CN110676043A - Preparation method of neodymium iron boron magnet - Google Patents

Preparation method of neodymium iron boron magnet Download PDF

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Publication number
CN110676043A
CN110676043A CN201910823181.0A CN201910823181A CN110676043A CN 110676043 A CN110676043 A CN 110676043A CN 201910823181 A CN201910823181 A CN 201910823181A CN 110676043 A CN110676043 A CN 110676043A
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neodymium
iron boron
neodymium iron
iron
ball milling
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王宏伟
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Xuzhou Awesome Magnetic Industry Co Ltd
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Xuzhou Awesome Magnetic Industry Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/026—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets protecting methods against environmental influences, e.g. oxygen, by surface treatment
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0266—Moulding; Pressing

Abstract

A preparation method of a neodymium iron boron magnet comprises the following steps: according to the chemical formula Ag (Nb)1‑xTax)O3The molar ratio of the components is that the raw material Ag is taken2O、Nb2O5And Ta2O5Mixing, adding the mixed raw materials and a solvent into a ball milling tank for ball milling, sieving, drying, presintering and ball milling to obtain a modifier; preparing neodymium iron boron sheets by adopting a traditional casting process, then crushing the prepared neodymium iron boron sheets by adopting a hydrogen explosion method to obtain neodymium iron boron powder, adding a modifier accounting for 2-3% of the mass of the neodymium iron boron powder, carrying out ball milling and refining to obtain modified neodymium iron boron powder, pressing the modified neodymium iron boron powder into a modified neodymium iron boron blank, sintering, tempering and cooling to room temperature to obtain a neodymium iron boron magnet; preparing an anticorrosive coating; spraying: and (3) uniformly spraying an anticorrosive paint on the surface of the modified neodymium iron boron magnet, and drying to obtain the anticorrosive neodymium iron boron magnet. The preparation method canThe corrosion resistance of the neodymium iron boron is improved.

Description

Preparation method of neodymium iron boron magnet
Technical Field
The invention relates to the technical field of magnet processing, in particular to a preparation method of a neodymium iron boron magnet.
Background
The Nd-Fe-B serving as a rare earth permanent magnet material has extremely high magnetic energy and coercive force, and the advantage of high energy density enables the Nd-Fe-B permanent magnet material to be widely applied to modern industry and electronic technology, so that miniaturization, light weight and thinning of instruments, electro-acoustic motors, magnetic separation magnetization and other equipment become possible. In order to improve the high temperature resistance and corrosion resistance of the ndfeb magnet, surface protection treatment such as electroplating, chemical plating, physical vapor deposition or composite plating is usually performed on the surface of the ndfeb magnet, but the current treatment method has great difficulty in process operation and unsatisfactory corrosion resistance. Based on the method, the invention provides a preparation method of the corrosion-resistant neodymium iron boron magnet.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a preparation method of a neodymium iron boron magnet.
In order to realize the purpose of the invention, the invention provides a preparation method of a neodymium iron boron magnet, which comprises the following steps:
(1) preparation of the modified body: according to the chemical formula Ag (Nb)1-xTax)O3The molar ratio of the components is that the raw material Ag is taken2O、Nb2O5And Ta2O5Mixing, and then mixing the mixed raw materials with a solvent according to a mass ratio of 1: 1 adding the mixture into a ball milling tank for ball milling, drying the ball milling material, sieving the ball milling material by a 100-mesh sieve to obtain dry powder with uniform particles, presintering the powder in air at 650-750 ℃ for 2-4h, and ball milling to obtain a modifier;
(2) preparing a sintered neodymium-iron-boron magnet: preparing neodymium iron boron sheets by adopting a traditional casting process, and then crushing the prepared neodymium iron boron sheets by adopting a hydrogen explosion method to obtain neodymium iron boron powder, wherein the mass ratio of the neodymium iron boron powder to the iron-based alloy powder is (50-60): 1, adding the mixture into a ball mill, adding a modifier accounting for 2-3% of the mass of the neodymium-iron-boron powder, performing ball milling and refining to obtain modified neodymium-iron-boron powder, pressing the modified neodymium-iron-boron powder into a modified neodymium-iron-boron green body, sintering the modified neodymium-iron-boron green body at 1000-1100 ℃ for 2-4h, tempering and insulating the modified neodymium-iron-boron green body at 650-750 ℃ for 1-2 h, and cooling the modified neodymium-iron-boron green body to room temperature at the speed of 4-6 ℃/min to obtain a sintered modified neodymium;
(3) preparing an anticorrosive coating: weighing raw materials according to 55-65 parts of epoxy resin, 0.8-1.2 parts of carbon black, 1-3 parts of titanium dioxide, 2-5 parts of silicon carbide, 1-3 parts of sodium tripolyphosphate, 0.1-0.3 part of graphene and 20-30 parts of epoxy resin diluent, mixing the epoxy resin and the epoxy resin diluent, adding the sodium tripolyphosphate, the graphene, the carbon black, the titanium dioxide, the silicon dioxide and the silicon carbide, and uniformly mixing to obtain the anticorrosive paint;
(4) spraying: and (3) uniformly spraying the anticorrosive paint prepared in the step (3) on the surface of the modified neodymium iron boron magnet prepared in the step (2), and drying to obtain the anticorrosive neodymium iron boron magnet.
Preferably, the solvent used in the ball milling in the step (1) is one or more of methanol, ethanol, acetone and deionized water.
Preferably, the ball milling beads used in the ball milling in the step (1) are one or more of zirconia, ceria or alumina.
Preferably, the iron-based alloy powder in the step (2) comprises the following raw materials in percentage by weight: 0.1-0.3% of P, 0.2-0.8% of Cr, 0.3-0.9% of Mo, 0.4-1.2% of Ga, 1-3% of Ni, 0.3-0.8% of Ti, 1-3% of Si, and the balance of Fe and inevitable impurities.
Preferably, the spraying thickness of the anticorrosive paint is 0.1-0.2 mm, and in the spraying process, the spraying direction of the anticorrosive paint forms an angle of 40-50 degrees with the surface of the modified neodymium iron boron magnet.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method provided by the invention has the advantages of simple operation process, low equipment requirement and low preparation cost, the iron-based alloy powder with a reasonable proportion is added into the neodymium iron boron powder when the sintered neodymium iron boron magnet is prepared, the neodymium iron boron magnet is modified, the corrosion resistance of the neodymium iron boron magnet is better, and the modifier Ag (Nb) is added in the ball milling process of the neodymium iron boron powder and the iron-based alloy powder1-xTax)O3The modifier can improve the magnetic energy and the coercive force of the neodymium iron boron magnet and improve the performance of the neodymium iron boron magnet.
(2) Sintering, tempering, heat preservation and cooling are carried out on the modified neodymium iron boron green body formed by pressing by adopting reasonable sintering parameters so as to improve the performance of the modified neodymium iron boron magnet;
(3) the anticorrosive coating used is reasonable in formula, the epoxy resin is used as a main material, the anticorrosive performance of the anticorrosive coating is improved by adding titanium dioxide, silicon carbide and sodium tripolyphosphate, the anticorrosive coating can be kept stable for a long time under acid and alkali conditions, and the magnetic permeability of the neodymium iron boron magnet is not influenced by the prepared anticorrosive coating.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A preparation method of a neodymium iron boron magnet comprises the following steps:
(1) preparation of the modified body: according to the chemical formula Ag (Nb)1-xTax)O3The molar ratio of the components is that the raw material Ag is taken2O、Nb2O5And Ta2O5Mixing, and then mixing the mixed raw materials with a solvent according to a mass ratio of 1: 1, adding the mixture into a ball milling tank for ball milling, drying the ball milled material, sieving the dried material by a 100-mesh sieve to obtain dry powder with uniform particles, presintering the powder in air at 650 ℃ for 4 hours, and ball milling to obtain a modifier; the solvent used for ball milling is one or more of methanol, ethanol, acetone and deionized water; the ball milling beads used for ball milling are one or more of zirconia, cerium oxide or alumina;
(2) preparing a sintered neodymium-iron-boron magnet: adopt traditional casting process preparation neodymium iron boron thin slice, then adopt the hydrogen explosion method to smash the neodymium iron boron thin slice of preparation, obtain neodymium iron boron powder, be 50 according to the mass ratio of neodymium iron boron powder and iron-based alloy powder: 1, adding the mixture into a ball mill, adding a modifier accounting for 2 percent of the mass of the neodymium-iron-boron powder, performing ball milling and refining to obtain modified neodymium-iron-boron powder, pressing the modified neodymium-iron-boron powder into a modified neodymium-iron-boron green body, sintering the modified neodymium-iron-boron green body at 1000 ℃ for 4 hours, tempering and insulating the modified neodymium-iron-boron green body at 650 ℃ for 2 hours, and cooling the modified neodymium-iron-boron green body to room temperature at the speed of 4 ℃/min to obtain a sintered modified neodymium; the iron-based alloy powder comprises the following raw materials in percentage by weight: 0.1% of P, 0.2% of Cr, 0.3% of Mo, 0.4% of Ga, 1% of Ni, 0.3% of Ti0, 1% of Si, and the balance of Fe and inevitable impurities;
(3) preparing an anticorrosive coating: weighing raw materials according to 55 parts of epoxy resin, 0.8 part of carbon black, 1 part of titanium dioxide, 2 parts of silicon carbide, 1 part of sodium tripolyphosphate, 0.1 part of graphene and 20 parts of epoxy resin diluent, mixing the epoxy resin and the epoxy resin diluent, adding the sodium tripolyphosphate, the graphene, the carbon black, the titanium dioxide, the silicon dioxide and the silicon carbide, and uniformly mixing to obtain the anticorrosive paint;
(4) spraying: uniformly spraying the anticorrosive paint prepared in the step (3) on the surface of the modified neodymium iron boron magnet prepared in the step (2), and drying to obtain the anticorrosive neodymium iron boron magnet; the spraying thickness of the anticorrosive paint is 0.1-0.2 mm, and in the spraying process, the spraying direction of the anticorrosive paint forms an angle of 40-50 degrees with the surface of the modified neodymium iron boron magnet.
Example 2
A preparation method of a neodymium iron boron magnet comprises the following steps:
(1) preparation of the modified body: according to the chemical formula Ag (Nb)1-xTax)O3The molar ratio of the components is that the raw material Ag is taken2O、Nb2O5And Ta2O5Mixing, and then mixing the mixed raw materials with a solvent according to a mass ratio of 1: 1, adding the mixture into a ball milling tank for ball milling, drying the ball milled material, sieving the dried material by a 100-mesh sieve to obtain dry powder with uniform particles, presintering the powder in air at 700 ℃ for 3 hours, and ball milling to obtain a modifier; the solvent used for ball milling is one or more of methanol, ethanol, acetone and deionized water; the ball milling beads used for ball milling are one or more of zirconia, cerium oxide or alumina;
(2) preparing a sintered neodymium-iron-boron magnet: adopt traditional casting process preparation neodymium iron boron thin slice, then adopt the hydrogen explosion method to smash the neodymium iron boron thin slice of preparation, obtain neodymium iron boron powder, be 55 according to the mass ratio of neodymium iron boron powder and iron-based alloy powder: 1, adding the mixture into a ball mill, adding a modifier accounting for 2.5 percent of the mass of the neodymium iron boron powder, performing ball milling and refining to obtain modified neodymium iron boron powder, pressing the modified neodymium iron boron powder into a modified neodymium iron boron green body, sintering the modified neodymium iron boron green body at 1050 ℃ for 3 hours, tempering and preserving heat at 700 ℃ for 1.5 hours, and cooling the modified neodymium iron boron green body to room temperature at the speed of 5 ℃/min to obtain a sintered modified neodymium iron boron magnet; the iron-based alloy powder in the step (2) comprises the following raw materials in percentage by weight: 0.2% of P, 0.5% of Cr, 0.6% of Mo, 0.8% of Ga0.8%, Ni 2%, 0.5% of Ti, 2% of Si, and the balance of Fe and inevitable impurities;
(3) preparing an anticorrosive coating: weighing the raw materials according to 60 parts of epoxy resin, 1.0 part of carbon black, 2 parts of titanium dioxide, 3.5 parts of silicon carbide, 2 parts of sodium tripolyphosphate, 0.2 part of graphene and 25 parts of epoxy resin diluent, mixing the epoxy resin and the epoxy resin diluent, adding the sodium tripolyphosphate, the graphene, the carbon black, the titanium dioxide, the silicon dioxide and the silicon carbide, and uniformly mixing to obtain the anticorrosive paint;
(4) spraying: uniformly spraying the anticorrosive paint prepared in the step (3) on the surface of the modified neodymium iron boron magnet prepared in the step (2), and drying to obtain the anticorrosive neodymium iron boron magnet; the spraying thickness of the anticorrosive paint is 0.1-0.2 mm, and in the spraying process, the spraying direction of the anticorrosive paint forms an angle of 40-50 degrees with the surface of the modified neodymium iron boron magnet.
Example 3
A preparation method of a neodymium iron boron magnet comprises the following steps:
(1) preparation of the modified body: according to the chemical formula Ag (Nb)1-xTax)O3The molar ratio of the components is that the raw material Ag is taken2O、Nb2O5And Ta2O5Mixing, and then mixing the mixed raw materials with a solvent according to a mass ratio of 1: 1, adding the mixture into a ball milling tank for ball milling, drying the ball milled material, sieving the dried material by a 100-mesh sieve to obtain dry powder with uniform particles, presintering the powder in air at 750 ℃ for 2 hours, and ball milling to obtain a modifier; the solvent used for ball milling is one or more of methanol, ethanol, acetone and deionized water; the ball milling beads used for ball milling are one or more of zirconia, cerium oxide or alumina;
(2) preparing a sintered neodymium-iron-boron magnet: adopt traditional casting process preparation neodymium iron boron thin slice, then adopt the hydrogen explosion method to smash the neodymium iron boron thin slice of preparation, obtain neodymium iron boron powder, be 60 according to the mass ratio of neodymium iron boron powder and iron-based alloy powder: 1, adding the mixture into a ball mill, adding a modifier accounting for 3% of the mass of the neodymium iron boron powder, performing ball milling and refining to obtain modified neodymium iron boron powder, pressing the modified neodymium iron boron powder into a modified neodymium iron boron green body, sintering the modified neodymium iron boron green body at 1100 ℃ for 2 hours, tempering and preserving heat at 750 ℃ for 1 hour, and cooling the modified neodymium iron boron green body to room temperature at the speed of 6 ℃/min to obtain a sintered modified neodymium iron boron magnet; the iron-based alloy powder in the step (2) comprises the following raw materials in percentage by weight: 0.3% of P, 0.8% of Cr, 0.9% of Mo, 1.2% of Ga, 3% of Ni, 0.8% of Ti, 3% of Si, and the balance of Fe and inevitable impurities;
(3) preparing an anticorrosive coating: weighing raw materials according to 65 parts of epoxy resin, 1.2 parts of carbon black, 3 parts of titanium dioxide, 5 parts of silicon carbide, 3 parts of sodium tripolyphosphate, 0.3 part of graphene and 30 parts of epoxy resin diluent, mixing the epoxy resin and the epoxy resin diluent, adding the sodium tripolyphosphate, the graphene, the carbon black, the titanium dioxide, the silicon dioxide and the silicon carbide, and uniformly mixing to obtain the anticorrosive paint;
(4) spraying: uniformly spraying the anticorrosive paint prepared in the step (3) on the surface of the modified neodymium iron boron magnet prepared in the step (2), and drying to obtain the anticorrosive neodymium iron boron magnet; the spraying thickness of the anticorrosive paint is 0.1-0.2 mm, and in the spraying process, the spraying direction of the anticorrosive paint forms an angle of 40-50 degrees with the surface of the modified neodymium iron boron magnet.

Claims (5)

1. The preparation method of the neodymium iron boron magnet is characterized by comprising the following steps:
(1) preparation of the modified body: according to the chemical formula Ag (Nb)1-xTax)O3The molar ratio of the components is that the raw material Ag is taken2O、Nb2O5And Ta2O5Mixing, and then mixing the mixed raw materials with a solvent according to a mass ratio of 1: 1 adding the mixture into a ball milling tank for ball milling, drying the ball milling material, sieving the ball milling material by a 100-mesh sieve to obtain dry powder with uniform particles, presintering the powder in air at 650-750 ℃ for 2-4h, and ball milling to obtain a modifier;
(2) preparing a sintered neodymium-iron-boron magnet: preparing neodymium iron boron sheets by adopting a traditional casting process, and then crushing the prepared neodymium iron boron sheets by adopting a hydrogen explosion method to obtain neodymium iron boron powder, wherein the mass ratio of the neodymium iron boron powder to the iron-based alloy powder is (50-60): 1, adding the mixture into a ball mill, adding a modifier accounting for 2-3% of the mass of the neodymium-iron-boron powder, performing ball milling and refining to obtain modified neodymium-iron-boron powder, pressing the modified neodymium-iron-boron powder into a modified neodymium-iron-boron green body, sintering the modified neodymium-iron-boron green body at 1000-1100 ℃ for 2-4h, tempering and insulating the modified neodymium-iron-boron green body at 650-750 ℃ for 1-2 h, and cooling the modified neodymium-iron-boron green body to room temperature at the speed of 4-6 ℃/min to obtain a sintered modified neodymium;
(3) preparing an anticorrosive coating: weighing raw materials according to 55-65 parts of epoxy resin, 0.8-1.2 parts of carbon black, 1-3 parts of titanium dioxide, 2-5 parts of silicon carbide, 1-3 parts of sodium tripolyphosphate, 0.1-0.3 part of graphene and 20-30 parts of epoxy resin diluent, mixing the epoxy resin and the epoxy resin diluent, adding the sodium tripolyphosphate, the graphene, the carbon black, the titanium dioxide, the silicon dioxide and the silicon carbide, and uniformly mixing to obtain the anticorrosive paint;
(4) spraying: and (3) uniformly spraying the anticorrosive paint prepared in the step (3) on the surface of the modified neodymium iron boron magnet prepared in the step (2), and drying to obtain the anticorrosive neodymium iron boron magnet.
2. The method for preparing a neodymium-iron-boron magnet according to claim 1, wherein the solvent used for ball milling in step (1) is one or more of methanol, ethanol, acetone and deionized water.
3. The method for preparing a neodymium iron boron magnet according to claim 1, characterized in that ball milling beads used in the ball milling in the step (1) are one or more of zirconia, ceria or alumina.
4. The method for preparing a neodymium iron boron magnet according to claim 1, wherein the iron-based alloy powder in the step (2) comprises the following raw materials in percentage by weight: 0.1-0.3% of P, 0.2-0.8% of Cr, 0.3-0.9% of Mo, 0.4-1.2% of Ga, 1-3% of Ni, 0.3-0.8% of Ti, 1-3% of Si, and the balance of Fe and inevitable impurities.
5. The method for preparing the neodymium-iron-boron magnet according to claim 1, wherein the spraying thickness of the anticorrosive paint is 0.1-0.2 mm, and in the spraying process, the spraying direction of the anticorrosive paint forms an angle of 40-50 degrees with the surface of the modified neodymium-iron-boron magnet.
CN201910823181.0A 2019-09-02 2019-09-02 Preparation method of neodymium iron boron magnet Pending CN110676043A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113755066A (en) * 2021-08-02 2021-12-07 安徽省瀚海新材料股份有限公司 Anti-oxidation adhesive for coating hydride on sintered neodymium iron boron and application thereof
CN117165152A (en) * 2023-07-28 2023-12-05 浙江大学 Preparation method of neodymium-iron-boron magnet anticorrosive paint with high surface tension

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113755066A (en) * 2021-08-02 2021-12-07 安徽省瀚海新材料股份有限公司 Anti-oxidation adhesive for coating hydride on sintered neodymium iron boron and application thereof
CN117165152A (en) * 2023-07-28 2023-12-05 浙江大学 Preparation method of neodymium-iron-boron magnet anticorrosive paint with high surface tension

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