CN115472371B - Processing method of sintered neodymium iron boron - Google Patents
Processing method of sintered neodymium iron boron Download PDFInfo
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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
- H01F1/0577—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 sintered
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- 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
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Abstract
The invention discloses a processing method of sintered neodymium iron boron, which relates to the technical field of magnetic materials and comprises the following steps: s1, pulverizing waste neodymium iron boron; s2, preparing additive powder; s3, mixing powder; s4, blank making, sintering and tempering; and S5, surface treatment. The processing method of the sintered neodymium iron boron, disclosed by the invention, has the advantages of high processing precision, simple flow, shorter production period and high qualified rate of outturn rate; the sintered Nd-Fe-B permanent magnetic material prepared by the processing method has lower cost and excellent comprehensive magnetic property and corrosion resistance.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a processing method of sintered neodymium iron boron.
Background
The neodymium iron boron permanent magnet material rapidly enters an industrialized society due to excellent characteristics of high residual magnetism, high coercive force, high magnetic energy product, easiness in processing and the like, is particularly widely applied to various fields of aerospace, national defense and military, magnetic transmission devices, electronic instruments, medical instruments, household appliances and the like, and continuously appears in a new application field. The development, production and application degree of the compound is one of the marks of the economic development degree of the modern countries, and plays an important role in national economy and social activities.
The sintered Nd-Fe-B permanent magnet material is a common Nd-Fe-B permanent magnet material, and is used as an important basic functional material which is a permanent magnet material with the strongest performance so far. However, the sintered nd-fe-b material also has certain defects, such as poor temperature resistance, insufficient corrosion resistance and high processing cost. On the other hand, the vacuum sintering blank of the current sintered neodymium iron boron processing method has larger size, completely densified material, higher density and hardness, and increased difficulty of subsequent processing, and simultaneously has a series of problems of low processing precision, complex flow, longer production period, low qualified rate of outturn, higher cost and the like.
In order to solve the above problems, chinese patent document CN102360910B discloses a method for processing a neodymium iron boron magnet capable of improving boundary phase electronegativity. The technical scheme adopted by the invention is as follows: a processing method of a neodymium iron boron magnet comprises the following steps: (1) taking an alloy R a Co b Ga 100-a-b-c Cu c Wherein R is rare earth element, a is more than or equal to 60 and less than or equal to 70, b is more than or equal to 10 and less than or equal to 15,5 and less than or equal to 10; carrying out heat treatment on the alloy, and then crushing to obtain alloy powder; (2) mixing the alloy powder and neodymium iron boron raw material powder under the protection of nitrogen; (3) the mixed powder is oriented and molded in a magnetic field to obtain a pressed compact; (4) and sintering and tempering the pressed compact. By adding the alloy powder, the invention fundamentally improves the boundary phase microstructure and the electronegativity of the boundary phase of the neodymium iron boron magnet, reduces the corrosion potential difference between the neodymium iron boron main phase and the rare earth-rich boundary phase as much as possible, weakens or avoids intergranular corrosion, and reduces corrosionThe current density is corroded, so that the weight loss of the magnet is reduced, and the corrosion resistance is improved. However, the cost of the material is still high, and the comprehensive magnetic performance is still to be further improved.
Therefore, a more effective processing method for sintering neodymium iron boron is needed to be found, and the sintered neodymium iron boron permanent magnet material with lower cost, excellent comprehensive magnetic performance and excellent corrosion resistance is prepared.
Disclosure of Invention
The invention mainly aims to provide a processing method of sintered neodymium iron boron, which has the advantages of high processing precision, simple flow, short production period and high qualified rate of outturn rate; the sintered Nd-Fe-B permanent magnet material prepared by the processing method has lower cost and excellent comprehensive magnetic property and corrosion resistance.
In order to achieve the above purpose, the invention provides a processing method of sintered neodymium iron boron, comprising the following steps:
step S1, pulverizing waste neodymium iron boron: removing a coating/plating layer, an oxidation layer and other pollutants on the surface of the recovered waste neodymium iron boron by using a mechanical polishing and ultrasonic washing mode; then crushing the mixture into waste neodymium iron boron powder;
step S2, preparation of additive powder: taking additive Re a M b F c Si d Fe (100-a-b-c-d) Wherein a is more than or equal to 25 and less than or equal to 35,0 and less than or equal to b is more than or equal to 1,0.01 and less than or equal to c is more than or equal to 0.03,0.8 and less than or equal to 1.0, re is at least three of Gd, tb, dy, ho, er, nd and Pr, and M is a mixture of Ni, sm, sc, ge, zn, bi and Zr; carrying out heat treatment on the additive and then crushing to obtain additive powder;
step S3, mixing powder: uniformly mixing the waste neodymium iron boron powder prepared in the step S1, the additive powder prepared in the step S2 and the nano boron carbide in an inert gas atmosphere;
s4, blank making, sintering and tempering: under the protection of nitrogen, the magnetic powder is aligned and molded in a magnetic field with the magnetic field intensity of 1.5-3.5T, and then is made into a blank through isostatic pressing at 350-430 MPa; then sintering and tempering are carried out in sequence to obtain a magnet;
step S5, surface treatment: and sequentially carrying out cutting, polishing and sand blasting treatment on the surface of the magnet, then coating an Everlube E/M6340 molybdenum disulfide solid coating on the surface of the magnet, and finally drying and curing the product coated with the coating to obtain the sintered neodymium-iron-boron permanent magnet material.
Preferably, the waste neodymium iron boron in the step S1 is Nd 30 Fe 69 B 1 (ii) a The average grain diameter of the waste neodymium iron boron powder is 2 mu m.
Preferably, in the step S2, M is a mixture formed by mixing Ni, sm, sc, ge, zn, bi and Zr according to the mass ratio of (1-2): (0.4-0.7): (0.3-0.5): (0.05-0.1): (0.1-0.3): (0.05-0.08): 0.2.
Preferably, the heat treatment in step S2 is specifically heat preservation at 1000-1100 ℃ for 8-12 hours.
Preferably, the average particle diameter of the additive powder in step S2 is 3 μm.
Preferably, the mass ratio of the waste neodymium iron boron powder, the additive powder and the nano boron carbide in the step S3 is (10-15): 0.3-0.6): 0.1.
Preferably, the particle size of the nano boron carbide in the step S3 is 50-100nm.
Preferably, the inert gas in step S3 is any one of nitrogen, helium, neon and argon.
Preferably, the sintering temperature in the step S4 is 1030-1070 ℃, the sintering time is 4-6 hours, and the sintering vacuum degree is kept at 0.02-0.05Pa.
Preferably, the tempering treatment in the step S4 comprises secondary tempering treatment, wherein the temperature of the primary tempering treatment is 850-900 ℃, and the time is 2-3 hours; the temperature of the secondary tempering treatment is 450-550 ℃, and the time is 3-5 hours.
Preferably, the drying and curing temperature in the step S5 is 190-220 ℃, and the time is 12-18h.
Another object of the present invention is to provide a sintered nd-fe-b permanent magnet material manufactured according to the above processing method of sintered nd-fe-b.
Due to the application of the technical scheme, the invention has the following beneficial effects:
(1) The processing method of the sintered neodymium iron boron disclosed by the invention has the advantages of low dependence on equipment, high processing efficiency and finished product qualification rate, convenience in operation and low energy consumption, and is suitable for continuous large-scale production.
(2) According to the processing method of the sintered neodymium iron boron, waste neodymium iron boron is used as a raw material, waste materials are changed into valuable materials, waste resources are recycled, resources are saved, and the problem of ring caused by idling of the waste resources is solved; through reasonable selection of components and proportions of waste neodymium-iron-boron powder, additive powder, nano boron carbide and the like, the waste neodymium-iron-boron powder, the additive powder, the nano boron carbide and the like can be better matched with each other, and under the combined action, the prepared sintered neodymium-iron-boron permanent magnet material is lower in cost, and excellent in comprehensive magnetic performance and corrosion resistance. The additive powder and the nano boron carbide are added into the alloy main phase, so that the micro morphology of the magnetic material can be improved, and the specific magnetization intensity, the coercive force and the magnetic conductivity can be improved. The product has synergistic effect with other components, and can improve stability, improve magnetic pollution, and reduce energy consumption.
(3) The invention discloses a processing method of sintered neodymium iron boron, and an additive Re a M b F c Si d Fe (100-a-b-c-d) Wherein a is more than or equal to 25 and less than or equal to 35,0, b is more than or equal to 1,0.01, c is more than or equal to 0.03,0.8, d is more than or equal to 1.0, re is at least three of Gd, tb, dy, ho, er, nd and Pr, and M is a mixture formed by mixing Ni, sm, sc, ge, zn, bi and Zr according to the mass ratio of (1-2), (0.4-0.7), (0.3-0.5), (0.05-0.1), (0.1-0.3) and (0.05-0.08) respectively; through reasonable selection of the components and the proportion, the loss of the rare earth elements of the waste neodymium iron boron can be compensated, and the components and other components have synergistic effect, so that the comprehensive magnetic property and the corrosion resistance can be further improved.
(4) According to the processing method of the sintered neodymium iron boron, disclosed by the invention, the Everlube E/M6340 molybdenum disulfide solid coating is coated on the surface of the magnet, so that the corrosion resistance of the magnet can be further improved, and the service life of the magnet is prolonged.
(5) According to the processing method of the sintered neodymium iron boron, disclosed by the invention, through reasonable selection of technological parameters such as heat treatment, sintering, tempering and the like, the comprehensive magnetic property and the corrosion resistance of the prepared sintered neodymium iron boron are better.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
Example 1
A processing method of sintered neodymium iron boron comprises the following steps:
step S1, pulverizing waste neodymium iron boron: removing a coating/plating layer, an oxidation layer and other pollutants on the surface of the recovered waste neodymium iron boron by using a mechanical polishing and ultrasonic washing mode; then crushing the mixture into waste neodymium iron boron powder;
step S2, preparation of additive powder: taking additive Re 25 M 0.1 F 0.01 Si 0.8 Fe 74.09 Re is a mixture formed by mixing Gd, tb and Dy according to the mass ratio of 1; carrying out heat treatment on the additive and then crushing to obtain additive powder;
step S3, mixing powder: uniformly mixing the waste neodymium iron boron powder prepared in the step S1, the additive powder prepared in the step S2 and the nano boron carbide in an inert gas atmosphere;
s4, blank making, sintering and tempering: under the protection of nitrogen, the magnetic powder is subjected to orientation die pressing in a magnetic field with the magnetic field intensity of 3.5T, and then a blank is prepared by isostatic pressing at 350 MPa; then sintering and tempering are carried out in sequence to obtain a magnet;
step S5, surface treatment: and sequentially carrying out cutting, polishing and sand blasting treatment on the surface of the magnet, then coating an Everlube E/M6340 molybdenum disulfide solid coating on the surface of the magnet, and finally drying and curing the product coated with the coating to obtain the sintered neodymium-iron-boron permanent magnet material.
The waste neodymium iron boron in the step S1 is Nd 30 Fe 69 B 1 (ii) a The average grain diameter of the waste neodymium-iron-boron powder is 2 mu m.
In the step S2, M is a mixture formed by mixing Ni, sm, sc, ge, zn, bi and Zr according to a mass ratio of 1; the heat treatment is specifically heat preservation for 8 hours at 1000 ℃; the additive powder had an average particle size of 3 μm.
In the step S3, the mass ratio of the waste neodymium iron boron powder to the additive powder to the nano boron carbide is 10.3; the particle size of the nano boron carbide is 100nm; the inert gas is nitrogen.
In the step S4, the sintering temperature is 1030 ℃ for 4 hours, and the sintering vacuum degree is kept at 0.02Pa; the tempering treatment comprises secondary tempering treatment, wherein the temperature of the primary tempering treatment is 850 ℃, and the time is 2 hours; the temperature of the second-stage tempering treatment is 450 ℃ and the time is 3 hours.
In the step S5, the drying and curing temperature is 190 ℃ and the time is 12h.
A sintered Nd-Fe-B permanent magnetic material prepared by the processing method of sintered Nd-Fe-B.
Example 2
A processing method of sintered neodymium iron boron comprises the following steps:
step S1, pulverizing waste neodymium iron boron: removing a coating/plating layer, an oxidation layer and other pollutants on the surface of the recovered waste neodymium iron boron by using a mechanical polishing and ultrasonic washing mode; then crushing the neodymium iron boron into waste neodymium iron boron powder;
step S2, preparation of additive powder: taking additive Re 27 M 0.3 F 0.015 Si 0.85 Fe 71.835 Re is a mixture formed by mixing Ho, er, nd and Pr according to a mass ratio of 1; carrying out heat treatment on the additive and then crushing to obtain additive powder;
step S3, mixing powder: uniformly mixing the waste neodymium iron boron powder prepared in the step S1, the additive powder prepared in the step S2 and the nano boron carbide in an inert gas atmosphere;
s4, blank making, sintering and tempering: under the protection of nitrogen, the magnetic powder is subjected to orientation die pressing in a magnetic field with the magnetic field intensity of 3T, and then is subjected to isostatic pressing at 370MPa to prepare a blank; then sintering and tempering are carried out in sequence to obtain a magnet;
step S5, surface treatment: and sequentially carrying out cutting, polishing and sand blasting treatment on the surface of the magnet, then coating an Everlube E/M6340 molybdenum disulfide solid coating on the surface of the magnet, and finally drying and curing the product coated with the coating to obtain the sintered neodymium-iron-boron permanent magnet material.
The waste neodymium iron boron in the step S1 is Nd 30 Fe 69 B 1 (ii) a The average grain diameter of the waste neodymium-iron-boron powder is 2 mu m.
In the step S2, M is a mixture formed by mixing Ni, sm, sc, ge, zn, bi and Zr according to the mass ratio of 1.3; the heat treatment is specifically heat preservation for 9 hours at 1030 ℃; the additive powder had an average particle size of 3 μm.
The mass ratio of the waste neodymium iron boron powder, the additive powder and the nano boron carbide in the step S3 is (11) 0.4; the particle size of the nano boron carbide is 90nm; the inert gas is helium.
In the step S4, the sintering temperature is 1040 ℃, the time is 4.5 hours, and the sintering vacuum degree is kept at 0.03Pa; the tempering treatment comprises secondary tempering treatment, wherein the temperature of the primary tempering treatment is 865 ℃, and the time is 2.3 hours; the temperature of the second-stage tempering treatment is 470 ℃ and the time is 3.5 hours.
In the step S5, the drying and curing temperature is 200 ℃ and the time is 14h.
A sintered Nd-Fe-B permanent magnet material prepared according to the processing method of the sintered Nd-Fe-B.
Example 3
A processing method of sintered neodymium iron boron comprises the following steps:
step S1, pulverizing waste neodymium iron boron: removing a coating/plating layer, an oxidation layer and other pollutants on the surface of the recovered waste neodymium iron boron by using a mechanical polishing and ultrasonic washing mode; then crushing the mixture into waste neodymium iron boron powder;
step S2, preparation of additive powder: taking additive Re 30 M 0.5 F 0.02 Si 0.9 Fe 68.58 Re is a mixture formed by mixing Gd, dy, ho, nd and Pr according to a mass ratio of 2;the additive is crushed after being subjected to heat treatment to obtain additive powder;
step S3, mixing powder: uniformly mixing the waste neodymium iron boron powder prepared in the step S1, the additive powder prepared in the step S2 and the nano boron carbide in an inert gas atmosphere;
s4, blank making, sintering and tempering: under the protection of nitrogen, the magnetic powder is subjected to orientation die pressing in a magnetic field with the magnetic field intensity of 2.5T, and then is subjected to isostatic pressing under 390MPa to prepare a blank; then sintering and tempering are carried out in sequence to obtain a magnet;
step S5, surface treatment: and sequentially carrying out cutting, polishing and sand blasting treatment on the surface of the magnet, then coating an Everlube E/M6340 molybdenum disulfide solid coating on the surface of the magnet, and finally drying and curing the product coated with the coating to obtain the sintered neodymium-iron-boron permanent magnet material.
The waste neodymium iron boron in the step S1 is Nd 30 Fe 69 B 1 (ii) a The average grain diameter of the waste neodymium-iron-boron powder is 2 mu m.
In the step S2, M is a mixture formed by mixing Ni, sm, sc, ge, zn, bi and Zr according to a mass ratio of 1.5; the heat treatment is specifically heat preservation for 10 hours at 1050 ℃; the average particle size of the additive powder was 3 μm.
In the step S3, the mass ratio of the waste neodymium iron boron powder to the additive powder to the nano boron carbide is 13.45; the particle size of the nano boron carbide is 75nm; the inert gas is neon.
In the step S4, the sintering temperature is 1050 ℃, the time is 5 hours, and the sintering vacuum degree is kept at 0.035Pa; the tempering treatment comprises secondary tempering treatment, wherein the temperature of the primary tempering treatment is 880 ℃, and the time is 2.5 hours; the temperature of the second-stage tempering treatment is 500 ℃ and the time is 4 hours.
In the step S5, the drying and curing temperature is 210 ℃, and the time is 15h.
A sintered Nd-Fe-B permanent magnetic material prepared by the processing method of sintered Nd-Fe-B.
Example 4
A processing method of sintered neodymium iron boron comprises the following steps:
step S1, pulverizing waste neodymium iron boron: removing a coating/plating layer, an oxidation layer and other pollutants on the surface of the recovered waste neodymium iron boron by using a mechanical polishing and ultrasonic washing mode; then crushing the mixture into waste neodymium iron boron powder;
step S2, preparation of additive powder: taking additive Re 33 M 0.8 F 0.025 Si 0.95 Fe 65.225 Re is a mixture formed by mixing Gd, tb, dy, ho, er, nd, pr in a mass ratio of 1; carrying out heat treatment on the additive and then crushing to obtain additive powder;
step S3, mixing powder: uniformly mixing the waste neodymium iron boron powder prepared in the step S1, the additive powder prepared in the step S2 and the nano boron carbide in an inert gas atmosphere;
s4, blank making, sintering and tempering: under the protection of nitrogen, the magnetic powder is subjected to orientation die pressing in a magnetic field with the magnetic field intensity of 2T, and then a blank is prepared by isostatic pressing under 420 MPa; then sintering and tempering are carried out in sequence to obtain a magnet;
step S5, surface treatment: and sequentially carrying out cutting, polishing and sand blasting treatment on the surface of the magnet, then coating an Everlube E/M6340 molybdenum disulfide solid coating on the surface of the magnet, and finally drying and curing the product coated with the coating to obtain the sintered neodymium-iron-boron permanent magnet material.
The waste neodymium iron boron in the step S1 is Nd 30 Fe 69 B 1 (ii) a The average grain diameter of the waste neodymium iron boron powder is 2 mu m.
In the step S2, M is a mixture formed by mixing Ni, sm, sc, ge, zn, bi and Zr according to a mass ratio of 1.8; the heat treatment is specifically heat preservation at 1090 ℃ for 11 hours; the additive powder had an average particle size of 3 μm.
In the step S3, the mass ratio of the waste neodymium iron boron powder to the additive powder to the nano boron carbide is 14.55; the particle size of the nano boron carbide is 60nm; the inert gas is argon.
In the step S4, the sintering temperature is 1060 ℃, the time is 5.5 hours, and the sintering vacuum degree is kept at 0.045Pa; the tempering treatment comprises secondary tempering treatment, wherein the temperature of the primary tempering treatment is 890 ℃, and the time is 2.8 hours; the temperature of the second-stage tempering treatment is 530 ℃ and the time is 4.5 hours.
In the step S5, the drying and curing temperature is 215 ℃, and the time is 17h.
A sintered Nd-Fe-B permanent magnet material prepared according to the processing method of the sintered Nd-Fe-B.
Example 5
A processing method of sintered neodymium iron boron comprises the following steps:
step S1, pulverizing waste neodymium iron boron: removing a coating/plating layer, an oxidation layer and other pollutants on the surface of the recovered waste neodymium iron boron by using a mechanical polishing and ultrasonic washing mode; then crushing the mixture into waste neodymium iron boron powder;
step S2, preparation of additive powder: taking additive Re 35 M 1 F 0.03 Si 1 Fe 62.97 Re is a mixture formed by mixing Gd, ho, er and Nd according to a mass ratio of 2; carrying out heat treatment on the additive and then crushing to obtain additive powder;
step S3, mixing powder: uniformly mixing the waste neodymium iron boron powder prepared in the step S1, the additive powder prepared in the step S2 and the nano boron carbide in an inert gas atmosphere;
s4, blank making, sintering and tempering: under the protection of nitrogen, the magnetic powder is subjected to orientation die pressing in a magnetic field with the magnetic field intensity of 1.5T, and then a blank is prepared by isostatic pressing under 430 MPa; then sintering and tempering are carried out in sequence to obtain a magnet;
step S5, surface treatment: and sequentially carrying out cutting, polishing and sand blasting treatment on the surface of the magnet, then coating an Everlube E/M6340 molybdenum disulfide solid coating on the surface of the magnet, and finally drying and curing the product coated with the coating to obtain the sintered neodymium-iron-boron permanent magnet material.
In the step S1, the waste neodymium iron boron comprisesNd 30 Fe 69 B 1 (ii) a The average grain diameter of the waste neodymium-iron-boron powder is 2 mu m.
In the step S2, M is a mixture formed by mixing Ni, sm, sc, ge, zn, bi and Zr according to a mass ratio of 2.7; the heat treatment is specifically heat preservation for 12 hours at 1100 ℃; the average particle diameter of the additive powder in step S2 was 3 μm.
In the step S3, the mass ratio of the waste neodymium iron boron powder to the additive powder to the nano boron carbide is 15.6; the particle size of the nano boron carbide is 50nm; the inert gas is nitrogen.
In the step S4, the sintering temperature is 1070 ℃, the time is 6 hours, and the sintering vacuum degree is kept at 0.05Pa; the tempering treatment comprises secondary tempering treatment, wherein the temperature of the primary tempering treatment is 900 ℃, and the time is 3 hours; the temperature of the secondary tempering treatment is 550 ℃ and the time is 5 hours.
In the step S5, the drying and curing temperature is 220 ℃ and the time is 18h.
A sintered Nd-Fe-B permanent magnet material prepared according to the processing method of the sintered Nd-Fe-B.
Comparative example 1
The invention provides a processing method of sintered neodymium iron boron and a sintered neodymium iron boron permanent magnet material prepared by the processing method, which are similar to those in embodiment 1, except that no additive powder is added in step S3.
Comparative example 2
The invention provides a processing method of sintered neodymium iron boron and a sintered neodymium iron boron permanent magnet material prepared by the processing method, which are similar to those in embodiment 1, except that nano boron carbide is not added in step S3.
In order to further explain the beneficial technical effects of the processing method of the sintered nd-fe-b manufactured by the embodiments of the present invention, the sintered nd-fe-b permanent magnet material manufactured by the embodiments of the present invention is subjected to the related performance test, the test result is shown in table 1, and the test method is as follows: detecting the comprehensive magnetic property of the magnetic material according to a GB/T3217-2013 permanent magnet (hard magnet) material magnetic test method; the corrosion resistance is realized by performing a neutral salt spray test on the neodymium iron boron magnetic material, performing a spray salt spray test on the test material by using a sodium chloride aqueous solution with the concentration of 5wt%, wherein the test temperature is 30 ℃, and observing the corrosion condition after 430 h.
TABLE 1 Performance test results of sintered Nd-Fe-B permanent-magnet materials
| Sample (I) | Remanence (KGs) | Coercive force (KOe) | Maximum magnetic energy product (MGOe) | Corrosion resistance |
| Example 1 | 13.52 | 27.69 | 44.65 | Does not rust |
| Example 2 | 13.49 | 27.76 | 44.58 | Does not rust |
| Example 3 | 13.45 | 27.86 | 44.49 | Does not rust |
| Example 4 | 13.38 | 27.98 | 44.31 | Does not rust |
| Example 5 | 13.32 | 28.04 | 44.10 | Does not rust |
| Comparative example 1 | 13.01 | 24.31 | 42.18 | Rusting |
| Comparative example 2 | 13.26 | 26.15 | 43.22 | Rusting |
As can be seen from table 1, the sintered nd-fe-b permanent magnet material prepared by the processing method of sintered nd-fe-b disclosed in the embodiment of the present invention has more excellent comprehensive magnetic performance and corrosion resistance compared to the comparative product, which is the result of synergistic effect of each component.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. The processing method of the sintered neodymium iron boron is characterized by comprising the following steps:
step S1, pulverizing waste neodymium iron boron: removing a coating/plating layer, an oxidation layer and other pollutants on the surface of the recovered waste neodymium iron boron by using a mechanical polishing and ultrasonic washing mode; then crushing the mixture into waste neodymium iron boron powder; the waste neodymium iron boron is composed of Nd 30 Fe 69 B 1 (ii) a The average particle size of the waste neodymium iron boron powder is 2 mu m;
step S2, preparation of additive powder: taking additive Re a M b F c Si d Fe (100-a-b-c-d) Wherein a is more than or equal to 25 and less than or equal to 35,0 and less than or equal to 1,0.01 and less than or equal to c and less than or equal to 0.03,0.8 and less than or equal to 1.0, re is at least three of Gd, tb, dy, ho, er, nd and Pr; carrying out heat treatment on the additive and then crushing to obtain additive powder; the M is a mixture formed by mixing Ni, sm, sc, ge, zn, bi and Zr according to the mass ratio of (1-2): (0.4-0.7): (0.3-0.5): (0.05-0.1): (0.1-0.3): 0.05-0.08): 0.2;
step S3, mixing powder: uniformly mixing the waste neodymium iron boron powder prepared in the step S1, the additive powder prepared in the step S2 and the nano boron carbide in an inert gas atmosphere;
s4, blank making, sintering and tempering: under the protection of nitrogen, the magnetic powder is subjected to orientation die pressing in a magnetic field with the magnetic field intensity of 1.5-3.5T, and then is subjected to isostatic pressing at 350-430MPa to prepare a blank; then sintering and tempering are carried out in sequence to obtain a magnet;
step S5, surface treatment: and sequentially carrying out cutting, polishing and sand blasting treatment on the surface of the magnet, then coating an Everlube E/M6340 molybdenum disulfide solid coating on the surface of the magnet, and finally drying and curing the product coated with the coating to obtain the sintered neodymium-iron-boron permanent magnet material.
2. The processing method of the sintered neodymium iron boron according to the claim 1, characterized in that the heat treatment in the step S2 is specifically heat preservation at 1000-1100 ℃ for 8-12 hours; the average particle diameter of the additive powder in step S2 was 3 μm.
3. The processing method of sintered NdFeB as claimed in claim 1, wherein the mass ratio of the waste NdFeB powder, the additive powder and the nano boron carbide in the step S3 is (10-15): 0.3-0.6): 0.1.
4. The processing method of sintered neodymium iron boron according to claim 1, wherein the particle size of the nano boron carbide in step S3 is 50-100nm; the inert gas is any one of nitrogen, helium, neon and argon.
5. The processing method of sintered neodymium iron boron according to claim 1, characterized in that in step S4, the sintering temperature is 1030-1070 ℃, the time is 4-6 hours, and the sintering vacuum degree is maintained at 0.02-0.05Pa.
6. The processing method of sintered neodymium iron boron according to claim 1, wherein the tempering treatment in step S4 includes a secondary tempering treatment, the temperature of the primary tempering treatment is 850-900 ℃, and the time is 2-3 hours; the temperature of the secondary tempering treatment is 450-550 ℃, and the time is 3-5 hours.
7. The processing method of the sintered NdFeB as claimed in claim 1, wherein the drying and curing temperature in the step S5 is 190-220 ℃ and the time is 12-18h.
8. A sintered nd-fe-b permanent magnet material made by the method of processing sintered nd-fe-b according to any one of claims 1 to 7.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009200425A (en) * | 2008-02-25 | 2009-09-03 | Osaka Industrial Promotion Organization | Manufacturing method of rare-earth magnet, and rare-earth magnet manufactured by the manufacturing method |
| CN105702405A (en) * | 2016-04-29 | 2016-06-22 | 湖北工程学院 | Nano composite NdFeB (neodymium iron boron) permanent magnetic material and preparation method |
| CN106158339A (en) * | 2016-06-22 | 2016-11-23 | 北京科技大学 | Sintered NdFeB reclaims the method that waste material prepares high-performance permanent magnet through diffusion penetration |
| CN114171276A (en) * | 2021-12-24 | 2022-03-11 | 余姚市宏伟磁材科技有限公司 | Magnetostatic coupling high-strength composite neodymium iron boron magnet and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009200425A (en) * | 2008-02-25 | 2009-09-03 | Osaka Industrial Promotion Organization | Manufacturing method of rare-earth magnet, and rare-earth magnet manufactured by the manufacturing method |
| CN105702405A (en) * | 2016-04-29 | 2016-06-22 | 湖北工程学院 | Nano composite NdFeB (neodymium iron boron) permanent magnetic material and preparation method |
| CN106158339A (en) * | 2016-06-22 | 2016-11-23 | 北京科技大学 | Sintered NdFeB reclaims the method that waste material prepares high-performance permanent magnet through diffusion penetration |
| CN114171276A (en) * | 2021-12-24 | 2022-03-11 | 余姚市宏伟磁材科技有限公司 | Magnetostatic coupling high-strength composite neodymium iron boron magnet and preparation method thereof |
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