CN115798916A - Infiltration method of sintered neodymium-iron-boron magnet and high-performance sintered neodymium-iron-boron magnet - Google Patents
Infiltration method of sintered neodymium-iron-boron magnet and high-performance sintered neodymium-iron-boron magnet Download PDFInfo
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Abstract
The invention provides a permeation method of a sintered neodymium-iron-boron magnet and a high-performance sintered neodymium-iron-boron magnet. Compared with the non-pressure permeation, the process can recover the verticality of the magnet, can more easily diffuse heavy rare earth elements into the interior of the magnet, can effectively improve the coercive force of the sintered neodymium-iron-boron magnet, and can effectively improve the problem of magnet deformation after diffusion heat treatment through pressure tempering treatment.
Description
Technical Field
The invention relates to the field of rare earth permanent magnet materials, in particular to a permeation method of a sintered neodymium-iron-boron magnet and a high-performance sintered neodymium-iron-boron magnet.
Background
The sintered Nd-Fe-B magnet is widely applied to various fields such as household appliances, intelligent electronic equipment, new energy automobiles, wind power generation and the like by virtue of excellent magnetic performance, is an indispensable functional material in emerging industries and high and new technical fields at present, and promotes the development of modern information technology and industrial development to the directions of integration, intellectualization and miniaturization. After technical innovation, process improvement and equipment optimization for decades, the current maximum magnetic energy and remanence of the sintered neodymium-iron-boron magnet can reach more than 90% of a theoretical value, but the coercive force can only reach one third of the theoretical value. Therefore, how to improve the coercive force of the sintered neodymium iron boron magnet on the premise of keeping higher maximum magnetic energy and remanence becomes a research hotspot in recent years.
However, the effective diffusion depth of the prior art using grain boundary diffusion alone is very limited, and the prior art can only be applied to very thin bulk magnets. In addition, insufficient driving force of the diffusant to the grain boundary of the sintered neodymium iron boron magnet also causes uneven distribution of the diffusant in the magnet, which in turn causes large surface coercivity of the magnet, and relatively low internal coercivity, which inevitably reduces the squareness of the magnet after diffusion. Therefore, it is imperative to enhance the diffusion driving force and to enhance the effective diffusion depth of the magnet.
In view of the problems and disadvantages of the prior art, further improvement and development of the infiltration method of sintered nd-fe-b magnet is needed.
Disclosure of Invention
The invention provides a sintered neodymium-iron-boron magnet, a permeation method and a sintered neodymium-iron-boron magnet with high coercivity, and the specific technical scheme is as follows:
the infiltration method of the sintered neodymium-iron-boron magnet comprises the following steps:
depositing a diffusion source on the surface of the sintered neodymium-iron-boron magnet, and performing sectional gradient pressure permeation diffusion treatment on the magnet subjected to diffusion source deposition to obtain the sintered neodymium-iron-boron magnet with high coercivity;
further, the pretreatment steps before the surface of the sintered neodymium iron boron magnet is deposited with the diffusion source are as follows: polishing the surface of the neodymium iron boron magnet, sequentially performing ultrasonic treatment on the surface of the neodymium iron boron magnet by using distilled water, dilute nitric acid solution and absolute ethyl alcohol, and drying the surface of the neodymium iron boron magnet;
further, the diffusion source is heavy rare earth Dy, heavy rare earth Tb, an alloy containing Dy component, a compound or an alloy containing Tb component, a compound;
further, the method for depositing the diffusion source on the surface of the sintered neodymium-iron-boron magnet comprises the following specific steps: depositing diffusion sources on two surfaces of the sintered NdFeB magnet, which are vertical to the direction of the easy magnetization axis;
further, the deposition manner includes but is not limited to magnetron sputtering, coating, electrophoretic deposition;
further, the deposited sintered NdFeB magnet obtains a Tb film or Dy film with the thickness of 4-10 mu m;
further, the step gradient pressure infiltration diffusion treatment comprises diffusion heat treatment and pressure tempering treatment, wherein the pressure of the diffusion heat treatment is 2-10MPa, and the pressure of the pressure tempering treatment is 1-5MPa;
further, the pressure of diffusion heat treatment is 8MPa, and the pressure of pressure tempering treatment is 3MPa;
further, the diffusion temperature of the diffusion heat treatment is 800-900 ℃, and the temperature of the pressure tempering treatment is 450-490 ℃;
furthermore, the diffusion time of the diffusion heat treatment is 5-8 hours, and the heat preservation time of the pressure tempering treatment is 1-3 hours;
in addition, the invention also provides a high-performance sintered neodymium-iron-boron magnet obtained by the infiltration method of the sintered neodymium-iron-boron magnet.
Due to the adoption of the technical scheme, the invention has the beneficial technical effects that:
1. compared with the method without pressure permeation, the method can recover the verticality of the magnet, can more easily diffuse heavy rare earth elements into the interior of the magnet, and can effectively improve the coercive force of the sintered neodymium iron boron magnet;
2. the problem of magnet deformation after diffusion heat treatment can be effectively solved through the pressure tempering treatment;
3. the enhancement of the diffusion driving force of the invention can not only improve the effective depth of diffusion and improve the coercive force and squareness of the magnet, but also improve the efficiency of grain boundary diffusion and reduce the energy consumption.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The infiltration method of the sintered neodymium-iron-boron magnet comprises the following steps: and depositing a diffusion source on the surface of the sintered neodymium-iron-boron magnet, and performing sectional gradient pressure permeation diffusion treatment on the magnet after the deposition of the diffusion source to obtain the sintered neodymium-iron-boron magnet with high coercivity. The step gradient pressure infiltration diffusion treatment comprises diffusion heat treatment and pressure tempering treatment, wherein the pressure of the diffusion heat treatment is 2-10MPa, and the pressure of the pressure tempering treatment is 1-5MPa. After the magnet subjected to the deposition of the diffusion source is subjected to the step gradient pressure permeation diffusion, the efficiency of grain boundary diffusion can be effectively improved, and the high-coercivity sintered neodymium-iron-boron magnet is prepared. The air pressure value of diffusion heat treatment and the air pressure value of pressurization tempering treatment form different gradients, compared with non-pressure permeation, the verticality of the magnet can be recovered, heavy rare earth elements can be more easily diffused into the magnet, the coercive force of the sintered neodymium-iron-boron magnet can be effectively improved, and the problem of magnet deformation after diffusion heat treatment can be effectively solved by pressure tempering.
The pretreatment steps before the surface of the sintered neodymium-iron-boron magnet is deposited with the diffusion source are as follows: polishing the surface of the neodymium iron boron magnet, sequentially performing ultrasonic treatment on the surface of the neodymium iron boron magnet by using distilled water, dilute nitric acid solution and absolute ethyl alcohol, and drying the surface of the neodymium iron boron magnet after ultrasonic treatment for 5min, 30s and 5min respectively, thereby obtaining the magnet with a clean surface and to be deposited.
The diffusion source is heavy rare earth Dy, heavy rare earth Tb, alloy and compound containing Dy or alloy and compound containing Tb, and the sintered neodymium-iron-boron magnet surface deposition diffusion source comprises the following specific steps: depositing Dy or Tb on two surfaces of the sintered NdFeB magnet perpendicular to the direction of the easy magnetization axis by means of magnetron sputtering, coating or electrophoretic deposition, placing a magnet sample to be sputtered and deposited at a sample table in a magnetron sputtering furnace chamber, vacuumizing to 1 x 10 by adopting 99.9wt.% of high-purity Tb target or Dy target as the target material -3 -1×10 -4 And Pa, filling argon, and controlling the sputtering time to obtain Tb films or Dy films with different thicknesses, wherein the thickness of the heavy rare earth Tb film layer or Dy film is 4-10 mu m.
Example 1
A penetration method of a sintered NdFeB magnet comprises the following steps:
(1) Pretreatment before the surface of the sintered neodymium iron boron magnet is deposited with a diffusion source:
selecting a sintered NdFeB magnet with the grade of N40H as a diffusion substrate, and carrying out linear cutting on the sintered NdFeB magnet to form a square sample with the size of 15mm multiplied by 10mm multiplied by 3mm, wherein the sample size along the direction of the easy magnetization axis is 3mm;
and (3) polishing the surface of the magnet sample by using sand paper until the surface is smooth and flat, sequentially performing ultrasonic treatment on the cleaned magnet sample by using distilled water for 5min, 5wt.% dilute nitric acid solution for 30s and absolute ethyl alcohol for 5min, and drying the surface of the magnet.
(2) Deposition of a diffusion source:
tb is deposited on two surfaces of the magnet sample perpendicular to the direction of the easy magnetization axis, the magnet sample to be sputtered and deposited is placed on a sample table in a magnetron sputtering furnace chamber, 99.9wt.% of high-purity Tb target is adopted as the target material, and the vacuum degree is reduced to 1 x 10 -3 Below Pa, argon gas and working gas are filledThe pressure is 0.6-0.8Pa, tb films with different thicknesses are obtained by controlling the sputtering time, and the thickness of the plating layer Tb is 6 mu m of each plating surface;
(3) Step-by-step gradient pressure infiltration diffusion treatment:
diffusion heat treatment: performing diffusion heat treatment on a magnet sample to be diffused in an argon high-pressure atmosphere, and pumping the vacuum degree in a diffusion furnace to 9 x 10 -3 Introducing argon under 2MPa below Pa, and performing diffusion heat treatment under the pressure of 2 MPa; diffusion temperature: 850 ℃, diffusion time: for 5 hours.
And (3) tempering: argon pressure is 1MPa, tempering temperature is 450 ℃, and heat preservation time is 1.5 hours, so that the infiltrated sintered neodymium iron boron magnet is obtained.
Example 2
A penetration method of a sintered NdFeB magnet comprises the following steps:
(1) Pretreatment before the surface of the sintered neodymium iron boron magnet is deposited with a diffusion source:
selecting a sintered NdFeB magnet with the grade of N40H as a diffusion substrate, and carrying out wire cutting on the sintered NdFeB magnet to form a square sample with the diameter of 15mm multiplied by 10mm multiplied by 3mm, wherein the size of the sample along the direction of an easy magnetization axis is 3mm;
and (3) polishing the surface of the magnet sample by using sand paper until the surface is smooth and flat, sequentially performing ultrasonic treatment on the cleaned magnet sample by using distilled water for 5min, 5wt.% dilute nitric acid solution for 30s and absolute ethyl alcohol for 5min, and drying the surface of the magnet.
(2) Deposition of a diffusion source:
tb is deposited on two surfaces of the magnet sample perpendicular to the direction of the easy magnetization axis, the magnet sample to be sputtered and deposited is placed on a sample table in a magnetron sputtering furnace chamber, 99.9wt.% of high-purity Tb target is adopted as the target material, and the vacuum degree is reduced to 1 x 10 -3 Introducing argon under Pa, wherein the working pressure is 0.6-0.8Pa, and controlling the sputtering time to obtain Tb films with different thicknesses, wherein the thickness of each plating layer Tb is 4 mu m;
(3) And (3) carrying out segmented gradient pressure infiltration diffusion treatment:
diffusion heat treatment: carrying out diffusion heat treatment on a magnet sample to be diffused in an argon high-pressure atmosphere, pumping the vacuum degree in a diffusion furnace to be less than 9 multiplied by 10 < -3 > Pa, filling argon into the diffusion furnace to be 4MPa, and carrying out diffusion heat treatment under the pressure of 4 MPa; diffusion temperature: 900 ℃, diffusion time: for 6 hours.
And (3) tempering: argon pressure is 1MPa, tempering temperature is 480 ℃, and heat preservation time is 1 hour, so that the infiltrated sintered neodymium-iron-boron magnet is obtained.
Example 3
A penetration method of a sintered neodymium-iron-boron magnet comprises the following steps:
(1) Pretreatment before the surface of the sintered neodymium iron boron magnet is deposited with a diffusion source:
selecting a sintered NdFeB magnet with the grade of N40H as a diffusion substrate, and carrying out wire cutting on the sintered NdFeB magnet to form a square sample with the diameter of 15mm multiplied by 10mm multiplied by 3mm, wherein the size of the sample along the direction of an easy magnetization axis is 3mm;
and (3) polishing the surface of the magnet sample by using sand paper until the surface is smooth and flat, sequentially performing ultrasonic treatment on the cleaned magnet sample by using distilled water for 5min, 5wt.% dilute nitric acid solution for 30s and absolute ethyl alcohol for 5min, and drying the surface of the magnet.
(2) Deposition of a diffusion source:
dy is deposited on two surfaces of a magnet sample perpendicular to the direction of the easy magnetization axis, the magnet sample to be sputtered and deposited is placed on a sample table in a magnetron sputtering furnace chamber, the target material is 99.9wt.% of high-purity Dy target material, and the magnet sample is vacuumized to 1 x 10 -3 Introducing argon under Pa, wherein the working pressure is 0.6-0.8Pa, and controlling the sputtering time to obtain Dy films with different thicknesses, wherein the thickness of each coating Dy is 10 mu m;
(3) Step-by-step gradient pressure infiltration diffusion treatment:
diffusion heat treatment: performing diffusion heat treatment on a magnet sample to be diffused in an argon high-pressure atmosphere, and pumping the vacuum degree in a diffusion furnace to 9 x 10 -3 Introducing argon gas under the pressure of less than Pa, and performing diffusion heat treatment under the pressure of 6 MPa; diffusion temperature: 800 ℃, diffusion time: for 7 hours.
And (3) tempering: argon pressure is 2MPa, tempering temperature is 480 ℃, and heat preservation time is 3 hours, so that the infiltrated sintered neodymium-iron-boron magnet is obtained.
Example 4
A penetration method of a sintered neodymium-iron-boron magnet comprises the following steps:
(1) Pretreatment before the surface of the sintered neodymium iron boron magnet is deposited with a diffusion source:
selecting a sintered NdFeB magnet with the grade of N40H as a diffusion substrate, and carrying out linear cutting on the sintered NdFeB magnet to form a square sample with the size of 15mm multiplied by 10mm multiplied by 3mm, wherein the sample size along the direction of the easy magnetization axis is 3mm;
and (3) polishing the surface of the magnet sample by using sand paper until the surface is smooth and flat, sequentially performing ultrasonic treatment on the cleaned magnet sample by using distilled water for 5min, 5wt.% dilute nitric acid solution for 30s and absolute ethyl alcohol for 5min, and drying the surface of the magnet.
(2) Deposition of a diffusion source:
tb is deposited on two surfaces of the magnet sample perpendicular to the direction of the easy magnetization axis, the magnet sample to be sputtered and deposited is placed on a sample table in a magnetron sputtering furnace chamber, 99.9wt.% of high-purity Tb target is adopted as the target material, and the vacuum degree is reduced to 1 x 10 -3 Introducing argon under Pa, wherein the working pressure is 0.6-0.8Pa, and controlling the sputtering time to obtain Tb films with different thicknesses, wherein the thickness of each plating layer Tb is 8 mu m;
(3) And (3) carrying out segmented gradient pressure infiltration diffusion treatment:
diffusion heat treatment: performing diffusion heat treatment on a magnet sample to be diffused in an argon high-pressure atmosphere, and pumping the vacuum degree in a diffusion furnace to 9 x 10 -3 Introducing argon under the pressure of below Pa, and performing diffusion heat treatment under the pressure of 8 MPa; diffusion temperature: 850 ℃, diffusion time: for 8 hours.
And (3) tempering: the argon pressure is 1MPa, the tempering temperature is 490 ℃, and the heat preservation time is 3 hours, so as to obtain the infiltrated sintered neodymium iron boron magnet.
Example 5
A penetration method of a sintered neodymium-iron-boron magnet comprises the following steps:
(1) Pretreatment before the surface of the sintered neodymium iron boron magnet is deposited with a diffusion source:
selecting a sintered NdFeB magnet with the grade of N40H as a diffusion substrate, and carrying out linear cutting on the sintered NdFeB magnet to form a square sample with the size of 15mm multiplied by 10mm multiplied by 3mm, wherein the sample size along the direction of the easy magnetization axis is 3mm;
and (3) polishing the surface of the magnet sample by using sand paper until the surface is smooth and flat, sequentially performing ultrasonic treatment on the cleaned magnet sample by using distilled water for 5min, 5wt.% dilute nitric acid solution for 30s and absolute ethyl alcohol for 5min, and drying the surface of the magnet.
(2) Deposition of a diffusion source:
tb is deposited on two surfaces of the magnet sample perpendicular to the direction of the easy magnetization axis, the magnet sample to be sputtered and deposited is placed on a sample table in a magnetron sputtering furnace chamber, 99.9wt.% of high-purity Tb target is adopted as the target material, and the vacuum degree is reduced to 1 x 10 -3 Introducing argon under Pa, wherein the working pressure is 0.6-0.8Pa, and controlling the sputtering time to obtain Tb films with different thicknesses, wherein the thickness of each plating layer Tb is 8 mu m;
(3) And (3) carrying out segmented gradient pressure infiltration diffusion treatment:
diffusion heat treatment: performing diffusion heat treatment on a magnet sample to be diffused in an argon high-pressure atmosphere, and pumping the vacuum degree in a diffusion furnace to 9 x 10 -3 Introducing argon under 10MPa below Pa, and performing diffusion heat treatment under the pressure of 10 MPa; diffusion temperature: 850 ℃, diffusion time: for 8 hours.
And (3) tempering: argon pressure is 1MPa, tempering temperature is 490 ℃, and the holding time is 3 hours, obtain the sintered neodymium iron boron magnet after permeating.
Example 6
The same parts of this embodiment as embodiment 1 are not described again, except that: the vacuum degree in the furnace is pumped to 9 multiplied by 10 -3 Introducing argon under the pressure of below Pa, and performing diffusion heat treatment under the pressure of 8 MPa; the argon pressure in the tempering stage was 3MPa.
Example 7
The same parts of this embodiment as embodiment 1 are not described again, except that: the vacuum degree in the furnace is pumped to 9 multiplied by 10 -3 Introducing argon under the pressure of below Pa, and performing diffusion heat treatment under the pressure of 8 MPa; the argon pressure in the tempering stage is 5MPa.
Comparative example 1
The parts of this comparative example that are the same as those in example 1 are not described again, except that:
the heat treatment process is a conventional heat treatment process and does not adopt a pressurizing mode. The parameters of the heat treatment process are as follows: 850 ℃, diffusion time: 5 hours, the tempering temperature is 450 ℃, and the heat preservation time is 1.5 hours.
Comparative example 2
The parts of this comparative example which are the same as those of example 1 are not described again, except that: the vacuum degree in the furnace is pumped to 9 multiplied by 10 -3 Introducing argon under the pressure of below Pa, and performing diffusion heat treatment under the pressure of 8 MPa; the tempering stage is not carried out in a pressure maintaining mode.
The magnetic properties of the high-performance neodymium-iron-boron permanent magnet materials obtained by the examples 1-7 and the comparative examples 1-2 under different pressure diffusion processes are shown in table 1.
TABLE 1 results of magnetic properties of Nd-Fe-B permanent-magnet materials obtained in examples 1-7 and comparative examples 1-2 under different pressure diffusion processes
As can be seen from table 1: compared with the original magnet and the comparative example 1, the sintered neodymium iron boron magnet subjected to segmented pressure diffusion heat treatment can effectively improve the coercive force of the magnet, and compared with the comparative example 1, the squareness after pressure diffusion and permeation has a certain rise, which shows that the uniformity of the coercive force is improved, the internal and external coercive force distribution of the magnet is more uniform, and the depth of the grain boundary diffusion Tb is effectively improved. Meanwhile, the coercive force of the magnet obtained by sectional pressure diffusion is improved by comparing the embodiments 1 to 7 with the comparative example 1. In example 6, the coercive force was the largest when the pressure of the diffusion heat treatment was 8MPa and the pressure at the tempering stage was 3MPa, which was 6.36kOe higher than that of the original magnet; in examples 5 and 7, the pressure of the diffusion heat treatment is 10MPa, which is increased by 5.6kOe and 5.14kOe compared with the coercive force of the original magnet, respectively, but the remanence thereof is also decreased more, and the remanence loss is 0.49kGs and 0.51kGs, respectively, which may be related to the pressure being too large and the heavy rare earth element Tb entering the main phase more.
Compared with the non-pressurized comparative example 2 in the tempering stage, the coercive force of the magnets of the samples of the examples 4 and 6 to 7 is increased to a certain extent, which shows that the pressure in the tempering stage is favorable for promoting the formation of the rare earth-rich phase around the grain boundary and is favorable for improving the coercive force of the magnets. On the other hand, in comparative example 4 and examples 6 to 7, when the pressure at the tempering stage is 3MPa, the coercive force is maximized, and when the coercive force and the remanence are reduced beyond 3MPa, which may be related to the rare earth-rich phase entering the main phase. Meanwhile, the surface of the sample of comparative example 2 was curved, which was not favorable for the subsequent processing, while the surface curvature of the sample of example 4 was slightly improved, and the problem of deformation and warpage of the magnet samples of examples 6 to 7 was improved, without occurrence of warpage.
In summary, it is preferable that the sample performance is optimum when the pressure of the diffusion heat treatment is 8MPa and the pressure at the tempering stage is 3MPa.
Furthermore, it should be understood that although the present specification describes embodiments, not every embodiment includes only a single embodiment, and such description is for clarity purposes only, and it is to be understood that all embodiments may be combined as appropriate by one of ordinary skill in the art to form other embodiments as will be apparent to those of skill in the art from the description herein.
Claims (10)
1. The infiltration method of the sintered NdFeB magnet is characterized in that a diffusion source is deposited on the surface of the sintered NdFeB magnet, and the magnet after deposition of the diffusion source is subjected to sectional gradient pressure infiltration diffusion treatment to obtain the sintered NdFeB magnet with high performance.
2. The infiltration method of sintered NdFeB magnet as claimed in claim 1, wherein the pretreatment step before the deposition of the diffusion source on the surface of the sintered NdFeB magnet is as follows: polishing the surface of the neodymium iron boron magnet, then sequentially carrying out ultrasonic treatment on the surface of the neodymium iron boron magnet by using distilled water, dilute nitric acid solution and absolute ethyl alcohol, and then drying the surface of the neodymium iron boron magnet.
3. The infiltration method of sintered neodymium-iron-boron magnet according to claim 1, characterized in that, the diffusion source is heavy rare earth Dy, heavy rare earth Tb, alloy containing Dy component, compound or alloy containing Tb component, compound.
4. The infiltration method of sintered NdFeB magnet according to claim 3, wherein the surface deposition diffusion source of sintered NdFeB magnet comprises the following specific steps: and depositing diffusion sources on two surfaces of the sintered NdFeB magnet, which are perpendicular to the direction of the easy magnetization axis.
5. The infiltration method of sintered nd-fe-b magnet of claim 4, wherein the sintered nd-fe-b magnet after deposition obtains a Tb film or Dy film of 4-10 μm.
6. The infiltration method of sintered nd-fe-b magnet as claimed in claim 1, wherein the step gradient pressure infiltration diffusion treatment is divided into diffusion heat treatment and pressure tempering treatment, the pressure of diffusion heat treatment is 2-10MPa, and the pressure of pressure tempering treatment is 1-5MPa.
7. The infiltration method of sintered nd-fe-b magnet of claim 6, wherein the pressure of diffusion heat treatment is 8MPa, and the pressure of pressure tempering treatment is 1MPa.
8. The infiltration method of sintered nd-fe-b magnet of claim 6, wherein the diffusion temperature of the diffusion heat treatment is 800-900 ℃ and the temperature of the pressure tempering treatment is 450-490 ℃.
9. The infiltration method of sintered nd-fe-b magnet as claimed in claim 1, wherein the diffusion time of diffusion heat treatment is 5-8 hours, and the holding time of pressure tempering treatment is 1-3 hours.
10. A high performance sintered ndfeb magnet obtained by the infiltration method of a sintered ndfeb magnet according to any one of claims 1 to 9.
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