;
s4, placing the molded blank into a sintering furnace under the protection of argon gas for sintering, firstly heating to 600-700 ℃, preserving heat for 3-4 hours, then heating to 1080-1180 ℃ for sintering for 3 hours, and cooling to room temperature;
s5, carrying out tempering treatment twice on the sintered molded blank, and then carrying out aging treatment to obtain a high-performance sintered neodymium-iron-boron magnet material; the primary tempering temperature is 900-910 ℃, and the heat preservation time is 2-3 hours; the secondary tempering temperature is 500-560 ℃, the time is 1-3h, the aging treatment temperature is 210 ℃, and the heat preservation time is 25h.
In summary, the application has the following advantages:
1. aiming at the problems in the background art, the application improves the coarse powder separation efficiency through cyclone separation equipment, guides the air flow downwards through arranging the guide column in the separation cylinder, improves the speed of guiding the air flow downwards through arranging the spiral guide plate spirally downwards on the outer circumferential wall of the guide column in the separation cylinder, ensures that the air flow in the separation cylinder can not collide, generates larger centrifugal force when rotating in the cylinder body of the separation cylinder, ensures larger quality and density of neodymium iron boron coarse powder in the air flow, ensures larger centrifugal force, and rotates and throws the air flow towards the cylinder wall under the action of the centrifugal force to separate the air flow, thereby having high separation efficiency;
2. the high-performance sintered NdFeB magnet material is prepared from NdFeB powder, copper alloy powder and iron-silicon raw materials; the Nd-Fe-B magnetic material is composed of a main phase, an Nd-rich phase and a B-rich phase, wherein the Nd-rich phase can inhibit grain growth, promote the improvement of coercive force, and rare earth Nd, gd and Ce in elements can form a primary main phase, a secondary main phase and a tertiary main phase, the main phase is a magnetic phase in an alloy, the excellent magnetic performance of the Nd-Fe-B magnetic material is mainly due to the high saturation magnetization and anisotropic field of the three main phases, and the Fe-Si powder is a magnetic phase, and the magnetic phase and the three main phases have mutually good mutual coordination, so that the growth of the phases in sintering is greatly inhibited; the alpha-Fe coarsens local crystal grains, the magnetism is deteriorated, if P is added, the growth of the crystal grains can be greatly prevented, the copper alloy powder can prevent the growth of the crystal grains, copper and zinc atoms on the surfaces of the neodymium-iron-boron particles gradually diffuse from the surfaces of the neodymium-iron-boron particles to the inside of the alpha-Fe during sintering, the irreversible loss of magnetic flux can be obviously reduced by adding silicon, sn and Si are dissolved in a main phase, the remanence and magnetic energy product can be improved, and the coercive force Hcj of a magnet can be obviously improved by replacing Nd by Ce.
Drawings
FIG. 1 is a schematic view of a cyclonic separating apparatus of the present application;
FIG. 2 is a schematic view of a guide column within a separator cartridge according to the present application;
FIG. 3 is a schematic view of a spiral baffle according to the present application;
FIG. 4 is a mass ratio block diagram of the formulation of the present application.
Description of the drawings: 1. a cyclone separation device; 11. a separation cylinder; 12. a spiral air inlet pipe; 13. a flow guiding column; 14. spiral deflector.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application. The embodiments described below by referring to the drawings are illustrative only and are not to be construed as limiting the application.
Hereinafter, an embodiment of the present application will be described in accordance with its entire structure.
Examples
Referring to fig. 1-4, a high-performance sintered neodymium-iron-boron magnet material is prepared by sintering neodymium-iron-boron powder, copper alloy powder and iron-silicon powder in a mass ratio of 1:0.05-0.10:0.03-0.09, wherein the raw materials of the sintered neodymium-iron-boron magnet material are as follows: the alloy is prepared from 99.5wt% of metal neodymium Nd, 99.5wt% of metal iron Fe, 99.5wt% of metal cerium Ce, 99.5wt% of metal nickel Ni, 99.5wt% of metal tin Sn, 80wt% of gadolinium Gd content gadolinium iron alloy and 22% of boron B content ferroboron alloy serving as raw materials according to the mass ratio Nd: gd: fe: ni: ce: sn: b=25-28: proportioning 4-6:60-65:1-3:3-6:0.3-0.6:1-3, weighing all raw materials, loading the proportioned neodymium iron boron powder raw materials into smelting equipment for alloy smelting, and rotating a molybdenum roller to obtain a neodymium iron boron alloy sheet; wherein the rotating speed of the molybdenum roller during alloy smelting is 1.3-1.7m/s, and the casting temperature is 1480-1530 ℃; carrying out normal dehydrogenation treatment on the powder in the hydrogen crushing process to obtain neodymium iron boron coarse powder, and controlling the hydrogen content in the neodymium iron boron coarse powder to be 940-980ppm; cooling the air flow grinding chamber, the carrier gas and the neodymium iron boron coarse powder, wherein the temperature of the air flow grinding chamber is 20 ℃, the temperature of the carrier gas is 15 ℃, the temperature of the neodymium iron boron coarse powder is 20-25 ℃, and the temperature of the grinding chamber and the temperature of the material are maintained to be less than or equal to 38 ℃ in the air flow grinding treatment process; carrying out secondary cyclone separation on the material subjected to the air current grinding through cyclone separation equipment 1 to obtain neodymium iron boron powder with the particle size distribution of 3.2-3.7 mu m; the cyclone separation equipment 1 comprises a separation cylinder 11, wherein the separation cylinder 11 is in a cylindrical structure with a large top and a small bottom, a spiral air inlet pipe 12 is connected with the outer wall of one side of the top of the separation cylinder 11 in a penetrating way, a guide column 13 is connected with the inside of the separation cylinder 11 in a penetrating way, and a spiral guide plate 14 is connected with the outer circumferential wall of the guide column 13 in the separation cylinder 11 in a spiral downward rotating way; the top of the spiral guide plate 14 is close to the airflow inlet of the spiral air inlet pipe 12 and corresponds to the airflow direction of the spiral air inlet pipe; preparing copper alloy powder: taking waste materials of HMn62-3-3-1 alloy, putting the waste materials into a melting furnace for melting, adding other elements Zn, fe and P into the melting furnace, wherein the melting temperature is 1200-1280 ℃, and then casting the alloy ingot into alloy ingots, wherein the obtained alloy ingots comprise the following components: 61-63% of Cu, 0.5-1.3% of Fe, 0.2-0.6% of Pb, 2.2-3.8% of Si, 0.01-0.03% of P, less than 0.6% of Ni and the balance of zinc; placing alloy ingots into an induction furnace crucible, wherein a diameter of 1-2mm is arranged in a bottom hole of the crucible, after alloy in the crucible is melted, the alloy can flow out under the action of nitrogen pressure, the alloy is just contacted with a rotating molybdenum alloy rotating wheel arranged at the lower part of the bottom hole of the crucible to form a melt-spun belt, the melting temperature is 650-690 ℃, the temperature is kept for 4-8min after the melting, the nitrogen pressure is 1.0-1.3 atm, the linear speed of the edge of the molybdenum alloy rotating wheel is 24-26m/s, then the alloy strips are heated to 300-320 ℃ and kept for 20-30 min, the alloy strips are taken out and then are directly placed into an environment of minus 50-minus 60 ℃, and after the temperature is kept for 20-30 min, the alloy strips are placed into a ball mill to be crushed into copper alloy powder with 20-30 microns of granularity for standby; preparing ferrosilicon powder: melting pure iron scraps in an induction furnace, adding silicon during melting at 1650-1700 ℃, and casting into alloy ingots, wherein the obtained iron ingots comprise the following components: the method comprises the steps of placing 0.4% -0.9% of Si and the balance of Fe into an induction furnace crucible, placing alloy ingots into the crucible, wherein a diameter of 1-2mm is arranged at a bottom hole of the crucible, after alloy in the crucible is melted, the alloy can flow out under the action of nitrogen pressure, the alloy is just contacted with a rotating molybdenum alloy rotating wheel arranged at the lower part of the bottom hole of the crucible to form a melt-spun strip, the melting temperature is 1650-1690 ℃, the temperature is kept for 4-8min after melting, the nitrogen pressure is 1.0-1.2 atm, the linear speed of the edge of the molybdenum alloy rotating wheel is 22-24m/s, then heating an alloy strip to 320-350 ℃, keeping the temperature for 20-30 min, taking out, directly placing the alloy strip into an environment of-60-70 ℃, keeping the temperature for 20-40 min, and placing the alloy strip into a ball mill to be crushed into iron silicon powder with the granularity of 20-30 microns for standby.
It should be noted that, in this embodiment, the cyclone separation device 1 improves the coarse powder separation efficiency, the air flow is guided downwards by arranging the guide column 12 inside the separation barrel 11, the speed of the air flow guiding downwards is improved by arranging the spiral guide plate 13 with the spiral downward on the outer circumferential wall of the guide column 12 inside the separation barrel 11, the air flow cannot collide inside the separation barrel 11, the air flow rotates inside the barrel body to generate larger centrifugal force, the quality and density of neodymium iron boron coarse powder inside the air flow are larger, the centrifugal force becomes larger, and the air flow is rotationally thrown to the barrel wall under the action of the centrifugal force to separate and the separation efficiency is high.
Referring to fig. 4, according to the above embodiment, there is further provided a method for preparing a high-performance sintered neodymium-iron-boron magnet, including the following steps:
s1, mixing materials according to the mass ratio of the magnetic composite material alloy material neodymium iron boron powder, copper alloy powder and iron silicon powder of 1:0.05-0.10:0.03-0.09, and adding the materials into a three-dimensional mixer to uniformly mix to obtain mixed powder;
s2, filling the mixed powder into a forming die, wherein the temperature of the materials in the die and a die cavity is not more than 30 ℃;
s3, orienting the mixed powder in a magnetic field press, performing compression molding, wherein the strength of an oriented magnetic field applied during compression molding is 2.0T, the pressure is 150KN, and the pressure is maintained for 15S;
s4, placing the molded blank into a sintering furnace under the protection of argon gas for sintering, firstly heating to 600-700 ℃, preserving heat for 3-4 hours, then heating to 1080-1180 ℃ for sintering for 3 hours, and cooling to room temperature;
s5, carrying out tempering treatment twice on the sintered molded blank, and then carrying out aging treatment to obtain a high-performance sintered neodymium-iron-boron magnet material; the primary tempering temperature is 900-910 ℃, and the heat preservation time is 2-3 hours; the secondary tempering temperature is 500-560 ℃, the time is 1-3h, the aging treatment temperature is 210 ℃, and the heat preservation time is 25h.
In this embodiment, the magnet prepared by orienting the powder mixture in the magnetic field press can obtain good magnetic properties;
further, the sintered molded blank is subjected to two tempering treatments to improve the toughness and flexibility of the material, wherein the primary tempering temperature is 900-910 ℃, the primary tempering is high-temperature tempering, the material has good comprehensive performance and high strength, and has good plasticity and toughness, the secondary tempering temperature is 500-560 ℃, the material is medium-high-temperature tempering, and the material has high elastic limit, yield strength and yield ratio and has plasticity and toughness at the same time;
further, after tempering, aging treatment is carried out, the sintered neodymium iron boron permanent magnet material adopts a powder metallurgy process, the smelted alloy is made into powder and pressed into a pressing blank in a magnetic field, the pressing blank is sintered in inert gas or vacuum to achieve densification, and the coercivity of the magnet is improved through aging heat treatment.
Example 1
S1, mixing materials according to the mass ratio of the magnetic composite material alloy material neodymium iron boron powder, copper alloy powder and iron silicon powder of 1:0.05:0.03, and adding the materials into a three-dimensional mixer to uniformly mix to obtain mixed powder;
s2, filling the mixed powder into a forming die, wherein the temperature of the materials in the die and a die cavity is not more than 30 ℃;
s3, orienting the mixed powder in a magnetic field press, performing compression molding, wherein the strength of an oriented magnetic field applied during compression molding is 2.0T, the pressure is 150KN, and the pressure is maintained for 15S;
s4, placing the molded blank into a sintering furnace under the protection of argon gas for sintering, firstly heating to 600-700 ℃, preserving heat for 3-4 hours, then heating to 1080-1180 ℃ for sintering for 3 hours, and cooling to room temperature;
s5, carrying out tempering treatment twice on the sintered molded blank, and then carrying out aging treatment to obtain a high-performance sintered neodymium-iron-boron magnet material; the primary tempering temperature is 900-910 ℃, and the heat preservation time is 2-3 hours; the secondary tempering temperature is 500-560 ℃, the time is 1-3h, the aging treatment temperature is 210 ℃, and the heat preservation time is 25h.
Example 2
S1, mixing materials according to the mass ratio of the magnetic composite material alloy material neodymium iron boron powder to the copper alloy powder to the iron silicon powder of 1:0.08:0.06, and adding the materials into a three-dimensional mixer to uniformly mix to obtain mixed powder;
s2, filling the mixed powder into a forming die, wherein the temperature of the materials in the die and a die cavity is not more than 30 ℃;
s3, orienting the mixed powder in a magnetic field press, performing compression molding, wherein the strength of an oriented magnetic field applied during compression molding is 2.0T, the pressure is 150KN, and the pressure is maintained for 15S;
s4, placing the molded blank into a sintering furnace under the protection of argon gas for sintering, firstly heating to 600-700 ℃, preserving heat for 3-4 hours, then heating to 1080-1180 ℃ for sintering for 3 hours, and cooling to room temperature;
s5, carrying out tempering treatment twice on the sintered molded blank, and then carrying out aging treatment to obtain a high-performance sintered neodymium-iron-boron magnet material; the primary tempering temperature is 900-910 ℃, and the heat preservation time is 2-3 hours; the secondary tempering temperature is 500-560 ℃, the time is 1-3h, the aging treatment temperature is 210 ℃, and the heat preservation time is 25h.
Example 3
S1, mixing materials according to the mass ratio of the magnetic composite material alloy material neodymium iron boron powder to the copper alloy powder to the iron silicon powder of 1:0.10:0.09, and adding the materials into a three-dimensional mixer to uniformly mix to obtain mixed powder;
s2, filling the mixed powder into a forming die, wherein the temperature of the materials in the die and a die cavity is not more than 30 ℃;
s3, orienting the mixed powder in a magnetic field press, performing compression molding, wherein the strength of an oriented magnetic field applied during compression molding is 2.0T, the pressure is 150KN, and the pressure is maintained for 15S;
s4, placing the molded blank into a sintering furnace under the protection of argon gas for sintering, firstly heating to 600-700 ℃, preserving heat for 3-4 hours, then heating to 1080-1180 ℃ for sintering for 3 hours, and cooling to room temperature;
s5, carrying out tempering treatment twice on the sintered molded blank, and then carrying out aging treatment to obtain a high-performance sintered neodymium-iron-boron magnet material; the primary tempering temperature is 900-910 ℃, and the heat preservation time is 2-3 hours; the secondary tempering temperature is 500-560 ℃, the time is 1-3h, the aging treatment temperature is 210 ℃, and the heat preservation time is 25h.
Example 4
S1, mixing materials according to the mass ratio of the magnetic composite material alloy material neodymium iron boron powder, copper alloy powder and iron silicon powder of 1:0.04:0.02, and adding the materials into a three-dimensional mixer to uniformly mix to obtain mixed powder;
s2, filling the mixed powder into a forming die, wherein the temperature of the materials in the die and a die cavity is not more than 30 ℃;
s3, orienting the mixed powder in a magnetic field press, performing compression molding, wherein the strength of an oriented magnetic field applied during compression molding is 2.0T, the pressure is 150KN, and the pressure is maintained for 15S;
s4, placing the molded blank into a sintering furnace under the protection of argon gas for sintering, firstly heating to 600-700 ℃, preserving heat for 3-4 hours, then heating to 1080-1180 ℃ for sintering for 3 hours, and cooling to room temperature;
s5, carrying out tempering treatment twice on the sintered molded blank, and then carrying out aging treatment to obtain a high-performance sintered neodymium-iron-boron magnet material; the primary tempering temperature is 900-910 ℃, and the heat preservation time is 2-3 hours; the secondary tempering temperature is 500-560 ℃, the time is 1-3h, the aging treatment temperature is 210 ℃, and the heat preservation time is 25h.
Example 5
S1, mixing materials according to the mass ratio of the magnetic composite material alloy material neodymium iron boron powder, copper alloy powder and iron silicon powder of 1:0.12:0.11, and adding the materials into a three-dimensional mixer to uniformly mix to obtain mixed powder;
s2, filling the mixed powder into a forming die, wherein the temperature of the materials in the die and a die cavity is not more than 30 ℃;
s3, orienting the mixed powder in a magnetic field press, performing compression molding, wherein the strength of an oriented magnetic field applied during compression molding is 2.0T, the pressure is 150KN, and the pressure is maintained for 15S;
s4, placing the molded blank into a sintering furnace under the protection of argon gas for sintering, firstly heating to 600-700 ℃, preserving heat for 3-4 hours, then heating to 1080-1180 ℃ for sintering for 3 hours, and cooling to room temperature;
s5, carrying out tempering treatment twice on the sintered molded blank, and then carrying out aging treatment to obtain a high-performance sintered neodymium-iron-boron magnet material; the primary tempering temperature is 900-910 ℃, and the heat preservation time is 2-3 hours; the secondary tempering temperature is 500-560 ℃, the time is 1-3h, the aging treatment temperature is 210 ℃, and the heat preservation time is 25h.
The working principle of the application is as follows:
s1, mixing materials according to the mass ratio of the magnetic composite material alloy material neodymium iron boron powder, copper alloy powder and iron silicon powder of 1:0.05-0.10:0.03-0.09, and adding the materials into a three-dimensional mixer to uniformly mix to obtain mixed powder;
s2, filling the mixed powder into a forming die, wherein the temperature of the materials in the die and a die cavity is not more than 30 ℃;
s3, orienting the mixed powder in a magnetic field press, performing compression molding, wherein the strength of an oriented magnetic field applied during compression molding is 2.0T, the pressure is 150KN, and the pressure is maintained for 15S;
s4, placing the molded blank into a sintering furnace under the protection of argon gas for sintering, firstly heating to 600-700 ℃, preserving heat for 3-4 hours, then heating to 1080-1180 ℃ for sintering for 3 hours, and cooling to room temperature;
s5, carrying out tempering treatment twice on the sintered molded blank, and then carrying out aging treatment to obtain a high-performance sintered neodymium-iron-boron magnet material; the primary tempering temperature is 900-910 ℃, and the heat preservation time is 2-3 hours; the secondary tempering temperature is 500-560 ℃, the time is 1-3h, the aging treatment temperature is 210 ℃, and the heat preservation time is 25h.
According to the cyclone separation device 1, coarse powder separation efficiency is improved, airflow is guided downwards through the guide column 12 arranged in the separation barrel 11, the downward airflow guiding speed is improved through the spiral guide plate 13 which is arranged on the outer circumferential wall of the guide column 12 in the separation barrel 11, the internal airflows cannot collide, the airflows rotate in the barrel of the separation barrel 11 to generate larger centrifugal force, the quality and density of neodymium iron boron coarse powder in the airflows are larger, the centrifugal force is larger, and the neodymium iron boron coarse powder is rotationally thrown to the barrel wall under the action of the centrifugal force to perform separation, so that the separation efficiency is high;
the high-performance sintered NdFeB magnet material is prepared from NdFeB powder, copper alloy powder and iron-silicon raw materials; the Nd-Fe-B magnetic material is composed of a main phase, an Nd-rich phase and a B-rich phase, wherein the Nd-rich phase can inhibit grain growth, promote the improvement of coercive force, and rare earth Nd, gd and Ce in elements can form a primary main phase, a secondary main phase and a tertiary main phase, the main phase is a magnetic phase in an alloy, the excellent magnetic performance of the Nd-Fe-B magnetic material is mainly due to the high saturation magnetization and anisotropic field of the three main phases, and the Fe-Si powder is a magnetic phase, and the magnetic phase and the three main phases have mutually good mutual coordination, so that the growth of the phases in sintering is greatly inhibited; the alpha-Fe coarsens local crystal grains, the magnetism is deteriorated, if P is added, the growth of the crystal grains can be greatly prevented, the copper alloy powder can prevent the growth of the crystal grains, copper and zinc atoms on the surfaces of the neodymium-iron-boron particles gradually diffuse from the surfaces of the neodymium-iron-boron particles to the inside of the alpha-Fe during sintering, the irreversible loss of magnetic flux can be obviously reduced by adding silicon, sn and Si are dissolved in a main phase, the remanence and magnetic energy product can be improved, and the coercive force Hcj of a magnet can be obviously improved by replacing Nd by Ce.
Although embodiments of the application have been shown and described, the detailed description is to be construed as exemplary only and is not limiting of the application as the particular features, structures, materials, or characteristics may be combined in any suitable manner in any one or more embodiments or examples, and modifications, substitutions, variations, etc. may be made in the embodiments as desired by those skilled in the art without departing from the principles and spirit of the application, provided that such modifications are within the scope of the appended claims.

Claims (10)

1. The high-performance sintered NdFeB magnet material is characterized in that the sintered NdFeB magnet material is formed by combining and sintering NdFeB powder, copper alloy powder and ferrosilicon powder, and the mass ratio of the NdFeB powder to the copper alloy powder to the ferrosilicon powder is 1:0.05-0.10:0.03-0.09.
2. The high-performance sintered neodymium-iron-boron magnet material according to claim 1, wherein the neodymium-iron-boron powder is prepared by: the alloy is prepared from 99.5wt% of metal neodymium Nd, 99.5wt% of metal iron Fe, 99.5wt% of metal cerium Ce, 99.5wt% of metal nickel Ni, 99.5wt% of metal tin Sn, 80wt% of gadolinium Gd content gadolinium iron alloy and 22% of boron B content ferroboron alloy serving as raw materials according to the mass ratio Nd: gd: fe: ni: ce: sn: b=25-28: 4-6:60-65:1-3:3-6:0.3-0.6:1-3, and weighing the raw materials.
3. The high-performance sintered neodymium-iron-boron magnet material according to claim 2, wherein the proportioned neodymium-iron-boron powder raw material is filled into smelting equipment for alloy smelting, and a neodymium-iron-boron alloy sheet is obtained through molybdenum roller rotation; wherein the rotating speed of the molybdenum roller during alloy smelting is 1.3-1.7m/s, and the casting temperature is 1480-1530 ℃; carrying out normal dehydrogenation treatment on the powder in the hydrogen crushing process to obtain neodymium iron boron coarse powder, and controlling the hydrogen content in the neodymium iron boron coarse powder to be 940-980ppm; cooling the air flow grinding chamber, the carrier gas and the neodymium iron boron coarse powder, wherein the temperature of the air flow grinding chamber is 20 ℃, the temperature of the carrier gas is 15 ℃, the temperature of the neodymium iron boron coarse powder is 20-25 ℃, and the temperature of the grinding chamber and the temperature of the material are maintained to be less than or equal to 38 ℃ in the air flow grinding treatment process; and carrying out secondary cyclone separation on the material subjected to the air current grinding through cyclone separation equipment (1) to obtain neodymium iron boron powder with the particle size distribution of 3.2-3.7 mu m.
4. The high-performance sintered neodymium-iron-boron magnet material according to claim 3, wherein the cyclone separation device (1) comprises a separation cylinder (11), the separation cylinder (11) is in a cylindrical structure with a large top and a small bottom, a spiral air inlet pipe (12) is connected to the outer wall of one side of the top of the separation cylinder (11) in a penetrating mode, a guide column (13) is connected to the inner portion of the separation cylinder (11) in a penetrating mode, and a spiral guide plate (14) is connected to the outer circumferential wall of the guide column (13) in a spiral downward rotating mode.
5. A high performance sintered neodymium-iron-boron magnet material according to claim 4, wherein the top of the spiral deflector (14) is close to the air inlet of the spiral air inlet pipe (12) and corresponds to the air flow direction.
6. The high-performance sintered neodymium-iron-boron magnet material according to claim 1, wherein the copper alloy powder is prepared by: taking waste materials of HMn62-3-3-1 alloy, putting the waste materials into a melting furnace for melting, adding other elements Zn, fe and P into the melting furnace, wherein the melting temperature is 1200-1280 ℃, and then casting the alloy ingot into alloy ingots, wherein the obtained alloy ingots comprise the following components: 61-63% of Cu, 0.5-1.3% of Fe, 0.2-0.6% of Pb, 2.2-3.8% of Si, 0.01-0.03% of P, less than 0.6% of Ni and the balance of zinc.
7. The high-performance sintered neodymium-iron-boron magnet material according to claim 5, wherein the alloy ingot is placed into a crucible of an induction furnace, a bottom hole of the crucible is provided with a diameter of 1-2mm, after the alloy in the crucible is melted, the alloy ingot can flow out under the action of nitrogen pressure and just contacts with a rotating molybdenum alloy rotating wheel arranged at the lower part of the bottom hole of the crucible to form a melt-spun tape, the melting temperature is 650-690 ℃, the temperature is kept for 4-8min after melting, the nitrogen pressure is 1.0-1.3 atm, the linear speed of the edge of the molybdenum alloy rotating wheel is 24-26m/s, then an alloy strip is heated to 300-320 ℃ for 20-30 min, the alloy strip is taken out and then placed into an environment of 50-60 ℃ directly, after 20-30 min of heat preservation, the alloy strip is placed into a ball mill and crushed into copper alloy powder with the granularity of 20-30 microns for standby.
8. The high-performance sintered neodymium-iron-boron magnet material according to claim 1, wherein the preparation of the ferrosilicon powder comprises the following steps: melting pure iron scraps in an induction furnace, adding silicon during melting at 1650-1700 ℃, and casting into alloy ingots, wherein the obtained iron ingots comprise the following components: si is 0.4% -0.9% and the balance is Fe.
9. The high-performance sintered neodymium-iron-boron magnet material according to claim 7, wherein the alloy ingot is placed into a crucible of an induction furnace, a bottom hole of the crucible is provided with a diameter of 1-2mm, after the alloy in the crucible is melted, the alloy ingot can flow out under the action of nitrogen pressure and just contacts with a rotating molybdenum alloy rotating wheel arranged at the lower part of the bottom hole of the crucible to form a melt-spun tape, the melting temperature is 1650-1690 ℃, the temperature is kept for 4-8min after the melting, the nitrogen pressure is 1.0-1.2 atm, the linear speed of the edge of the molybdenum alloy rotating wheel is 22-24m/s, then an alloy strip is heated to 320-350 ℃ and kept for 20-30 min, the alloy strip is taken out and is directly put into an environment of minus 60-70 ℃, and after 20-40 min of heat preservation, the alloy strip is put into a ball mill and crushed into iron silicon powder with the granularity of 20-30 microns for standby.
10. The method for preparing a high-performance sintered neodymium-iron-boron magnet according to claims 1 to 9, comprising the following steps:
s1, mixing materials according to the mass ratio of the magnetic composite material alloy material neodymium iron boron powder, copper alloy powder and iron silicon powder of 1:0.05-0.10:0.03-0.09, and adding the materials into a three-dimensional mixer to uniformly mix to obtain mixed powder;
s2, filling the mixed powder into a forming die, wherein the temperature of the materials in the die and a die cavity is not more than 30 ℃;
s3, orienting the mixed powder in a magnetic field press, performing compression molding, wherein the strength of an oriented magnetic field applied during compression molding is 2.0T, the pressure is 150KN, and the pressure is maintained for 15S;
s4, placing the molded blank into a sintering furnace under the protection of argon gas for sintering, firstly heating to 600-700 ℃, preserving heat for 3-4 hours, then heating to 1080-1180 ℃ for sintering for 3 hours, and cooling to room temperature;
s5, carrying out tempering treatment twice on the sintered molded blank, and then carrying out aging treatment to obtain a high-performance sintered neodymium-iron-boron magnet material; the primary tempering temperature is 900-910 ℃, and the heat preservation time is 2-3 hours; the secondary tempering temperature is 500-560 ℃, the time is 1-3h, the aging treatment temperature is 210 ℃, and the heat preservation time is 25h.
CN202311078740.2A 2023-08-24 2023-08-24 High-performance sintered NdFeB magnet material and preparation method thereof Pending CN117153511A (en)

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