CN112670048A - Partial pressure sintering manufacturing method of neodymium iron boron magnet - Google Patents

Partial pressure sintering manufacturing method of neodymium iron boron magnet Download PDF

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CN112670048A
CN112670048A CN202011468354.0A CN202011468354A CN112670048A CN 112670048 A CN112670048 A CN 112670048A CN 202011468354 A CN202011468354 A CN 202011468354A CN 112670048 A CN112670048 A CN 112670048A
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boron magnet
neodymium
heating
iron
green body
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CN112670048B (en
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詹前营
冉桂平
汪志远
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Dongguan Jiada Magnet Electronic Co ltd
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Abstract

The invention relates to the technical field of magnets, in particular to a partial pressure sintering manufacturing method of a neodymium iron boron magnet, which comprises the following steps: (1) taking neodymium iron boron magnet powder, orienting in a magnetic field, and pressing to prepare a green body; (2) and (3) carrying out isostatic pressing treatment on the green body, then placing the green body in a sintering furnace for partial pressure sintering, and carrying out tempering heat treatment to obtain the neodymium-iron-boron magnet. The partial pressure sintering manufacturing method of the neodymium iron boron magnet is simple and convenient to operate, easy to control, high in production efficiency and product yield, stable in product quality, good in mechanical property and magnetic property, good in machinability, not prone to cracking, and beneficial to large-scale production.

Description

Partial pressure sintering manufacturing method of neodymium iron boron magnet
Technical Field
The invention relates to the technical field of magnets, in particular to a partial pressure sintering manufacturing method of a neodymium iron boron magnet.
Background
The neodymium-iron-boron magnet is a magnet formed by neodymium, iron, boron and the like, has excellent magnetic performance, and is widely applied to the fields of electronics, electric machinery, medical instruments, toys, packaging, hardware machinery, aerospace and the like. With the development of science and technology and social progress, the performance of the neodymium iron boron magnet is continuously improved, and the neodymium iron boron magnet increasingly plays an important role in modern industrial production. However, the sintered nd-fe-b permanent magnet material in the prior art is generally produced in a vacuum sintering furnace, the sintering process is prone to overburning or under-sintering, the product yield is not high, the mechanical performance and magnetic performance need to be further improved, the preparation process is complex, the production efficiency is not high, and further improvement is needed.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide the partial pressure sintering manufacturing method of the neodymium iron boron magnet, which is simple and convenient to operate, easy to control, high in production efficiency, stable in product quality, high in product yield, good in mechanical property and magnetic property and beneficial to large-scale production.
The purpose of the invention is realized by the following technical scheme: a partial pressure sintering manufacturing method of a neodymium iron boron magnet comprises the following steps:
(1) taking neodymium iron boron magnet powder, orienting in a magnetic field, and pressing to prepare a green body;
(2) and (3) carrying out isostatic pressing treatment on the green body, then placing the green body in a sintering furnace for partial pressure sintering, and carrying out tempering heat treatment to obtain the neodymium-iron-boron magnet.
The partial pressure sintering manufacturing method of the neodymium iron boron magnet is simple and convenient to operate, easy to control, high in production efficiency and product yield, stable in product quality, good in mechanical property and magnetic property and good in machinability, and is beneficial to large-scale production.
Further, in the step (1), the neodymium iron boron magnet powder is oriented in a force magnetic field of 2.0-2.6T.
Further, in the step (1), the neodymium iron boron magnet powder comprises the following raw materials in percentage by mass: 22-26% of neodymium, 1.0-1.2% of boron, 0.7-1.1% of aluminum, 6.8-7.8% of praseodymium, 0.45-0.6% of nickel, 0.15-0.25% of gallium, 0.13-0.17% of zirconium, 0.18-0.23% of copper, 1.2-1.8% of silicon, 2.5-5% of graphene and the balance of iron.
According to the invention, the graphene is added into the neodymium iron boron alloy powder and is matched with components such as silicon, praseodymium, gallium and the like, so that the main phase crystal grains of the neodymium iron boron alloy are refined, the microstructure is optimized, the coercive force of the neodymium iron boron magnet is improved, and the prepared neodymium iron boron magnet has good mechanical properties and corrosion resistance.
Further, in the step (2), the pressure of the isostatic pressing treatment is 240-300MPa, and the treatment time is 90-150 s.
Further, in the step (2), the partial pressure sintering includes the following steps:
s1, placing the green body in a sintering furnace, vacuumizing until the vacuum degree in the furnace is less than 0.05Pa,
s2, filling argon into the sintering furnace, keeping the pressure at 80-120Pa, heating to 280 ℃ at the speed of 2-3 ℃/min, heating to the specified temperature, and then preserving the heat, wherein the total time of heating and preserving the heat is 180 min;
s3, continuously filling argon into the sintering furnace, keeping the pressure at 150-;
s4, continuously filling argon into the sintering furnace, keeping the pressure at 250-300Pa, heating to 800-850 ℃ at the speed of 2-3 ℃/min, and then preserving heat, wherein the total time of heating and preserving heat is 120-180 min;
s5, stopping filling the argon, keeping the pressure at 300Pa for 250-.
According to the invention, the partial pressure sintering is carried out by adopting the steps, the technological parameters such as sintering temperature, pressure and the like are controlled, the pressure difference between the gas inside the neodymium iron boron magnet green body and the gas outside a sintering furnace of the neodymium iron boron magnet green body in the sintering process is favorably reduced, the strength of gas deflation is reduced, the blank internal cracking is prevented, the neodymium iron boron magnet green body can be well protected in the argon atmosphere, the green body is protected from being oxidized easily, the temperature consistency during sintering is good, the consistency and uniformity of magnetic properties are ensured, the sintering time is favorably saved, the production efficiency is improved, the technological steps are easy to control, the production efficiency is high, the product quality is stable, the product yield is high, the mechanical properties and the magnetic properties are good, and.
Further, in the step (3), a tertiary tempering treatment is performed. The temperature of the first-stage tempering heat treatment is 870 plus 960 ℃, and the heat preservation time is 120 plus 180 min; the temperature of the second-stage tempering heat treatment is 620-690 ℃, and the heat preservation time is 120-180 min; the temperature of the third-stage tempering heat treatment is 560-. According to the invention, through carrying out three times of tempering treatment on the sintered neodymium iron boron magnet green body, the neodymium iron boron magnet has uniform and stable crystal grains, the coercive force or residual magnetism of the sintered neodymium iron boron magnet is improved, and the neodymium iron boron magnet has good mechanical strength, corrosion resistance and high temperature resistance, and is suitable for being used in a humid environment.
The invention has the beneficial effects that: the partial pressure sintering manufacturing method of the neodymium iron boron magnet is simple and convenient to operate, easy to control, high in production efficiency and product yield, stable in product quality, good in mechanical property and magnetic property, good in machinability, not prone to cracking, and beneficial to large-scale production.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
In this embodiment, a partial pressure sintering manufacturing method of a neodymium iron boron magnet includes the following steps:
(1) taking neodymium iron boron magnet powder, orienting in a magnetic field, and pressing to prepare a green body;
(2) and (3) carrying out isostatic pressing treatment on the green body, then placing the green body in a sintering furnace for partial pressure sintering, and carrying out tempering heat treatment to obtain the neodymium-iron-boron magnet.
Further, in the step (1), the neodymium iron boron magnet powder is oriented in a force magnetic field of 2.2T.
Further, in the step (1), the neodymium iron boron magnet powder comprises the following raw materials in percentage by mass: 24% of neodymium, 1.0% of boron, 0.9% of aluminum, 7% of praseodymium, 0.48% of nickel, 0.185% of gallium, 0.14% of zirconium, 0.19% of copper, 1.5% of silicon, 3.2% of graphene and the balance of iron.
Further, in the step (2), the pressure of the isostatic pressing treatment is 270MPa, and the treatment time is 120 s.
Further, in the step (2), the partial pressure sintering includes the following steps:
s1, placing the green body in a sintering furnace, vacuumizing until the vacuum degree in the furnace is less than 0.05Pa,
s2, filling argon into the sintering furnace, keeping the pressure at 100Pa, heating to 260 ℃ at the speed of 2.5 ℃/min, and keeping the temperature after heating to the specified temperature, wherein the total time of heating and keeping the temperature is 160 min;
s3, continuously filling argon into the sintering furnace, keeping the pressure at 180Pa, heating to 620 ℃ at the speed of 2.8 ℃/min, and then preserving heat, wherein the total time of heating and preserving heat is 160 min;
s4, continuously filling argon into the sintering furnace, keeping the pressure at 270Pa, heating to 830 ℃ at the speed of 2.5 ℃/min, and then preserving heat, wherein the total time of heating and preserving heat is 150 min;
and S5, stopping filling the argon, vacuumizing until the vacuum degree in the furnace is less than 0.1Pa, heating to 1060 ℃ at the speed of 3.5 ℃/min, heating to the specified temperature, and then preserving the heat for 200 min.
Further, in the step (3), a tertiary tempering treatment is performed. The temperature of the first-stage tempering heat treatment is 900 ℃, and the heat preservation time is 160 min; the temperature of the second-stage tempering heat treatment is 660 ℃, and the heat preservation time is 150 min; the temperature of the third-stage tempering heat treatment is 580 ℃, and the heat preservation time is 90 min.
Example 2
In this embodiment, a partial pressure sintering manufacturing method of a neodymium iron boron magnet includes the following steps:
(1) taking neodymium iron boron magnet powder, orienting in a magnetic field, and pressing to prepare a green body;
(2) and (3) carrying out isostatic pressing treatment on the green body, then placing the green body in a sintering furnace for partial pressure sintering, and carrying out tempering heat treatment to obtain the neodymium-iron-boron magnet.
Further, in the step (1), the neodymium iron boron magnet powder is oriented in a force magnetic field of 2.0T.
Further, in the step (1), the neodymium iron boron magnet powder comprises the following raw materials in percentage by mass: 22% of neodymium, 1.0% of boron, 0.7% of aluminum, 7.8% of praseodymium, 0.45% of nickel, 0.25% of gallium, 0.13% of zirconium, 0.23% of copper, 1.2% of silicon, 5% of graphene and the balance of iron.
Further, in the step (2), the pressure of the isostatic pressing treatment is 240MPa, and the treatment time is 150 s.
Further, in the step (2), the partial pressure sintering includes the following steps:
s1, placing the green body in a sintering furnace, vacuumizing until the vacuum degree in the furnace is less than 0.05Pa,
s2, filling argon into the sintering furnace, keeping the pressure at 80Pa, heating to 240 ℃ at the speed of 2 ℃/min, and then preserving the heat after heating to the specified temperature, wherein the total time of heating and preserving the heat is 210 min;
s3, continuously filling argon into the sintering furnace, keeping the pressure at 150Pa, heating to 600 ℃ at the speed of 2 ℃/min, and then preserving heat, wherein the total time of heating and preserving heat is 120 min;
s4, continuously filling argon into the sintering furnace, keeping the pressure at 2500Pa, heating to 800 ℃ at the speed of 2 ℃/min, and then preserving heat, wherein the total time of heating and preserving heat is 180 min;
and S5, stopping filling the argon, vacuumizing until the vacuum degree in the furnace is less than 0.1Pa, heating to 1020 ℃ at the speed of 3 ℃/min, and preserving the heat after the temperature is raised to the specified temperature for 240 min.
Further, in the step (3), a tertiary tempering treatment is performed. The temperature of the first-stage tempering heat treatment is 870 ℃, and the heat preservation time is 180 min; the temperature of the second-stage tempering heat treatment is 620 ℃, and the heat preservation time is 180 min; the temperature of the third-stage tempering heat treatment is 610 ℃, and the heat preservation time is 60 min.
Example 3
In this embodiment, a partial pressure sintering manufacturing method of a neodymium iron boron magnet includes the following steps:
(1) taking neodymium iron boron magnet powder, orienting in a magnetic field, and pressing to prepare a green body;
(2) and (3) carrying out isostatic pressing treatment on the green body, then placing the green body in a sintering furnace for partial pressure sintering, and carrying out tempering heat treatment to obtain the neodymium-iron-boron magnet.
Further, in the step (1), the neodymium iron boron magnet powder is oriented in a force magnetic field of 2.6T.
Further, in the step (1), the neodymium iron boron magnet powder comprises the following raw materials in percentage by mass: 26% of neodymium, 1.3% of boron, 1.1% of aluminum, 6.8% of praseodymium, 0.6% of nickel, 0.15% of gallium, 0.17% of zirconium, 0.18% of copper, 1.8% of silicon, 2.5% of graphene and the balance of iron.
Further, in the step (2), the pressure of the isostatic pressing treatment is 300MPa, and the treatment time is 90 s.
Further, in the step (2), the partial pressure sintering includes the following steps:
s1, placing the green body in a sintering furnace, vacuumizing until the vacuum degree in the furnace is less than 0.05Pa,
s2, filling argon into the sintering furnace, keeping the pressure at 120Pa, heating to 280 ℃ at a speed of 3 ℃/min, and then keeping the temperature after heating to the specified temperature, wherein the total time of heating and keeping the temperature is 150 min;
s3, continuously filling argon into the sintering furnace, keeping the pressure at 200Pa, heating to 650 ℃ at the speed of 3 ℃/min, and then preserving heat, wherein the total time of heating and preserving heat is 180 min;
s4, continuously filling argon into the sintering furnace, keeping the pressure at 300Pa, heating to 850 ℃ at a speed of 3 ℃/min, and then preserving heat, wherein the total time of heating and preserving heat is 120 min;
and S5, stopping filling the argon, vacuumizing until the vacuum degree in the furnace is less than 0.1Pa, heating to 1120 ℃ at a speed of 4 ℃/min, and preserving the heat after the temperature is raised to the specified temperature, wherein the heat preservation time is 180 min.
Further, in the step (3), a tertiary tempering treatment is performed. The temperature of the first-stage tempering heat treatment is 960 ℃, and the heat preservation time is 120 min; the temperature of the second-stage tempering heat treatment is 690 ℃, and the heat preservation time is 120 min; the temperature of the third-stage tempering heat treatment is 560 ℃, and the heat preservation time is 120 min.
Example 4
In this embodiment, a partial pressure sintering manufacturing method of a neodymium iron boron magnet includes the following steps:
(1) taking neodymium iron boron magnet powder, orienting in a magnetic field, and pressing to prepare a green body;
(2) and (3) carrying out isostatic pressing treatment on the green body, then placing the green body in a sintering furnace for partial pressure sintering, and carrying out tempering heat treatment to obtain the neodymium-iron-boron magnet.
Further, in the step (1), the neodymium iron boron magnet powder is oriented in a force magnetic field of 2.0-2.6T.
Further, in the step (1), the neodymium iron boron magnet powder comprises the following raw materials in percentage by mass: 23% of neodymium, 1.1% of boron, 0.8% of aluminum, 7% of praseodymium, 0.48% of nickel, 0.22% of gallium, 0.14% of zirconium, 0.2% of copper, 1.5% of silicon, 4% of graphene and the balance of iron.
Further, in the step (2), the pressure of the isostatic pressing treatment is 250MPa, and the treatment time is 120 s.
Further, in the step (2), the partial pressure sintering includes the following steps:
s1, placing the green body in a sintering furnace, vacuumizing until the vacuum degree in the furnace is less than 0.05Pa,
s2, filling argon into the sintering furnace, keeping the pressure at 90Pa, heating to 260 ℃ at the speed of 2.5 ℃/min, and keeping the temperature after heating to the specified temperature, wherein the total time of heating and keeping the temperature is 140 min;
s3, continuously filling argon into the sintering furnace, keeping the pressure at 170Pa, heating to 610 ℃ at the speed of 2 ℃/min, and then preserving heat, wherein the total time of heating and preserving heat is 150 min;
s4, continuously filling argon into the sintering furnace, keeping the pressure at 270Pa, heating to 830 ℃ at a speed of 3 ℃/min, and then preserving heat, wherein the total time of heating and preserving heat is 160 min;
and S5, stopping filling the argon, vacuumizing until the vacuum degree in the furnace is less than 0.1Pa, heating to 1100 ℃ at the speed of 3.5 ℃/min, heating to the specified temperature, and then preserving the heat for 210 min.
Further, in the step (3), a tertiary tempering treatment is performed. The temperature of the first-stage tempering heat treatment is 920 ℃, and the heat preservation time is 150 min; the temperature of the second-stage tempering heat treatment is 640 ℃, and the heat preservation time is 140 min; the temperature of the third-stage tempering heat treatment is 590 ℃, and the heat preservation time is 100 min.
Comparative example 1
This comparative example differs from the examples in that:
in the comparative example, the partial pressure sintering manufacturing method of the neodymium iron boron magnet comprises the following steps:
(1) taking neodymium iron boron magnet powder, orienting in a magnetic field, and pressing to prepare a green body;
(2) and (3) carrying out isostatic pressing treatment on the green body, then placing the green body in a sintering furnace for vacuum sintering, and carrying out tempering heat treatment to obtain the neodymium-iron-boron magnet.
In the step (2), the sintering comprises the following steps:
s1, placing the green body in a sintering furnace, vacuumizing until the vacuum degree in the furnace is less than 0.05Pa,
s2, heating to 260 ℃ at the speed of 2.5 ℃/min, and preserving heat after heating to the specified temperature, wherein the total time of heating and preserving heat is 150 min;
s3, heating to 620 ℃ at the speed of 2.8 ℃/min, and then preserving heat, wherein the total time of heating and preserving heat is 160 min;
s4, heating to 830 ℃ at the speed of 2.5 ℃/min, and then preserving heat, wherein the total time of heating and preserving heat is 150 min;
and S5, heating to 1060 ℃ at the speed of 3.5 ℃/min, heating to the specified temperature, and then preserving heat for 200 min.
The remainder of this comparative example is similar to example 1 and will not be described again here.
The Nd-Fe-B magnets of examples 1-4 were prepared as cylinder magnets with a height of 250mm × 25mm, and the observation and performance measurement of examples 1-4 were carried out according to GB/T13560-:
item Maximum magnetic energy product Intrinsic coercive force Compressive strength
Unit of MGoe KA/m N/mm2
Example 1 54 1017 1063
Example 2 52 1001 1057
Example 3 51 1026 1071
Example 4 50 1037 1052
Comparative example 1 46 1011 987
After the surface of the neodymium iron boron magnet of the embodiment 1-4 of the invention is flat, no crack is found, and the neodymium iron boron magnet of the comparative example 1 has fine cracks. The shape deviation of the coaxiality of the examples 1 to 4 is measured, and the deviation of the sintering surface of the example 1 is within +/-0.3 mm; the variation of the sintered surface of example 2 was within. + -. 0.3mm, the variation of the sintered surface of example 3 was within. + -. 0.4mm, and the variation of the sintered surface of example 4 was within. + -. 0.3 mm.
The partial pressure sintering manufacturing method of the neodymium iron boron magnet is simple and convenient to operate, easy to control, high in production efficiency and product yield, stable in product quality, good in mechanical property and magnetic property, good in machinability, not prone to cracking, and beneficial to large-scale production.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.

Claims (7)

1. A partial pressure sintering manufacturing method of a neodymium iron boron magnet is characterized by comprising the following steps: the method comprises the following steps:
(1) taking neodymium iron boron magnet powder, orienting in a magnetic field, and pressing to prepare a green body;
(2) and (3) carrying out isostatic pressing treatment on the green body, then placing the green body in a sintering furnace for partial pressure sintering, and carrying out tempering heat treatment to obtain the neodymium-iron-boron magnet.
2. The method for manufacturing a neodymium-iron-boron magnet according to claim 1, which is characterized in that: in the step (1), the neodymium iron boron magnet powder is oriented in a force magnetic field of 2.0-2.6T.
3. The method for manufacturing a neodymium-iron-boron magnet according to claim 1, which is characterized in that: in the step (2), the pressure of the isostatic pressing treatment is 240-300MPa, and the treatment time is 90-150 s.
4. The method for manufacturing a neodymium-iron-boron magnet according to claim 1, which is characterized in that: in the step (2), the partial pressure sintering comprises the following steps:
s1, placing the green body in a sintering furnace, vacuumizing until the vacuum degree in the furnace is less than 0.05Pa,
s2, filling argon into the sintering furnace, keeping the pressure at 80-120Pa, heating to 280 ℃ at the speed of 2-3 ℃/min, heating to the specified temperature, and then preserving the heat, wherein the total time of heating and preserving the heat is 180 min;
s3, continuously filling argon into the sintering furnace, keeping the pressure at 150-;
s4, continuously filling argon into the sintering furnace, keeping the pressure at 250-300Pa, heating to 800-850 ℃ at the speed of 2-3 ℃/min, and then preserving heat, wherein the total time of heating and preserving heat is 120-180 min;
s5, stopping filling the argon, vacuumizing until the vacuum degree in the furnace is less than 0.1Pa, heating to 1020-.
5. The method for manufacturing a neodymium-iron-boron magnet according to claim 1, which is characterized in that: and (4) in the step (3), carrying out three-stage tempering treatment.
6. The method for manufacturing a neodymium-iron-boron magnet according to claim 5, which is characterized in that: in the step (3), the temperature of the first-stage tempering heat treatment is 870-; the temperature of the second-stage tempering heat treatment is 620-690 ℃, and the heat preservation time is 120-180 min; the temperature of the third-stage tempering heat treatment is 560-.
7. The method for manufacturing a neodymium-iron-boron magnet according to claim 1, which is characterized in that: in the step (1), the neodymium iron boron magnet powder comprises the following raw materials in percentage by mass: 22-26% of neodymium, 1.0-1.2% of boron, 0.7-1.1% of aluminum, 6.8-7.8% of praseodymium, 0.45-0.6% of nickel, 0.15-0.25% of gallium, 0.13-0.17% of zirconium, 0.18-0.23% of copper, 1.2-1.8% of silicon, 2.5-5% of graphene and the balance of iron.
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CN113948303A (en) * 2021-10-20 2022-01-18 合肥工业大学 High-yield and high-performance sintered NdFeB radiation ring and preparation method thereof
CN114267532A (en) * 2021-12-27 2022-04-01 东莞市嘉达磁电制品有限公司 Processing method of high-magnetism sintered neodymium-iron-boron magnet
CN114267532B (en) * 2021-12-27 2024-04-09 东莞市嘉达磁电制品有限公司 Processing method of high-magnetism sintered NdFeB magnet

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