CN111180191A - Method for preparing high-performance sintered neodymium-iron-boron magnet - Google Patents
Method for preparing high-performance sintered neodymium-iron-boron magnet Download PDFInfo
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- CN111180191A CN111180191A CN202010043820.4A CN202010043820A CN111180191A CN 111180191 A CN111180191 A CN 111180191A CN 202010043820 A CN202010043820 A CN 202010043820A CN 111180191 A CN111180191 A CN 111180191A
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- 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
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- 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
- H01F41/0293—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 diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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Abstract
The invention relates to a method for preparing a high-performance sintered neodymium-iron-boron magnet, belongs to the technical field of rare earth permanent magnet materials, solves the technical problems of high difficulty and long flow of grain boundary diffusion, and comprises the following steps: carrying out vacuum rapid hardening and strip throwing, hydrogen breaking, powder milling by an air flow mill, magnetic field pressing and forming on a neodymium iron boron raw material, sintering at a high temperature, machining a sintered blank, pretreating the surface of the sintered blank, carrying out magnetron sputtering deposition on the surface of the pretreated sintered blank to obtain a diffusion source material, and maintaining the neodymium iron boron blank at 60-950 ℃ in the sputtering deposition process; then, primary heat treatment at 850-950 ℃ and secondary heat treatment at 450-650℃ are carried outAnd (5) processing to obtain the high-performance sintered neodymium-iron-boron magnet. The sputtering target can be: one simple substance metal or alloy composed of a plurality of simple substance metals of Dy, Tb, Ho, Nd and Pr, or (R1)x1(R2)100‑x1‑x2‑x3‑x4Alx2(M1)x3(M2)x4And (3) alloying. The method can effectively improve the coercive force of the neodymium iron boron magnet, is suitable for industrial production, and can obtain better economic benefit.
Description
Technical Field
The invention belongs to the technical field of rare earth permanent magnet materials, and particularly relates to a method for preparing a high-performance sintered neodymium-iron-boron magnet.
Background
With the improvement of the environmental protection requirement, the high-performance sintered neodymium iron boron magnet has wide application prospects in the aspects of new energy automobiles, wind power, variable frequency compressors and the like. It becomes important to improve the coercive force of the magnet to meet the use requirements in a high-temperature environment. The addition of the heavy rare earth elements Dy and Tb in the material is an important way for improving the coercive force of the sintered neodymium-iron-boron magnet, the heavy rare earth elements Dy and Tb can enter main phase grains to improve the anisotropy field of the material, but the saturation magnetization intensity of the main phase can also be reduced, so that the residual magnetism and the maximum magnetic energy product of the material are reduced.
By adopting the process of grain boundary diffusion, heavy rare earth elements are diffused into the magnet from the surface along the grain boundary of the magnet, so that the coercive force of the magnet can be obviously improved under the condition that the remanence and the maximum energy product loss of the neodymium iron boron magnet are small, the using amount of the heavy rare earth is reduced, and the utilization rate of the heavy rare earth is improved. Compared with methods such as coating, dipping and the like, the magnetron sputtering preparation process has firm film layer, controllable thickness and good product consistency. However, the diffusion source alloy and the compound containing the heavy rare earth elements generally have high melting points, large diffusion difficulty, long diffusion time and low diffusion efficiency. Generally, the preparation process of the high-performance neodymium iron boron magnet containing the magnetron sputtering grain boundary diffusion process further includes, after the magnetic field press forming: high-temperature sintering, two-stage heat treatment, surface pretreatment, sputtering deposition, diffusion heat treatment, tempering and the like, and the process flow and the time consumption are long.
Disclosure of Invention
In order to overcome the defects of the prior art and solve the problems of high difficulty and long process of grain boundary diffusion, the invention provides a novel method for preparing a high-performance sintered neodymium-iron-boron magnet, which can effectively improve the coercive force of the neodymium-iron-boron magnet and the utilization rate of a sputtering target material, and in addition, combines the primary heat treatment and diffusion heat treatment process and the secondary heat treatment and tempering treatment process, saves the cost and has better economic benefit.
The invention is realized by the following technical scheme.
A method for preparing a high-performance sintered NdFeB magnet comprises the following steps:
1) sintering the neodymium iron boron raw material for 1-5 hours at 1010-1080 ℃ after vacuum rapid hardening melt spinning, hydrogen breaking, airflow milling powder preparation and magnetic field pressing molding, then naturally cooling to 800-900 ℃, filling normal temperature argon or liquid argon into a sintering furnace, rapidly cooling to below 60 ℃, discharging, and preparing a sintered neodymium iron boron green body;
2) machining the sintered neodymium-iron-boron blank prepared in the step 1), and pretreating the surface of the sintered neodymium-iron-boron blank to enable the sintered neodymium-iron-boron blank to be smooth;
3) performing magnetron sputtering on the surface of the sintered blank pretreated in the step 2) to diffuse source materials, wherein the temperature of the sintered neodymium iron boron blank is maintained at 60-950 ℃ in the magnetron sputtering process;
4) carrying out primary heat treatment on the neodymium iron boron blank prepared in the step 3) in a vacuum or high-purity argon atmosphere at the treatment temperature of 850-950 ℃ for 1-18 hours, and then introducing normal-temperature argon or liquid argon into a heat treatment furnace to cool the neodymium iron boron blank to below 120 ℃;
5) and (3) carrying out secondary heat treatment on the neodymium iron boron blank prepared in the step 4), wherein the treatment temperature is 450-650 ℃, the treatment time is 1-6 hours, then introducing normal-temperature argon or liquid argon into the heat treatment furnace, rapidly cooling to below 60 ℃, and discharging to obtain the high-performance sintered neodymium iron boron magnet.
Further, the diffusion source material in the step 3) depends on the sputtering target material, and the sputtering target material has one or more of Dy, Tb, Ho, Nd and Pr, or (R1)x1(R2)100-x1-x2-x3-x4Alx2(M1)x3(M2)x4Wherein R1 is one or more of heavy rare earth elements Dy, Tb and Ho; r2 is one or two of light rare earth elements Nd and Pr; m1 is one or two of Cu and Mg(ii) a M2 is one or more of Ga, Zn, Ag and Sn; wherein x1, x2, x3 and x4 all represent atomic percentages, wherein x1 is 0-60, x2 is 1-50, x3 is 0-40, and x4 is 0-20. The conventional production process of sintered neodymium iron boron comprises the steps of carrying out vacuum rapid hardening and melt spinning, hydrogen breaking, powder milling by an air flow mill, magnetic field compression molding on a neodymium iron boron raw material, sintering at a high temperature of 1010-1080 ℃, and carrying out primary heat treatment at a temperature close to 900 ℃ and secondary heat treatment at a temperature close to 550 ℃ to obtain a sintered magnet. If grain boundary diffusion is further performed, it is generally necessary to perform machining and surface pretreatment of the sintered magnet, room temperature magnetron sputtering treatment, followed by thermal diffusion treatment and tempering treatment.
The invention provides a method for preparing neodymium iron boron, which comprises the steps of firstly carrying out vacuum rapid hardening and melt spinning, hydrogen breaking, powder milling by an air flow mill, magnetic field compression molding on a neodymium iron boron raw material, sintering at a high temperature of 1010-1080 ℃, processing a sintered neodymium iron boron blank, pretreating the surface of the sintered neodymium iron boron blank, and directly carrying out magnetron sputtering, wherein the sintered neodymium iron boron blank is kept at a high temperature of 60-950 ℃ while sputtering a diffusion source material on the surface of the sintered neodymium iron boron blank. According to Fick's law, because the higher temperature of neodymium iron boron body exists during sputtering, make diffusion source material quality diffusion coefficient improve, sputter target material element diffusion efficiency in the magnet increase, reduced the diffusion degree of difficulty. The maintaining temperature of the sintered neodymium iron boron blank in the magnetron sputtering process in the step 3) can be preferably within 450-700 ℃.
In the step 3), when Dy and Tb elemental metals are selected as diffusion source materials, the coercive force of the magnet prepared by the method can be greatly improved. Considering the high melting point of Dy and Tb, the invention also provides a low melting point (R1)x1(R2)100-x1-x2-x3-x4Alx2(M1)x3(M2)x4The alloy target material is characterized in that R1 is one or more of heavy rare earth elements Dy, Tb and Ho; r2 is one or two of light rare earth elements Nd and Pr; m1 is one or two of Cu and Mg; m2 is one or more of Ga, Zn, Ag and Sn; wherein x1, x2, x3 and x4 are all atomic percentages, wherein x1 is 0-60, x2 is 1-50, x3 is 0-40 and x4 is 0-20.
Compared with Dy and Tb, Pr and Nd have low melting points, and Al, Cu, Mg, Ga, Zn, Ag, Sn and other elements are meltedLower point, it (R1)x1(R2)100-x1-x2-x3-x4Alx2(M1)x3(M2)x4The alloy may have a lower melting point. The invention also provides a non-rare earth target Alx2(M1)x3(M2)x4The elements enter the grain boundary area of the magnet to improve the wettability, so that the main phase grains can be better wrapped, and the coercivity can be improved. In addition, these non-rare earth target elements are less expensive than rare earth elements. The invention adopts magnetron sputtering (R1)x1(R2)100-x1-x2-x3-x4Alx2(M1)x3(M2)x4The low-melting-point target alloy material can be used for obtaining a low-melting-point sputtering film material on the surface of the neodymium iron boron body, when the melting point temperature of the films is controlled to be 400-650 ℃, and meanwhile, the neodymium iron boron body is controlled to be 450-700 ℃ in the step 3), the diffusion source film material deposited on the surface of the neodymium iron boron body can be melted, and can easily enter the magnet from the surface of the neodymium iron boron body along the crystal boundary of the magnet, so that the accumulation of the diffusion source material on the surface of the magnet is reduced.
The invention shortens the conventional process flow, and the step 4) combines the primary heat treatment process of the conventional sintered neodymium-iron-boron magnet and the diffusion heat treatment process of the grain boundary process, so that the repair of the neodymium-rich liquid phase on the surface of the main phase grain can be achieved, and the diffusion source material elements can be further deeply diffused from the surface of the sintered blank body to the interior of the neodymium-iron-boron blank body along the grain boundary channel. And 5) combining the conventional secondary heat treatment process of the sintered neodymium iron boron blank and the tempering treatment process of the grain boundary diffusion process, and further adjusting the phase composition and the microstructure.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a method for preparing a high-performance sintered neodymium-iron-boron magnet, which can obviously improve the coercive force of the magnet, reduce the difficulty of diffusion of a diffusion source material in the magnet, increase the diffusion efficiency, improve the utilization rate of a sputtering target material, save the cost and have better economic benefit under the condition that the residual magnetism and the maximum energy product loss of the neodymium-iron-boron magnet are smaller.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. In addition, it will be apparent to those skilled in the art that various modifications or improvements can be made to the material components and amounts in these embodiments without departing from the spirit and scope of the invention as defined in the appended claims.
Example 1
A method for preparing a high-performance sintered NdFeB magnet comprises the following steps:
1) the neodymium iron boron raw material comprises the following components in percentage by weight: 23 wt% of Nd, 7 wt% of Pr, 0.3 wt% of Dy, 0.1 wt% of Al, 0.1 wt% of Ga, 1 wt% of Co, 0.3 wt% of Cu, 0.2 wt% of Zr, 1 wt% of B and 67 wt% of Fe, vacuum-fast-setting melt-spun, hydrogen-breaking, airflow-milling, pressing and forming in a magnetic field, vacuum-sintering at the temperature of 1065 ℃ for 4 hours, naturally cooling to 900 ℃, filling normal-temperature argon into a sintering furnace, rapidly cooling to 50 ℃ and discharging to obtain a sintered neodymium-iron-boron blank;
2) machining the sintered neodymium iron boron blank prepared in the step 1) to obtain a blank sheet with the thickness of 3 mm, and performing conventional pretreatment on the surface of the sintered neodymium iron boron blank to clean the surface without oil stains so as to prepare for subsequent magnetron sputtering;
3) magnetron sputtering diffusion source material on the surface of the sintered blank pretreated in the step 2), wherein the magnetron sputtering target material is metal Tb, and the background vacuum is 5 multiplied by 10-3Pa, the pressure of sputtering argon is 1Pa, the time is 1 hour, and the temperature of the sintered neodymium iron boron blank is maintained at 500 ℃ in the magnetron sputtering process;
4) putting the neodymium iron boron blank prepared in the step 3) in vacuum of 1 multiplied by 10-3Carrying out primary heat treatment in Pa atmosphere at 900 ℃ for 15 hours, and introducing normal-temperature argon into a heat treatment furnace to cool to below 100 ℃;
5) and (3) carrying out secondary heat treatment on the neodymium iron boron blank prepared in the step 4), wherein the treatment temperature is 530 ℃, the treatment time is 4 hours, then introducing normal-temperature argon into the heat treatment furnace, rapidly cooling to below 60 ℃, and discharging to obtain the high-performance sintered neodymium iron boron magnet.
The room temperature performance of the sintered nd-fe-b magnet prepared in this example 1 was tested: the remanence Br is 13.9kGs, the maximum energy product (BH) max is 48.3MGOe, and the coercive force Hcj is 24.2 kOe.
Example 2
In this example 2, the composition and weight percentage of the ndfeb raw material are the same as those in example 1, except that the sputtering target material has different components, the other process parameters are the same, and the sputtering target material in this example 2 is metal Dy10Nd60Al10Cu16Ga4。
The room temperature performance of the sintered nd-fe-b magnet prepared in this example 2 was tested: the remanence Br is 13.8kGs, the maximum energy product (BH) max is 47.2MGOe, and the coercive force Hcj is 17.1 kOe.
Comparative example 1
The composition and weight percentage of the raw material of neodymium iron boron in the comparative example 1 are the same as those in the example 1, and a magnet is prepared by adopting a conventional sintering process: vacuum rapid hardening and strip throwing, hydrogen breaking, airflow milling to prepare powder, and magnetic field pressing and forming, then vacuum high-temperature sintering is carried out, the sintering temperature is 1065 ℃, heat preservation is carried out for 4 hours, then natural cooling is carried out to 900 ℃, and normal-temperature argon is filled into a sintering furnace to be rapidly cooled to 50 ℃ and discharged, so as to prepare a sintered neodymium iron boron green body; the prepared neodymium iron boron green body is vacuumized by 1 multiplied by 10-3Carrying out primary heat treatment in Pa atmosphere at 900 ℃ for 3 hours, and introducing normal-temperature argon into a heat treatment furnace to cool to below 100 ℃; and then carrying out secondary heat treatment on the neodymium iron boron blank, wherein the treatment temperature is 530 ℃, the time is 4 hours, introducing normal-temperature argon into a heat treatment furnace, quickly cooling to below 60 ℃, discharging to obtain a sintered neodymium iron boron magnet, and measuring the room temperature performance of the sintered neodymium iron boron magnet as follows: the remanence Br is 14.1kGs, the maximum energy product (BH) max is 50MGOe, and the coercive force Hcj is 15 kOe.
Compared with the comparative example 1, the coercive force of the neodymium iron boron magnet can be obviously improved in the embodiments 1 and 2, which is caused by the fact that the diffusion source material sputtered on the neodymium iron boron sintered blank by magnetron sputtering in the embodiments can efficiently enter the neodymium iron boron sintered blank and effectively improve the coercive force.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention should be protected by the following claims.
Claims (2)
1. A method for preparing a high-performance sintered NdFeB magnet is characterized by comprising the following steps:
1) sintering the neodymium iron boron raw material for 1-5 hours at 1010-1080 ℃ after vacuum rapid hardening melt spinning, hydrogen breaking, airflow milling powder preparation and magnetic field pressing molding, then naturally cooling to 800-900 ℃, filling normal temperature argon or liquid argon into a sintering furnace, rapidly cooling to below 60 ℃, discharging, and preparing a sintered neodymium iron boron green body;
2) machining the sintered neodymium-iron-boron blank prepared in the step 1), and pretreating the surface of the sintered neodymium-iron-boron blank to enable the sintered neodymium-iron-boron blank to be smooth;
3) performing magnetron sputtering on the surface of the sintered blank pretreated in the step 2) to diffuse source materials, wherein the temperature of the sintered neodymium iron boron blank is maintained at 60-950 ℃ in the magnetron sputtering process;
4) carrying out primary heat treatment on the neodymium iron boron blank prepared in the step 3) in a vacuum or high-purity argon atmosphere at the treatment temperature of 850-950 ℃ for 1-18 hours, and then introducing normal-temperature argon or liquid argon into a heat treatment furnace to cool the neodymium iron boron blank to below 120 ℃;
5) and (3) carrying out secondary heat treatment on the neodymium iron boron blank prepared in the step 4), wherein the treatment temperature is 450-650 ℃, the treatment time is 1-6 hours, then introducing normal-temperature argon or liquid argon into the heat treatment furnace, rapidly cooling to below 60 ℃, and discharging to obtain the high-performance sintered neodymium iron boron magnet.
2. The method for preparing a high-performance sintered neodymium-iron-boron magnet according to claim 1, characterized in that: the diffusion source material in the step 3) depends on a sputtering target material, and the sputtering target material comprises one or more of Dy, Tb, Ho, Nd and Pr, or (R1)x1(R2)100-x1-x2-x3-x4Alx2(M1)x3(M2)x4Wherein R1 is one or more of heavy rare earth elements Dy, Tb and Ho; r2 is one or two of light rare earth elements Nd and PrSeed growing; m1 is one or two of Cu and Mg; m2 is one or more of Ga, Zn, Ag and Sn; wherein x1, x2, x3 and x4 all represent atomic percentages, wherein x1 is 0-60, x2 is 1-50, x3 is 0-40, and x4 is 0-20.
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Cited By (6)
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| CN112466645A (en) * | 2020-11-23 | 2021-03-09 | 北京麦戈龙科技有限公司 | Method for preparing rare earth permanent magnet |
| CN112725675A (en) * | 2020-12-23 | 2021-04-30 | 苏州希镝瑞新材料科技有限公司 | Method for manufacturing dysprosium/terbium target |
| CN113421761A (en) * | 2021-06-12 | 2021-09-21 | 山西汇镪磁性材料制作有限公司 | Preparation method of high-performance sintered neodymium iron boron capable of reducing adsorption energy of modified magnetic powder |
| CN114284057A (en) * | 2022-03-08 | 2022-04-05 | 山西金山磁材有限公司 | Neodymium iron boron particle continuous composite coating device and method for regulating and controlling depth of neodymium iron boron crystal boundary |
| CN115383122A (en) * | 2022-08-25 | 2022-11-25 | 太原科技大学 | Hydrogen crushing preparation method of 2 |
| CN115512954A (en) * | 2022-09-23 | 2022-12-23 | 安徽省瀚海新材料股份有限公司 | Method for improving consistency of intrinsic coercivity of sintered neodymium iron boron |
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