CN118197785A - Preparation method of fully dense anisotropic composite magnet - Google Patents
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- CN118197785A CN118197785A CN202410370393.9A CN202410370393A CN118197785A CN 118197785 A CN118197785 A CN 118197785A CN 202410370393 A CN202410370393 A CN 202410370393A CN 118197785 A CN118197785 A CN 118197785A
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- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title abstract 3
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 50
- 239000000956 alloy Substances 0.000 claims abstract description 50
- 238000010438 heat treatment Methods 0.000 claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000000137 annealing Methods 0.000 claims abstract description 13
- 238000005324 grain boundary diffusion Methods 0.000 claims abstract description 13
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 10
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000010949 copper Substances 0.000 claims description 26
- 238000005245 sintering Methods 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- 238000007578 melt-quenching technique Methods 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 230000006698 induction Effects 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 2
- 239000000696 magnetic material Substances 0.000 abstract description 5
- 238000010791 quenching Methods 0.000 abstract description 3
- 230000000171 quenching effect Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000000155 melt Substances 0.000 abstract description 2
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 description 2
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
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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
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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
- H01F41/0273—Imparting anisotropy
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
Description
技术领域Technical Field
本发明涉及磁性材料技术领域，尤其涉及一种全致密各向异性复合磁体的制备方法。The invention relates to the technical field of magnetic materials, and in particular to a method for preparing a fully dense anisotropic composite magnet.
背景技术Background technique
作为一种重要的功能材料，磁性材料在现代社会里扮演着极为重要的角色。特别是永磁材料的生产和开发应用程度是现代国家经济发展的标志之一。SmFe12合金发现于1980年代，因ThMn12型合金相为亚稳态相，造成其内禀磁参量一直未被测定，加之RE2Fe14B系永磁材料的冲击，SmFe12合金并未受到足够的重视，也大大延缓了其实用化进程。同时，SmCo7型合金具有高磁晶各向异性场、高居里温度和高温度稳定性而备受关注。但由于SmCo7型结构不稳定，制备单相合金较为困难，通常采用熔体快淬加等温回火、化学辅助高能球磨及超高压热变形等工艺使得晶粒纳米化并获得一定的磁各向异性。As an important functional material, magnetic materials play an extremely important role in modern society. In particular, the production, development and application of permanent magnetic materials is one of the signs of modern national economic development. SmFe 12 alloy was discovered in the 1980s. Because the ThMn 12 alloy phase is a metastable phase, its intrinsic magnetic parameters have not been measured. In addition, due to the impact of RE 2 Fe 14 B permanent magnetic materials, SmFe 12 alloy has not received enough attention, which has greatly delayed its practical application process. At the same time, SmCo 7 alloy has attracted much attention due to its high magnetocrystalline anisotropy field, high Curie temperature and high temperature stability. However, due to the unstable structure of SmCo 7 , it is difficult to prepare single-phase alloys. Usually, processes such as melt rapid quenching plus isothermal tempering, chemical-assisted high-energy ball milling and ultra-high pressure hot deformation are used to nano-size the grains and obtain a certain magnetic anisotropy.
为此，本发明采用熔体快淬法分别制备Sm(Fe,TM)12和Sm(Fe,TM)7合金薄带，并通过高能球磨技术制备低熔点Dy20Tb30Cu25Co25合金粉末，随后将Sm(Fe,TM)12合金、Sm(Fe,TM)7合金及Dy20Tb30Cu25Co25合金粉末按比例混合后进行放电等离子烧结及后续磁场下的一级晶界扩散热处理和二级退火热处理，最终获得全致密各向异性复合磁体。To this end, the present invention adopts a melt rapid quenching method to prepare Sm(Fe, TM) 12 and Sm(Fe, TM) 7 alloy thin strips respectively, and prepares low melting point Dy 20 Tb 30 Cu 25 Co 25 alloy powder by high-energy ball milling technology, and then the Sm(Fe, TM) 12 alloy, Sm(Fe, TM) 7 alloy and Dy 20 Tb 30 Cu 25 Co 25 alloy powders are mixed in proportion and then spark plasma sintering and subsequent primary grain boundary diffusion heat treatment and secondary annealing heat treatment under a magnetic field are carried out to finally obtain a fully dense anisotropic composite magnet.
发明内容Summary of the invention
针对现有技术中存在的问题，本发明目的在于提供一种全致密各向异性复合磁体的制备方法。In view of the problems existing in the prior art, the present invention aims to provide a method for preparing a fully dense anisotropic composite magnet.
本发明的全致密各向异性复合磁体的制备方法，包括如下步骤：The method for preparing the fully dense anisotropic composite magnet of the present invention comprises the following steps:
（1）采用熔体快淬法分别制备名义成分为Sm(Fe,TM)12和Sm(Fe,TM)7的合金薄带，铜辊转速为10~30 m/s，其中TM为Ti、Zr、Si、Co中的一种或几种；(1) Alloy strips with nominal compositions of Sm(Fe,TM) 12 and Sm(Fe,TM) 7 were prepared by melt quenching method, the rotation speed of the copper roller was 10-30 m/s, where TM was one or more of Ti, Zr, Si and Co;
（2）采用高真空感应熔炼技术制备按原子百分比的低熔点Dy20Tb30Cu25Co25合金铸锭，并通过高能球磨技术将其破碎至平均粒度为3~9 μm的Dy20Tb30Cu25Co25合金粉末，球磨时间为1~6 h；(2) A low melting point Dy 20 Tb 30 Cu 25 Co 25 alloy ingot was prepared by high vacuum induction melting technology, and then crushed into Dy 20 Tb 30 Cu 25 Co 25 alloy powder with an average particle size of 3-9 μm by high energy ball milling technology. The ball milling time was 1-6 h.
（3）将步骤（1）获得的Sm(Fe,TM)12和Sm(Fe,TM)7合金薄带与步骤（2）获得的Dy20Tb30Cu25Co25合金粉末按一定质量比例混合后放入硬质合金模具中进行放电等离子烧结，获得全致密块状复合磁体；(3) mixing the Sm(Fe,TM) 12 and Sm(Fe,TM) 7 alloy strips obtained in step (1) with the Dy 20 Tb 30 Cu 25 Co 25 alloy powder obtained in step (2) in a certain mass ratio, placing the mixture in a cemented carbide mold for spark plasma sintering, and obtaining a fully dense block composite magnet;
（4）将步骤（3）获得的块状复合磁体进行磁场下的一级晶界扩散热处理和二级退火热处理，最终获得全致密各向异性复合磁体。(4) The bulk composite magnet obtained in step (3) is subjected to a primary grain boundary diffusion heat treatment and a secondary annealing heat treatment under a magnetic field to finally obtain a fully dense anisotropic composite magnet.
进一步的，步骤（3）中所述的Sm(Fe,TM)12合金薄带、Sm(Fe,TM)7合金薄带与Dy20Tb30Cu25Co25合金粉末的质量比为1：0.5~1：0.01~0.03；所述的放电等离子烧结具体工艺参数为：烧结温度为650~900 ℃，压力为400~600 MPa，烧结保温时间为10~30 min。 Furthermore, the mass ratio of the Sm(Fe, TM) 12 alloy strip, the Sm(Fe, TM) 7 alloy strip and the Dy 20 Tb 30 Cu 25 Co 25 alloy powder in step (3) is 1:0.5~1:0.01~0.03; the specific process parameters of the spark plasma sintering are: sintering temperature of 650~900 ℃, pressure of 400~600 MPa, and sintering holding time of 10~30 min.
进一步的，步骤（4）中所述的磁场下的一级晶界扩散热处理的温度为800~950℃，升温速率为1~5 ℃/min，保温时间为5~10 h，磁场强度为2~3 T，随后急冷至室温；所述的磁场下的二级退火热处理的温度为400~600 ℃，升温速率为1~5 ℃/min，保温时间为1~3h，磁场强度为0.5~1 T，随后急冷至室温。Furthermore, the temperature of the primary grain boundary diffusion heat treatment under the magnetic field in step (4) is 800~950℃, the heating rate is 1~5℃/min, the holding time is 5~10h, the magnetic field strength is 2~3T, and then it is rapidly cooled to room temperature; the temperature of the secondary annealing heat treatment under the magnetic field is 400~600℃, the heating rate is 1~5℃/min, the holding time is 1~3h, the magnetic field strength is 0.5~1T, and then it is rapidly cooled to room temperature.
与现有的技术相比，本发明具有如下优点和有益效果：本发明采用熔体快淬法分别制备Sm(Fe,TM)12和Sm(Fe,TM)7合金薄带，并通过高能球磨技术制备低熔点Dy20Tb30Cu25Co25合金粉末，随后将Sm(Fe,TM)12合金、Sm(Fe,TM)7合金及Dy20Tb30Cu25Co25合金粉末按比例混合后进行放电等离子烧结及后续磁场下的一级晶界扩散热处理和二级退火热处理，最终获得全致密各向异性复合磁体。本发明工艺过程简单，易操作，有利于高性能各向异性复合磁体在更多永磁器件中的应用，以满足市场需求。Compared with the existing technology, the present invention has the following advantages and beneficial effects: the present invention adopts melt quenching method to prepare Sm(Fe,TM) 12 and Sm(Fe,TM) 7 alloy strips respectively, and prepares low melting point Dy 20 Tb 30 Cu 25 Co 25 alloy powder by high energy ball milling technology, then mixes Sm(Fe,TM) 12 alloy, Sm(Fe,TM) 7 alloy and Dy 20 Tb 30 Cu 25 Co 25 alloy powder in proportion, and then performs spark plasma sintering and subsequent primary grain boundary diffusion heat treatment and secondary annealing heat treatment under magnetic field, finally obtaining a fully dense anisotropic composite magnet. The present invention has a simple process and is easy to operate, which is conducive to the application of high-performance anisotropic composite magnets in more permanent magnetic devices to meet market demand.
具体实施方式Detailed ways
下面将结合实施例对本发明做进一步的详细说明，但本发明并不仅仅局限于以下实施例。The present invention will be further described in detail below with reference to the embodiments, but the present invention is not limited to the following embodiments.
实施例1Example 1
（1）采用熔体快淬法分别制备名义成分为Sm(Fe0.8Ti0.2)12和Sm(Fe0.7Zr0.3)7的合金薄带，铜辊转速为10 m/s；(1) Alloy strips with nominal compositions of Sm(Fe 0.8 Ti 0.2 ) 12 and Sm(Fe 0.7 Zr 0.3 ) 7 were prepared by melt quenching method, with the copper roller rotating speed of 10 m/s.
（2）采用高真空感应熔炼技术制备按原子百分比的低熔点Dy20Tb30Cu25Co25合金铸锭，并通过高能球磨技术将其破碎至平均粒度为9 μm的Dy20Tb30Cu25Co25合金粉末，球磨时间为2 h；(2) A low-melting-point Dy 20 Tb 30 Cu 25 Co 25 alloy ingot was prepared by high vacuum induction melting technology, and then crushed into Dy 20 Tb 30 Cu 25 Co 25 alloy powder with an average particle size of 9 μm by high-energy ball milling technology for 2 h;
（3）将步骤（1）获得Sm(Fe0.8Ti0.2)12和Sm(Fe0.7Zr0.3)7合金薄带与步骤（2）获得的Dy20Tb30Cu25Co25合金粉末按质量比为1：0.5：0.01的比例混合后放入硬质合金模具中进行放电等离子烧结，烧结温度为650 ℃，压力为400 MPa，烧结保温时间为10 min，获得全致密块状复合磁体；(3) The Sm(Fe 0.8 Ti 0.2 ) 12 and Sm(Fe 0.7 Zr 0.3 ) 7 alloy strips obtained in step (1) and the Dy 20 Tb 30 Cu 25 Co 25 alloy powder obtained in step (2) were mixed in a mass ratio of 1:0.5:0.01 and placed in a cemented carbide mold for spark plasma sintering at a sintering temperature of 650 °C, a pressure of 400 MPa, and a sintering holding time of 10 min to obtain a fully dense block composite magnet;
（4）将步骤（3）获得的块状复合磁体进行磁场下的一级晶界扩散热处理和二级退火热处理，所述的磁场下的一级晶界扩散热处理的温度为800 ℃，升温速率为5 ℃/min，保温时间为10 h，磁场强度为2 T，随后急冷至室温；所述的磁场下的二级退火热处理的温度为600 ℃，升温速率为1 ℃/min，保温时间为1 h，磁场强度为1 T，随后急冷至室温，最终获得全致密各向异性复合磁体。(4) The block composite magnet obtained in step (3) is subjected to primary grain boundary diffusion heat treatment and secondary annealing heat treatment under a magnetic field, wherein the temperature of the primary grain boundary diffusion heat treatment under the magnetic field is 800°C, the heating rate is 5°C/min, the holding time is 10 h, the magnetic field strength is 2 T, and then it is rapidly cooled to room temperature; the temperature of the secondary annealing heat treatment under the magnetic field is 600°C, the heating rate is 1°C/min, the holding time is 1 h, the magnetic field strength is 1 T, and then it is rapidly cooled to room temperature, thereby finally obtaining a fully dense anisotropic composite magnet.
采用本发明制备的全致密各向异性复合磁体经磁性能测试，矫顽力为15.3 kOe，磁能积为21.5 MGOe。The fully dense anisotropic composite magnet prepared by the present invention is tested for magnetic properties, and the coercive force is 15.3 kOe and the magnetic energy product is 21.5 MGOe.
实施例2Example 2
（1）采用熔体快淬法分别制备名义成分为Sm(Fe0.9Zr0.1)12和Sm(Fe0.8Si0.2)7的合金薄带，铜辊转速为20 m/s；(1) Alloy strips with nominal compositions of Sm(Fe 0.9 Zr 0.1 ) 12 and Sm(Fe 0.8 Si 0.2 ) 7 were prepared by melt quenching method, and the copper roller speed was 20 m/s;
（2）采用高真空感应熔炼技术制备按原子百分比的低熔点Dy20Tb30Cu25Co25合金铸锭，并通过高能球磨技术将其破碎至平均粒度为6 μm的Dy20Tb30Cu25Co25合金粉末，球磨时间为4 h；(2) A low-melting-point Dy 20 Tb 30 Cu 25 Co 25 alloy ingot was prepared by high vacuum induction melting technology, and then crushed into Dy 20 Tb 30 Cu 25 Co 25 alloy powder with an average particle size of 6 μm by high-energy ball milling technology for 4 h;
（3）将步骤（1）获得的Sm(Fe0.9Zr0.1)12和Sm(Fe0.8Si0.2)7合金薄带与步骤（2）获得的Dy20Tb30Cu25Co25合金粉末按质量比为1：0.8：0.02的比例混合后放入硬质合金模具中进行放电等离子烧结，烧结温度为750 ℃，压力为500 MPa，烧结保温时间为20 min，获得全致密块状复合磁体；(3) The Sm(Fe 0.9 Zr 0.1 ) 12 and Sm(Fe 0.8 Si 0.2 ) 7 alloy strips obtained in step (1) and the Dy 20 Tb 30 Cu 25 Co 25 alloy powder obtained in step (2) are mixed in a mass ratio of 1:0.8:0.02 and placed in a cemented carbide mold for spark plasma sintering at a sintering temperature of 750 °C, a pressure of 500 MPa, and a sintering holding time of 20 min to obtain a fully dense block composite magnet;
（4）将步骤（3）获得的块状复合磁体进行磁场下的一级晶界扩散热处理和二级退火热处理，所述的磁场下的一级晶界扩散热处理的温度为870 ℃，升温速率为3 ℃/min，保温时间为8 h，磁场强度为2 T，随后急冷至室温；所述的磁场下的二级退火热处理的温度为500 ℃，升温速率为3 ℃/min，保温时间为2 h，磁场强度为0.5 T，随后急冷至室温，最终获得全致密各向异性复合磁体。(4) The block composite magnet obtained in step (3) is subjected to primary grain boundary diffusion heat treatment and secondary annealing heat treatment under a magnetic field, wherein the temperature of the primary grain boundary diffusion heat treatment under the magnetic field is 870°C, the heating rate is 3°C/min, the holding time is 8 h, the magnetic field strength is 2 T, and then it is rapidly cooled to room temperature; the temperature of the secondary annealing heat treatment under the magnetic field is 500°C, the heating rate is 3°C/min, the holding time is 2 h, the magnetic field strength is 0.5 T, and then it is rapidly cooled to room temperature, finally obtaining a fully dense anisotropic composite magnet.
采用本发明制备的全致密各向异性复合磁体经磁性能测试，矫顽力为17.1 kOe，磁能积为23.2 MGOe。The fully dense anisotropic composite magnet prepared by the present invention is tested for magnetic properties, and the coercive force is 17.1 kOe and the magnetic energy product is 23.2 MGOe.
实施例3Example 3
（1）采用熔体快淬法分别制备名义成分为Sm(Fe0.7Si0.3)12和Sm(Fe0.9Co0.1)7的合金薄带，铜辊转速为30 m/s；(1) Alloy strips with nominal compositions of Sm(Fe 0.7 Si 0.3 ) 12 and Sm(Fe 0.9 Co 0.1 ) 7 were prepared by melt quenching method, and the copper roller speed was 30 m/s;
（2）采用高真空感应熔炼技术制备按原子百分比的低熔点Dy20Tb30Cu25Co25合金铸锭，并通过高能球磨技术将其破碎至平均粒度为3 μm的Dy20Tb30Cu25Co25合金粉末，球磨时间为6 h；(2) A low-melting-point Dy 20 Tb 30 Cu 25 Co 25 alloy ingot was prepared by high vacuum induction melting technology, and then crushed into Dy 20 Tb 30 Cu 25 Co 25 alloy powder with an average particle size of 3 μm by high-energy ball milling technology for 6 h;
（3）将步骤（1）获得的Sm(Fe0.7Si0.3)12和Sm(Fe0.9Co0.1)7合金薄带与步骤（2）获得的Dy20Tb30Cu25Co25合金粉末按质量比为1：1：0.03的比例混合后放入硬质合金模具中进行放电等离子烧结，烧结温度为900 ℃，压力为600 MPa，烧结保温时间为30 min，获得全致密块状复合磁体；(3) The Sm(Fe 0.7 Si 0.3 ) 12 and Sm(Fe 0.9 Co 0.1 ) 7 alloy strips obtained in step (1) and the Dy 20 Tb 30 Cu 25 Co 25 alloy powder obtained in step (2) were mixed in a mass ratio of 1:1:0.03 and placed in a cemented carbide mold for spark plasma sintering at a sintering temperature of 900 °C, a pressure of 600 MPa, and a sintering holding time of 30 min to obtain a fully dense block composite magnet;
（4）将步骤（3）获得的块状复合磁体进行磁场下的一级晶界扩散热处理和二级退火热处理，所述的磁场下的一级晶界扩散热处理的温度为950 ℃，升温速率为1 ℃/min，保温时间为5 h，磁场强度为3 T，随后急冷至室温；所述的磁场下的二级退火热处理的温度为400 ℃，升温速率为5 ℃/min，保温时间为3 h，磁场强度为0.5 T，随后急冷至室温，最终获得全致密各向异性复合磁体。(4) subjecting the bulk composite magnet obtained in step (3) to primary grain boundary diffusion heat treatment and secondary annealing heat treatment under a magnetic field, wherein the temperature of the primary grain boundary diffusion heat treatment under the magnetic field is 950°C, the heating rate is 1°C/min, the holding time is 5 h, the magnetic field strength is 3 T, and then the magnet is rapidly cooled to room temperature; the temperature of the secondary annealing heat treatment under the magnetic field is 400°C, the heating rate is 5°C/min, the holding time is 3 h, the magnetic field strength is 0.5 T, and then the magnet is rapidly cooled to room temperature, thereby finally obtaining a fully dense anisotropic composite magnet.
采用本发明制备的全致密各向异性复合磁体经磁性能测试，矫顽力为18.5 kOe，磁能积为25.1 MGOe。The fully dense anisotropic composite magnet prepared by the present invention is tested for magnetic properties, and the coercive force is 18.5 kOe and the magnetic energy product is 25.1 MGOe.
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