CN111883327A - Low-heavy rare earth content high-coercivity permanent magnet and method for preparing composite gold - Google Patents
Low-heavy rare earth content high-coercivity permanent magnet and method for preparing composite gold Download PDFInfo
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 46
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 44
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 15
- 239000010931 gold Substances 0.000 title claims abstract description 15
- 239000000956 alloy Substances 0.000 claims abstract description 171
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 169
- 239000000843 powder Substances 0.000 claims abstract description 54
- 239000000463 material Substances 0.000 claims abstract description 33
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 239000002184 metal Substances 0.000 claims abstract description 15
- 150000001875 compounds Chemical class 0.000 claims abstract description 13
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 7
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 7
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 7
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims description 23
- 239000002994 raw material Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 16
- 229910052771 Terbium Inorganic materials 0.000 claims description 15
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 14
- 238000003723 Smelting Methods 0.000 claims description 14
- 239000010949 copper Substances 0.000 claims description 13
- 238000005266 casting Methods 0.000 claims description 12
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 229910052733 gallium Inorganic materials 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 150000002739 metals Chemical class 0.000 claims description 7
- 229910052758 niobium Inorganic materials 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- 229910052720 vanadium Inorganic materials 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910001021 Ferroalloy Inorganic materials 0.000 claims description 3
- 238000005275 alloying Methods 0.000 claims description 2
- 150000002222 fluorine compounds Chemical class 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 7
- 229910001172 neodymium magnet Inorganic materials 0.000 description 27
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 16
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 10
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- 238000010298 pulverizing process Methods 0.000 description 4
- 229910000640 Fe alloy Inorganic materials 0.000 description 3
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
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- 230000008018 melting Effects 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 3
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- 229910000592 Ferroniobium Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- MOSURRVHVKOQHA-UHFFFAOYSA-N [Tb].[Dy] Chemical compound [Tb].[Dy] MOSURRVHVKOQHA-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- LFHISGNCFUNFFM-UHFFFAOYSA-N chloropicrin Chemical compound [O-][N+](=O)C(Cl)(Cl)Cl LFHISGNCFUNFFM-UHFFFAOYSA-N 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
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- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- ZFGFKQDDQUAJQP-UHFFFAOYSA-N iron niobium Chemical compound [Fe].[Fe].[Nb] ZFGFKQDDQUAJQP-UHFFFAOYSA-N 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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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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- Chemical & Material Sciences (AREA)
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- Metallurgy (AREA)
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- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a low heavy rare earth content high coercivity permanent magnet, which comprises: a main alloy, an auxiliary alloy; taking a heavy-rare earth-free alloy as a main alloy, wherein the main alloy comprises (RE) xFe (100-x-Y-z) My Bz, and RE is one or more of Pr, Nd, Pr, La, Ce and Y; m is a non-rare earth metal element except Fe, x, y and z are mass percentages, wherein x is more than or equal to 27.0 and less than or equal to 36.0, y is more than or equal to 0 and less than or equal to 5.0, and z is more than or equal to 0.8 and less than or equal to 1.5; the auxiliary alloy is one or more of metal powder, oxide, fluoride and compound of heavy rare earth elements. The invention also discloses a method for preparing the composite gold by using the permanent magnet with low content of heavy rare earth and high coercivity. The invention adopts a complex alloy method to distribute heavy rare earth elements around the main phase crystal grains and prevent the heavy rare earth elements from entering the interior of the crystal grains in large quantity, thereby obviously reducing the use amount of the heavy rare earth and reducing the material cost.
Description
Technical Field
The invention belongs to a preparation method of a permanent magnet material, and particularly relates to a permanent magnet with low content of heavy rare earth and high coercivity and a preparation method of composite gold.
Background
The Nd-Fe-B rare earth permanent magnetic material is widely applied to the fields of electric drive, electronics, rail transit, green new energy, energy-saving household appliances and the like because of high cost performance, and is one of essential basic materials for modern technological development and social progress. The theoretical magnetic energy product of the neodymium iron boron magnet is 509kJ/m3(64MGOe), the laboratory maximum level has reached 474kJ/m3(59.6 MGOe). At present, the maximum magnetic energy product of the magnets produced by enterprises in batches is achievedTo above 52 MGOe. However, the coercive force of the magnet can only reach about 1/4 to l/3 of a theoretical value, the temperature stability is poor, the working temperature is low, and the application of the magnet in the high-temperature field is greatly limited.
In recent years, with the rapid development of new energy vehicles, industrial robots, rail transit and other industries, how to increase the working temperature of sintered neodymium-iron-boron magnets becomes a major problem in the field of industrial research. The effective method for improving the working temperature of the neodymium iron boron magnet is to improve the coercive force. Comparison of RE of different rare earth elements2Fel4Intrinsic Property of B Compound, Dy2Fe14B and Tb2Fe14The magnetocrystalline anisotropy field of B is 11940kA/m and 17572kA/m respectively, which are much higher than Nd2Fe14The magnetocrystalline anisotropy field of the main phase can be greatly improved after Dy and Tb are added to replace Nd, so that the coercive force is effectively improved. The addition of Tb and Dy in the magnet for the hybrid electric vehicle, which is produced by the conventional direct smelting addition process, reaches more than 4 percent. However, Dy and Tb added by direct smelting easily enter main phase grains, so that saturation magnetization is reduced, and residual magnetism and magnetic energy product are reduced due to magnetic dilution. How to keep the remanence and the magnetic energy product from being reduced while improving the coercivity is a challenge for ndfeb materials. In general, the sum of intrinsic coercivity and maximum magnetic energy product is used as a measure of the overall magnetic performance of the ultra-high performance magnet in gauss units.
In addition, the price of heavy rare earth elements Dy and Tb is high, and the smelting addition can increase the cost of the magnet, so that the cost of the high-grade neodymium-iron-boron permanent magnet material is obviously increased. How to increase the coercive force without or with less heavy rare earth Dy and Tb is another challenge to the Nd-Fe-B material. Therefore, the development of ultra-high comprehensive performance magnets and low-heavy rare earth high-coercivity magnets becomes a research hotspot at home and abroad at present. Therefore, since 2007 in japan, the low-heavy rare earth sintered nd-fe-b permanent magnet material has been implemented as a national strategic project, and three sintered nd-fe-b enterprises of metals (nemax), transceive chemical industry and TDK have all focused research and development efforts on reducing the use of heavy rare earth as much as possible in order to further reduce the cost and improve the product competitiveness. China pays great attention to the development and application of sintered Nd-Fe-B permanent magnetic materials, so that the Nd-Fe-B industry in China gains a leap development.
In order to obtain a magnet with high magnetic energy product, Otsuki. E et al adopted a double alloy method made of other powder metallurgy materials in the preparation process of sintered NdFeB magnet in 1990, namely, the component is very close to Nd2Fe14The main alloy powder of the component B and the auxiliary alloy powder rich in rare earth are mixed according to a certain proportion, and then the mixture is subjected to magnetic field forming and sintering to prepare the magnet with the required components. In 1995, M.Velicescu et al added a certain proportion of low melting point Dy in 28 wt% Nd-1 wt.% B-residual Fe alloy powder in order to improve the coercive force of a high magnetic energy product Nd-Fe-B magnet3Co、Nd3Co and Dyl.5Nd1.5Co2The powders were alloyed to obtain an NdFeB magnet having Br of 1.4T and jHc of 13.5 kOe. Microscopic structure analysis shows that only a small amount of Dy enters the surface layer of the main phase grains, but grain growth easily occurs. In 1999, T.S.ZHao et al in Nd14.7Dy0.3FebalAl0.3B6FeGa with low melting point (824 ℃) is added into master alloy3The research result of the alloy shows that 0.1-0.2 wt.% FeCa is added3The coercivity can be significantly increased without reducing remanence. EPMA analysis of Nd occurrence inside sintered magnet6Fe14-xGax (x ≈ 1) phase, it is considered that the intrinsic coercivity increase may be related to this term.
In 2000, in order to improve the defect of low intrinsic coercivity of a high-performance neodymium iron boron permanent magnet material, the research of NdDyTbCo low-melting-point intercrystalline diffusion alloy is added into an Nd30 wt-b 1.0 wt-residual Fe alloy by the institute of baotou rare earth research institute, liu symbol and the like, so that the intrinsic coercivity is improved on the premise that the remanence is hardly reduced, and a high-performance magnet with higher coercivity is obtained. However, the microstructure formed by diffusion of the low-melting-point intercrystalline alloy and its influence on the properties of the magnet were not studied in more detail.
In 2002, A.M.Gabaz performed the addition of Nd, an auxiliary alloy, using Nd-Fe-B as a master alloy23Fe66Co4.35B5.65Ga1When 0.18 at.% Ga was contained in the magnet, the remanence hardly decreased, and the coercive force was remarkably improved.
In 2005, the shin-Etsu chemical industry (Ltd.) contained R to reduce Dy content2(Fe(Co) Si)14In the alloy of the B compound, an R-Fe (Co) -Si grain boundary phase is added, rare earth elements such as Dy are concentrated at the grain boundary of the magnet by adopting a grain boundary diffusion double-alloy method, the intrinsic coercive force is improved by 30 percent under the condition of keeping the remanence basically unchanged, and the heat resistance of the magnet is improved.
From the different researches, the intrinsic coercive force of the magnet can be improved by elemental diffusion of different grain boundary phase alloys in the sintered Nd-Fe-B rare earth permanent magnet material, and the magnetic energy product is hardly reduced. Therefore, the preparation of the sintered Nd-Fe-B rare earth permanent magnet material by the intercrystalline element diffusion double alloy method is likely to be an important preparation method of future permanent magnet materials, and particularly under the condition that resources of heavy rare earth elements Dy and Tb are in short supply, the preparation method is further emphasized.
At present, the coercive force of a thin magnet can be effectively improved by utilizing the intergranular diffusion technology of surface dysprosium and terbium diffusion without reducing residual magnetism, but the technology is only limited to a small magnet with the thickness of less than 6mm, and a large-size magnet cannot be prepared.
Disclosure of Invention
The invention aims to provide a permanent magnet with low heavy rare earth content and high coercivity and a preparation method of the complex alloy.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a low heavy rare earth content high coercivity permanent magnet comprising: a main alloy, an auxiliary alloy; taking a heavy-rare-earth-free alloy as a main alloy, wherein the main alloy component is (RE) xFe (100-x-Y-z) MyBz, and RE is one or more of Pr, Nd, Pr, La, Ce and Y; m is a non-rare earth metal element except Fe, x, y and z are mass percentages, wherein x is more than or equal to 27.0 and less than or equal to 36.0, y is more than or equal to 0 and less than or equal to 5.0, and z is more than or equal to 0.8 and less than or equal to 1.5; the auxiliary alloy is one or more of metal powder, oxide, fluoride and compound of heavy rare earth elements.
Further, non-rare earth metal elements are selected from: al, Ga, Cu and Co, Nb, Zr, Ti, W or V.
Furthermore, in the auxiliary alloy, Dy or Tb is selected as the heavy rare earth element.
Further, B is between 0.8 and 1.5 wt%.
Further, the Al content is less than 2 wt%, the Ga content is 0.1-1 wt%, the Co content is 0.2-3 wt%, the Cu content is 0.1-0.5 wt%, the Nb content is 0.05-0.8 wt%, and the Zr content is 0.05-0.3 wt%.
The method for preparing the composite gold by the permanent magnet with low content of heavy rare earth and high coercivity comprises the following steps:
respectively preparing a main alloy raw material and auxiliary alloy powder, smelting the main alloy raw material and casting to generate a main alloy, and crushing the main alloy into main alloy powder;
mixing the main alloy powder and the auxiliary alloy powder in a powder making process or a magnetic field forming process, and preparing the permanent magnet through magnetic field forming, sintering and heat treatment.
Preferably, the heavy-rare earth-free alloy is taken as a main alloy, and the main alloy component is (RE) xFe (100-x-y-z) MyBz; the main alloy comprises the following raw materials: single metals or alloys of rare earth elements Pr, Nd, Pr, La, Ce, Y, single metals, alloys or ferroalloys of non-rare earth elements, and ferroboron alloys; non-rare earth metal elements are selected from: al, Ga, Cu, Co, Nb, Zr, Ti, W or V.
Preferably, the auxiliary alloy raw material is one or more of metal powder, oxide, fluoride and compound of heavy rare earth elements.
Preferably, the prepared main alloy raw materials are smelted by a vacuum rapid hardening furnace to generate the main alloy, the casting temperature of the main alloy is 1400-1460 ℃, and the rotating speed of a copper roller is 2-8 m/s.
Preferably, the main alloy and the auxiliary alloy raw materials are respectively prepared into powder, the average particle size of the main alloy is 2-8 mu m, and the particle size of the auxiliary alloy powder is less than 2-8 mu m; mixing and forming the main alloy powder and the auxiliary alloy powder to form a pressed compact, and sintering the pressed compact in a vacuum sintering furnace at 980-1120 ℃; and carrying out heat treatment on the sintered blank at 850-950 ℃, and carrying out secondary heat treatment on the sintered blank at 400-650 ℃.
The invention has the technical effects that:
the invention can solve the defects of the intergranular diffusion technology and has advantages in the preparation of low-heavy rare earth high-content permanent magnet (such as neodymium iron boron magnet) products. The invention adopts a composite gold method, takes (RE) xFe (100-x-y-z) MyBz as a main alloy, and takes one or more of metal powder, oxide, fluoride and intermetallic compound containing heavy rare earth elements as an auxiliary alloy. The main and auxiliary alloys are mixed in a certain proportion in the process of milling or magnetic field forming, and the magnet with low content of heavy rare earth and high coercivity can be prepared.
1. By adopting the complex alloy method, the heavy rare earth elements with high price can be distributed around the main phase crystal grains, and a large amount of the heavy rare earth elements can be prevented from entering the interior of the crystal grains, so that the using amount of the heavy rare earth can be obviously reduced, and the material cost can be reduced.
2. The grain boundary is the weak point of the magnet material, and due to the existence of a transition layer, a sharp corner, a defect and the like, a nucleation domain of reverse magnetization is easy to form at the grain boundary, so that the coercive force of the magnet is reduced. The permanent magnet (neodymium iron boron) prepared by the complex alloy method can effectively distribute heavy rare earth elements around the grain boundary and play a large role in strengthening the main phase grain boundary, thereby obviously improving the coercive force of the magnet.
3. Because the heavy rare earth element can reduce the residual magnetism of the magnet, the content of the heavy rare earth in the magnet can be effectively reduced by a complex alloy method, thereby improving the residual magnetism of the magnet and improving the magnetic performance.
4. The effective method for improving the remanence and the maximum energy product of the magnet (neodymium iron boron) material and reducing the content of heavy rare earth in the permanent magnet material without reducing the coercive force is surface dysprosium terbium penetration, but the method has the defect that the method can only be applied to the magnet with the thickness not more than 6mm and cannot be used for manufacturing a large magnet. The composite gold method can break through the limitation while ensuring the advantages of the method, and prepare the large-size ultrahigh-performance magnet.
Detailed Description
The following description sufficiently illustrates specific embodiments of the invention to enable those skilled in the art to practice and reproduce it.
A low heavy rare earth content high coercivity permanent magnet comprising: a main alloy, an auxiliary alloy; taking a heavy-rare-earth-free alloy as a main alloy, wherein the main alloy component is (RE) xFe (100-x-y-z) MyBz; RE is one or more of Pr, Nd, Pr, La, Ce and Y; m is a non-rare earth metal element except Fe, x, y and z are mass percentages, wherein x is more than or equal to 27.0 and less than or equal to 36.0, y is more than or equal to 0 and less than or equal to 5.0, and z is more than or equal to 0.8 and less than or equal to 1.5; the auxiliary alloy is one or more of metal powder, oxide, fluoride and compound of heavy rare earth elements.
The main alloy should form sufficient RE as much as possible2Fe14B main phase to ensure the material to obtain saturation magnetization as high as possible; on the other hand, a certain amount of rare earth-rich with low melting point must be formed to ensure the smoothness of a diffusion channel. The total amount of the rare earth of the main alloy can be selected within the range of x being more than or equal to 27.0 and less than or equal to 36.0 according to the process characteristics and the difference of rare earth elements.
Non-rare earth metal elements are selected from: al, Ga, Cu and Co, Nb, Zr, in addition to the above non-rare earth elements, the present invention includes addition of Ti, W, V, etc.
In the auxiliary alloy, the heavy rare earth elements are typically Dy and Tb. Dy and Tb can improve magnetocrystalline anisotropy of the material, so that the coercive force Hcj of the material can be greatly improved, wherein the coupling between heavy rare earth elements Tb and Fe belongs to antiparallel coupling, and therefore the temperature coefficient of the material can be reduced, and the thermal stability of the magnetic material is improved. However, excessive addition of Dy and Tb not only increases the production cost, but also adversely affects the magnetic properties of the neodymium-iron-boron material, so their addition amounts are as low as possible.
B is formation of Re2Fe14B is indispensable element, the content of the indispensable element is 0.8-1.5 wt%, and too little B can not form enough tetragonal phase, namely RE2Fe14B, due toThis cannot obtain a high-performance magnet. However, excessive addition of B will form more B phase, resulting in deterioration of the magnetic properties of the material.
The coercive force of the material can be obviously improved by adding a small amount of Al and Ga, wherein the addition amount of Al cannot be more than 2 wt%, and the addition amount of Ga is 0.1-1 wt%.
The heat resistance of the material can be improved by the composite addition of Cu and Co; co can improve the Curie temperature of the material, but excessive Co can cause the crystal grains of the material to grow excessively, so that the magnetic property of the material is deteriorated, and the production cost is increased, so that the reasonable addition amount is 0.2-3 wt%; the amount of Cu added is 0.1 to 0.5 wt%.
Nb can effectively inhibit the growth of crystal grains, so that the coercive force of the material can be obviously improved, and the addition amount is 0.05-0.8 wt%.
Zr also has the characteristics of inhibiting the growth of crystal grains and improving the mechanical property of the magnet, and the addition amount of the Zr is 0.05 to 0.3 weight percent.
The method for preparing the composite gold by the permanent magnet with low content of heavy rare earth and high coercive force comprises the steps of proportioning, smelting, milling, molding, sintering and heat treatment;
step 1: respectively preparing a main alloy raw material and an auxiliary alloy raw material;
taking a heavy-rare earth-free alloy as a main alloy, wherein the main alloy component is (RE) xFe (100-x-y-z) MyBz; the main alloy raw materials adopt single metals or alloys of rare earth elements Pr, Nd, Pr, La, Ce and Y, single metals, alloys or iron alloys of non-rare earth elements and ferroboron.
Non-rare earth metal elements are selected from: al, Ga, Cu, Co, Nb, Zr, Ti, W or V. The ferroalloy can adopt ferroniobium and ferroboron.
The auxiliary alloy raw material is one or more of metal powder, oxide, fluoride and compound of heavy rare earth elements.
Before batching, the raw materials must be pretreated by polishing oxide scales, crushing particles and the like.
Step 2: smelting and casting the main alloy raw material to generate a main alloy;
smelting the prepared main alloy raw materials by using a vacuum rapid hardening furnace to generate main alloy, wherein the casting temperature of the main alloy is 1400-1460 ℃, and the rotating speed of a copper roller is 2-8 m/s.
And step 3: mixing the main alloy powder and the auxiliary alloy powder in a powder making process or a magnetic field forming process, and preparing the permanent magnet through magnetic field forming, sintering and heat treatment.
Step 31: respectively pulverizing the main alloy and the auxiliary alloy raw materials;
grinding the smelted main alloy into main alloy powder with the average particle size of 2-8 mu m by powder preparation means such as hydrogen crushing, inert gas jet milling and the like; independently preparing the auxiliary alloy raw material into finer powder (the granularity is less than 2-8 mu m); or mixing the coarsely crushed main alloy powder and the auxiliary alloy according to a certain proportion, and grinding into mixed powder with the average particle size of 2-8 mu m by means of jet milling and the like under the protection of inert gas.
Step 32: mixing and forming the main alloy powder and the auxiliary alloy powder to form a pressed blank;
the molding method is divided into three cases:
1. pressing and molding the uniformly mixed and finely ground main alloy powder and auxiliary alloy powder through corresponding grinding tools under an oriented magnetic field;
2. uniformly mixing the separately prepared main alloy and auxiliary alloy powder according to a certain proportion, and then pressing and molding the mixture by a corresponding grinding tool in an oriented magnetic field;
3. the independently prepared main alloy powder and auxiliary alloy powder are respectively stored in containers with independent spaces, the main alloy powder and the auxiliary alloy powder are controlled by a controller to be distributed in a layered and crossed manner during filling, the independent distribution height of the main alloy and the auxiliary alloy can be adjusted according to alloy components and performance requirements, and the main alloy and the auxiliary alloy are pressed and molded under the action of an oriented magnetic field after filling.
Step 33: sintering the pressed compact in a vacuum sintering furnace at 980-1120 ℃;
step 34: and carrying out heat treatment on the sintered blank at 850-950 ℃, and carrying out secondary heat treatment on the sintered blank at 400-650 ℃.
Example 1
The method for preparing the composite gold by the low-heavy rare earth content high-coercivity neodymium iron boron permanent magnet comprises the following steps:
table 1 main alloy composition in example 1:
| element(s) | RE | Fe | M | B |
| Wt％ | 30.2 | 65.79 | 3 | 1.01 |
Compounding alloy: dysprosium-containing compounds
Then, the neodymium iron boron permanent magnet material is manufactured by the following steps:
(1) smelting and casting, namely smelting the prepared main alloy in a vacuum induction rapid hardening furnace uniformly, and throwing the main alloy into a casting sheet with the thickness of 0.2-0.45 mm;
(2) and pulverizing, namely, mixing the smelted main and auxiliary alloys according to the weight ratio of 98: 2, and grinding the mixture into powder with the granularity of 3-5 mu m by using an air flow mill;
(3) molding, namely pressing the prepared powder into a blank by mould pressing under an oriented magnetic field, and then further compacting by isostatic pressing;
(4) sintering, namely sintering the pressed compact in a vacuum sintering furnace at 1050 ℃ for 2 hours.
(5) And heat treatment, namely, preserving the heat of the sintered blank for 1 hour at 880 ℃ in a vacuum sintering furnace, and then performing secondary heat treatment for 1.5 hours at 600 ℃ to prepare a blank.
Comparative example 1: the sintered neodymium-iron-boron magnet is prepared by calculating the main and auxiliary alloy components in the embodiment 1, converting the main and auxiliary alloy components and adopting a single-alloy method under the condition that other processes are the same.
Table 2 magnetic properties of example 1 and comparative example 1:
| BHm(kJ/m3) | Br(T) | Hcj(kA/m) | |
| example 1 | 361.5 | 1.38 | 1993 |
| Comparative example 1 | 349.6 | 1.35 | 1412 |
As can be seen by comparison in Table 2, the magnet produced by the single alloy method has significantly lower overall magnetic properties than the composite gold method.
Example 2
Table 3 main alloy composition in example 2:
| element(s) | RE | Fe | M | B |
| Wt％ | 29.8 | 66.19 | 3 | 1.01 |
Auxiliary alloying: dysprosium-containing compounds
Then, the neodymium iron boron permanent magnet material is manufactured by the following steps:
(1) smelting and casting, namely smelting the prepared main alloy in a vacuum induction rapid hardening furnace uniformly, and throwing the main alloy into a casting sheet with the thickness of 0.2-0.45 mm;
(2) and pulverizing, namely, mixing the smelted main and auxiliary alloys according to the weight ratio of 98: 2, and grinding the mixture into powder with the granularity of 3-5 mu m by using an air flow mill;
(3) molding, namely pressing the prepared powder into a blank by mould pressing under an oriented magnetic field, and then further compacting by isostatic pressing;
(4) sintering, namely sintering the pressed compact in a vacuum sintering furnace at 1055 ℃ for 2 hours;
(5) and heat treatment, namely, preserving the heat of the sintered blank for 1 hour at 900 ℃ in a vacuum sintering furnace, and then performing secondary heat treatment for 1.5 hours at 550 ℃ to prepare a blank.
Comparative example 2: the sintered neodymium-iron-boron magnet is prepared by calculating the main and auxiliary alloy components in the embodiment 2, converting the main and auxiliary alloy components and adopting a single-alloy method under the condition that other processes are the same.
Table 4 magnetic properties of example 2 and comparative example 2:
| BHm(kJ/m3) | Br(T) | Hcj(kA/m) | |
| example 2 | 375.1 | 1.40 | 1913 |
| Comparative example 2 | 355.2 | 1.36 | 1398 |
As can be seen from Table 4, the overall magnetic properties of the magnet made by the single alloy method are significantly lower than those of the multiple alloy method.
Example 3
Table 5 main alloy composition in example 3:
| element(s) | RE | Fe | M | B |
| Wt％ | 29.2 | 66.99 | 2.8 | 1.01 |
Compounding alloy: powder of terbium-containing compound
Then, the neodymium iron boron permanent magnet material is manufactured by the following steps:
(1) smelting and casting, namely smelting the prepared main alloy in a vacuum induction rapid hardening furnace uniformly, and throwing the main alloy into a casting sheet with the thickness of 0.2-0.45 mm;
(2) pulverizing, namely crushing the smelted main alloy by hydrogen, and grinding the crushed main alloy into powder with the particle size of 3-5 microns by airflow milling;
(3) respectively storing the prepared main alloy powder and terbium-containing compound powder by adopting containers with independent spaces, controlling the main alloy and the auxiliary alloy to be distributed in a layered and crossed manner by a controller during filling, wherein the overall material ratio of the main alloy to the auxiliary alloy is 98: 2, pressing and forming under the action of an oriented magnetic field after filling;
(4) sintering, namely sintering the pressed compact in a vacuum sintering furnace at 1065 ℃ for 2 hours;
(5) and heat treatment, namely, preserving the heat of the sintered blank for 1 hour at 890 ℃ in a vacuum sintering furnace, and then carrying out secondary heat treatment for 1.5 hours at 520 ℃ to prepare a blank.
Table 6 magnetic properties of example 3 and comparative example 3:
comparative example 3: the sintered neodymium-iron-boron magnet is prepared by calculating the main and auxiliary alloy components in the embodiment 3, converting the main and auxiliary alloy components and adopting a single-alloy method under the condition that other processes are the same.
As can be seen from Table 6, the comprehensive magnetic performance of the magnet prepared by the single alloy method is obviously lower than that of the magnet prepared by the complex alloy method, and the sintered Nd-Fe-B magnet with excellent large-size comprehensive performance can be prepared.
The terminology used herein is for the purpose of description and illustration, rather than of limitation. As the present invention may be embodied in several forms without departing from the spirit or essential characteristics thereof, it should also be understood that the above-described embodiments are not limited by any of the details of the foregoing description, but rather should be construed broadly within its spirit and scope as defined in the appended claims, and therefore all changes and modifications that fall within the meets and bounds of the claims, or equivalences of such meets and bounds are therefore intended to be embraced by the appended claims.
Claims (10)
1. A low heavy rare earth content high coercivity permanent magnet comprising: a main alloy, an auxiliary alloy; taking a heavy-rare earth-free alloy as a main alloy, wherein the main alloy comprises (RE) xFe (100-x-Y-z) MyBz, and RE is one or more of Pr, Nd, Pr, La, Ce and Y; m is a non-rare earth metal element except Fe, x, y and z are mass percentages, wherein x is more than or equal to 27.0 and less than or equal to 36.0, y is more than or equal to 0 and less than or equal to 5.0, and z is more than or equal to 0.8 and less than or equal to 1.5; the auxiliary alloy is one or more of metal powder, oxide, fluoride and compound of heavy rare earth elements.
2. The low heavy rare earth content high coercivity permanent magnet of claim 1 wherein the non-rare earth elements are selected from the group consisting of: al, Ga, Cu and Co, Nb, Zr, Ti, W or V.
3. The low heavy rare earth content high coercivity permanent magnet according to claim 1 wherein Dy or Tb is selected as the heavy rare earth element in the auxiliary alloy.
4. The low heavy rare earth content high coercivity permanent magnet of claim 1 wherein B is between 0.8 and 1.5 wt%.
5. The low-rare-earth-content high-coercivity permanent magnet according to claim 2, wherein the Al content is less than 2 wt%, the Ga content is between 0.1 and 1 wt%, the Co content is between 0.2 and 3 wt%, the Cu content is between 0.1 and 0.5 wt%, the Nb content is between 0.05 and 0.8 wt%, and the Zr content is between 0.05 and 0.3 wt%.
6. The method for preparing the composite gold by the permanent magnet with low content of heavy rare earth and high coercivity comprises the following steps:
respectively preparing a main alloy raw material and auxiliary alloy powder, smelting the main alloy raw material and casting to generate a main alloy, and crushing the main alloy into main alloy powder;
mixing the main alloy powder and the auxiliary alloy powder in a powder making process or a magnetic field forming process, and preparing the permanent magnet through magnetic field forming, sintering and heat treatment.
7. The method for preparing the composite gold by using the low heavy rare earth content high coercivity permanent magnet according to claim 6, wherein a heavy rare earth-free alloy is used as a main alloy, and the main alloy component is (RE) xFe (100-x-y-z) My Bz; the main alloy comprises the following raw materials: single metals or alloys of rare earth elements Pr, Nd, Pr, La, Ce, Y, single metals, alloys or ferroalloys of non-rare earth elements, and ferroboron alloys; non-rare earth metal elements are selected from: al, Ga, Cu, Co, Nb, Zr, Ti, W or V.
8. A method of making a composite gold by making a low heavy rare earth high coercivity permanent magnet as claimed in claim 6 wherein the auxiliary alloying material is selected from one or more of metal powders, oxides, fluorides and compounds of heavy rare earth elements.
9. The method for preparing the composite gold by the low-heavy rare earth-content high-coercivity permanent magnet according to claim 6, wherein the prepared main alloy raw material is smelted by a vacuum rapid hardening furnace to generate the main alloy, the casting temperature of the main alloy is 1400-1460 ℃, and the rotation speed of a copper roller is 2-8 m/s.
10. The method for preparing the composite gold by using the permanent magnet with low heavy rare earth content and high coercivity as claimed in claim 6, wherein the main alloy and the auxiliary alloy raw materials are respectively prepared into powder, the average particle size of the main alloy is 2-8 μm, and the particle size of the auxiliary alloy powder is less than 2-8 μm; mixing and forming the main alloy powder and the auxiliary alloy powder to form a pressed compact, and sintering the pressed compact in a vacuum sintering furnace at 980-1120 ℃; and carrying out heat treatment on the sintered blank at 850-950 ℃, and carrying out secondary heat treatment on the sintered blank at 400-650 ℃.
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