CN103632835B - A kind of quick forming method of high-performance neodymium-iron-boron magnet - Google Patents
A kind of quick forming method of high-performance neodymium-iron-boron magnet Download PDFInfo
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- CN103632835B CN103632835B CN201310638198.1A CN201310638198A CN103632835B CN 103632835 B CN103632835 B CN 103632835B CN 201310638198 A CN201310638198 A CN 201310638198A CN 103632835 B CN103632835 B CN 103632835B
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 44
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims abstract description 47
- 230000008021 deposition Effects 0.000 claims abstract description 25
- 229910000521 B alloy Inorganic materials 0.000 claims abstract description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000005496 tempering Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000005728 strengthening Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 230000001681 protective effect Effects 0.000 claims abstract description 4
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 2
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 2
- 229910052771 Terbium Inorganic materials 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 229910052735 hafnium Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 10
- 239000013078 crystal Substances 0.000 abstract description 9
- 229910052779 Neodymium Inorganic materials 0.000 abstract description 8
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 239000000696 magnetic material Substances 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 230000005389 magnetism Effects 0.000 description 8
- 229910000859 α-Fe Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005266 casting Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000007712 rapid solidification Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
Abstract
The invention discloses a kind of quick forming method of high-performance neodymium-iron-boron magnet, relate to permanent magnetic material technology of preparing.The steps include: 1) weigh each element raw material according to magnet composition, mixed; 2) Nd Fe B alloys strip is obtained by rapid hardening belt-rejecting technology; 3) Nd Fe B alloys strip is successively carried out magnetic field assistant laser melt deposition under protective atmosphere or vacuum, obtained neodymium iron boron magnetic body; 4) neodymium iron boron magnetic body is carried out thermal deformation, strengthening magnetic texture; 5) thermal deformation neodymium iron boron magnetic body is carried out vacuum and low temperature tempering, improve grain boundary structure, improve magnet performance.The present invention is applicable to the preparation of large volume neodymium iron boron magnetic body, and obtained neodymium iron boron magnetic body crystal grain is tiny, and rich neodymium Entropy density deviation is even, and density is high, and oxygen content is low, is conducive to the raising of magnet performance.Present invention process is simple, and flow process is short, is easy to operation, is suitable for large-scale batch production.
Description
Technical field
The present invention relates to technical field of permanent magnetic material preparation, refer in particular to a kind of quick forming method of high-performance neodymium-iron-boron magnet.
Background technology
Neodymium iron boron magnetic body is the rare earth permanent-magnetic material of new generation with advantages such as excellent comprehensive magnetic energy, high performance-price ratio and easy processing, now be widely used in various new high-tech industry field, be especially suitable for being applied in requirement miniaturization, lightweight, integrated various regeneration products.
The magnetic property of neodymium iron boron magnetic body is mainly derived from Nd
2fe
14the intrinsic magnetic parameter of B Hard Magnetic phase, as anisotropy field, saturation magnetization etc., simultaneously closely related with the microstructure of magnet, as crystal particle scale, grain boundary structure etc.Powder metallurgical technique is one of important method preparing high-performance neodymium-iron-boron magnet, and the maximum magnetic energy product of the Sintered NdFeB magnet obtained by this technique is at present close to 93% of theoretical value, but its actual coercive force is only the 1/3-1/30 of theoretical value.In addition, powder metallurgical technique process is complicated, easily introduces more oxygen content, and not easily realizes effective refinement of crystal grain.This not only bad for the raising of neodymium iron boron magnetic body combination property, and wastes energy, and adds production cost.
Based on this, preparation technology simply casts-and thermal deformation technique causes and pays close attention to widely, and it also becomes one of important method manufacturing neodymium iron boron magnetic body.But the neodymium iron boron cast ingot that casting technique obtains exists to be organized thick, lack of homogeneity, easily form the equal problem of α-Fe soft magnetism, seriously constrain the raising of magnet magnetic property.Neodymium iron boron cast ingot tissue has material impact for the high performance heat distortion magnet of preparation.Therefore, in order to improve the magnetic property of neodymium iron boron magnetic body, its microstructure must be optimized, especially ingot structure.Desirable neodymium iron boron cast ingot is organized normally: Nd
2fe
14b Hard Magnetic phase crystal grain is tiny; Separate out mutually without α-Fe soft magnetism and crystal boundary rich neodymium Entropy density deviation even as far as possible.For this reason, need to develop a kind of new neodymium-iron-boron preparation process, under guarantee has the prerequisite of excellent institutional framework, simplify preparation technology, boost productivity, reduce production cost.
For the problems referred to above, the combination process that the present invention proposes to adopt rapid hardening belt-rejecting technology, magnetic field assistant laser melt deposition technology combines with thermal deformation technique prepares the method for high-performance neodymium-iron-boron magnet fast in the mode of successively laying and successively orientation melt deposition.Rapid hardening belt-rejecting technology effectively can suppress the precipitation of α-Fe soft magnetism phase, refinement principal phase Nd
2fe
14the institutional framework of B, makes rich neodymium be uniformly distributed in principal phase interface mutually; It provide not only magnetic field assistant laser melt deposition band used, and for subsequent technique carry out tissue prepare.Magnetic field assistant laser melt deposition technology is the magnetic aligning quick solidification forming technique that a kind of flexibility is high, the feature of its rapid solidification makes the neodymium iron boron magnetic body main phase grain that obtains tiny, separate out mutually without α-Fe soft magnetism, and maintaining the mutually equally distributed feature of rich neodymium in rapid casting, it is applicable to the neodymium iron boron magnetic body preparing all size and shape; In addition, magnetic field orientating can be induced and be produced certain magnetic texture, and this all contributes to the raising of final magnet performance.Thermal deformation technique further enhances magnet texture on the basis of magnetic field orientating, improves magnet density.The combination of above-mentioned three kinds of techniques can not only obtain the magnet institutional framework of optimization, and simplifies preparation technology, reduces production cost.
Summary of the invention
The object of the invention is for solving prior art Problems existing, a kind of quick forming method of high-performance neodymium-iron-boron magnet is provided, it is characterized in that the combination process adopting rapid hardening belt-rejecting technology, magnetic field assistant laser melt deposition technology combines with thermal deformation technique suppresses soft magnetism to be formed mutually, crystal grain thinning tissue, the rich neodymium Entropy density deviation of homogenizing, induced synthesis magnetic texture, prepares high-performance neodymium-iron-boron magnet fast.
The technical scheme that the present invention solves the problem is: adopt rapid hardening belt-rejecting technology, combination process that magnetic field assistant laser melt deposition technology combines with thermal deformation technique prepares high-performance neodymium-iron-boron magnet fast in the mode of successively laying and successively orientation melt deposition, obtain the heterogeneous microstructure optimized, improve magnet combination property.The steps include:
1) weigh each element raw material according to magnet composition, mixed;
2) Nd Fe B alloys strip is obtained by rapid hardening belt-rejecting technology;
3) Nd Fe B alloys strip is successively carried out magnetic field assistant laser melt deposition under protective atmosphere or vacuum, obtained neodymium iron boron magnetic body;
4) neodymium iron boron magnetic body is carried out thermal deformation, strengthening magnetic texture;
5) thermal deformation neodymium iron boron magnetic body is carried out vacuum and low temperature tempering, improve grain boundary structure, improve magnet performance.
The atomic percent of described magnet composition is Nd
ar
bfe
100-a-b-c-db
cm
d, wherein 14≤a+b≤18,0.1≤b≤5,6≤c≤8,0.1≤d≤4, R is one or more in Pr, Dy, Tb, Ho, Gd element, and M is one or more in Al, Cu, Ga, Mg, Zn, Sn, Si, Co, Ni, Nb, Zr, Ti, W, V, Hf element.
Described magnetic field is high-intensity magnetic field, and magnetic field intensity is 10-20T.
Described laser is continuous laser, and the technological parameter of Laser Melting Deposition is: laser power 300-5000W, sweep speed 10-100mm/s, spot diameter 0.2-1mm, overlapping rate 20%-80%.
Described thermal deformation technique parameter is: temperature is 650-1000 DEG C, and pressure is 50-300MPa.
Described low tempering temperatures is 480-650 DEG C, and tempering time is 0.5-4h.
Major advantage of the present invention is: the precipitation that effectively can be suppressed α-Fe soft magnetism phase by rapid hardening belt-rejecting technology, refinement principal phase Nd
2fe
14the institutional framework of B, the rich neodymium Entropy density deviation of homogenizing crystal boundary, prepares for magnetic field assistant laser melt deposition provides band and carries out tissue; The processing flexibility of magnetic field assistant laser melt deposition technology is good, be applicable to the neodymium iron boron magnetic body preparing all size and shape, can not only the certain magnetic texture of induced synthesis, and the advantage of its rapid solidification be conducive to obtaining main phase grain tiny, without the neodymium iron boron magnetic body of α-Fe soft magnetism phase, and the rich neodymium crystal boundary that hands down can be kept to be uniformly distributed; Thermal deformation technique can strengthen magnet magnetic texture further, improves magnet density.These three kinds of techniques cooperatively interact and can not only obtain the magnet institutional framework of optimization, realize the preparation of high-performance neodymium-iron-boron magnet, and simplify preparation technology, improve productivity ratio, reduce production cost.Therefore, the present invention effectively can suppress the formation of α-Fe soft magnetism phase, refinement main phase grain, reduces oxygen content, rich neodymium is uniformly distributed mutually and grain orientation good, prepare high-performance neodymium-iron-boron magnet, expand its practical ranges further.This technical process is simple, and flow process is short, is easy to operation, is suitable for large-scale batch production.Therefore, high-performance neodymium-iron-boron magnet can be prepared fast by the present invention.
Embodiment
In the present invention high-performance neodymium-iron-boron magnet be adopt rapid hardening belt-rejecting technology, combination process that magnetic field assistant laser melt deposition technology combines with thermal deformation technique is prepared from fast in the mode of successively laying and successively orientation melt deposition.First will the mixed material of assignment system be become to carry out vacuum melting by magnet; Nd Fe B alloys strip is obtained by rapid hardening belt-rejecting technology; then by Nd Fe B alloys strip under protective atmosphere or vacuum by magnetic field assistant laser melt deposition technology successively melt deposition become neodymium iron boron magnetic body; and neodymium iron boron magnetic body is carried out thermal deformation; further strengthening magnetic texture; finally thermal deformation neodymium iron boron magnetic body is carried out vacuum and low temperature tempering, optimize magnet heterogeneous microstructure further, improve magnet performance.The neodymium iron boron magnetic body crystal grain adopting the present invention to obtain is tiny, Grain-Boundary Phase is evenly distributed, magnetic texture is good, and oxygen content is low, achieves the quick preparation of high-performance neodymium-iron-boron magnet, has expanded its practical application.
Embodiment 1:
1) according to magnet composition Nd
13pr
5fe
73.6b
8al
0.3ga
0.1weigh each element raw material, mixed;
2) obtain Nd Fe B alloys strip by rapid hardening belt-rejecting technology, copper roller rotating speed is 1.0m/s;
3) Nd Fe B alloys strip is successively carried out magnetic field assistant laser melt deposition under Ar protection, magnetic field intensity is 10T, and laser power is 5000W, and sweep speed is 100mm/s, and spot diameter is 0.8mm, and overlapping rate is 60%, obtained neodymium iron boron magnetic body;
4) neodymium iron boron magnetic body is carried out thermal deformation at 700 DEG C, pressure is 100MPa, strengthening magnetic texture;
5) thermal deformation neodymium iron boron magnetic body is carried out the tempering of 0.5h vacuum and low temperature at 650 DEG C, improve grain boundary structure, improve magnet performance.
Neodymium iron boron magnetic body prepared by employing the present invention is compared with casting-thermal deformation technique, and maximum magnetic energy product improves about 13%.
Embodiment 2:
1) according to magnet composition Nd
14dy
2fe
73co
2.5b
7cu
1.5weigh each element raw material, mixed;
2) obtain Nd Fe B alloys strip by rapid hardening belt-rejecting technology, copper roller rotating speed is 1.6m/s;
3) Nd Fe B alloys strip is successively carried out magnetic field assistant laser melt deposition under vacuo, magnetic field intensity is 12T, and laser power is 1000W, and sweep speed is 50mm/s, and spot diameter is 0.5mm, and overlapping rate is 20%, obtained neodymium iron boron magnetic body;
4) neodymium iron boron magnetic body is carried out thermal deformation at 650 DEG C, pressure is 300MPa, strengthening magnetic texture;
5) thermal deformation neodymium iron boron magnetic body is carried out the tempering of 2h vacuum and low temperature at 480 DEG C, improve grain boundary structure, improve magnet performance.
Neodymium iron boron magnetic body prepared by employing the present invention is compared with casting-thermal deformation technique, and coercive force improves about 7%.
Embodiment 3:
1) according to magnet composition Nd
12pr
1ho
1fe
79.9b
6zr
0.1weigh each element raw material, mixed;
2) obtain Nd Fe B alloys strip by rapid hardening belt-rejecting technology, copper roller rotating speed is 2m/s;
3) Nd Fe B alloys strip is successively carried out magnetic field assistant laser melt deposition under vacuo, magnetic field intensity is 20T, and laser power is 300W, and sweep speed is 80mm/s, and spot diameter is 0.2mm, and overlapping rate is 80%, obtained neodymium iron boron magnetic body;
4) neodymium iron boron magnetic body is carried out thermal deformation at 1000 DEG C, pressure is 200MPa, strengthening magnetic texture;
5) thermal deformation neodymium iron boron magnetic body is carried out the tempering of 4h vacuum and low temperature at 580 DEG C, improve grain boundary structure, improve magnet performance.
Neodymium iron boron magnetic body prepared by employing the present invention is compared with casting-thermal deformation technique, and coercive force improves about 11%.
Embodiment 4:
1) according to magnet composition Nd
13pr
2gd
2fe
72.5ni
1b
8sn
1ti
0.5weigh each element raw material, mixed;
2) obtain Nd Fe B alloys strip by rapid hardening belt-rejecting technology, copper roller rotating speed is 1.2m/s;
3) Nd Fe B alloys strip is successively carried out magnetic field assistant laser melt deposition under Ar protection, magnetic field intensity is 15T, and laser power is 3000W, and sweep speed is 10mm/s, and spot diameter is 1mm, and overlapping rate is 40%, obtained neodymium iron boron magnetic body;
4) neodymium iron boron magnetic body is carried out thermal deformation at 900 DEG C, pressure is 50MPa, strengthening magnetic texture;
5) thermal deformation neodymium iron boron magnetic body is carried out the tempering of 3h vacuum and low temperature at 600 DEG C, improve grain boundary structure, improve magnet performance.
Neodymium iron boron magnetic body prepared by employing the present invention is compared with casting-thermal deformation technique, and maximum magnetic energy product improves about 10%.
Embodiment 5:
1) according to magnet composition Nd
15tb
0.1fe
76.9b
6.5cu
1ga
0.5weigh each element raw material, mixed;
2) obtain Nd Fe B alloys strip by rapid hardening belt-rejecting technology, copper roller rotating speed is 1.6m/s;
3) Nd Fe B alloys strip is successively carried out magnetic field assistant laser melt deposition under vacuo, magnetic field intensity is 18T, and laser power is 2000W, and sweep speed is 30mm/s, and spot diameter is 0.6mm, and overlapping rate is 50%, obtained neodymium iron boron magnetic body;
4) neodymium iron boron magnetic body is carried out thermal deformation at 800 DEG C, pressure is 150MPa, strengthening magnetic texture;
5) thermal deformation neodymium iron boron magnetic body is carried out the tempering of 1h vacuum and low temperature at 520 DEG C, improve grain boundary structure, improve magnet performance.
Neodymium iron boron magnetic body prepared by employing the present invention is compared with casting-thermal deformation technique, and coercive force improves about 8%.
Claims (4)
1. the quick forming method of a high-performance neodymium-iron-boron magnet, it is characterized in that, adopt band is got rid of in rapid hardening, magnetic field assistant laser melt deposition combines with thermal deformation complex method to prepare high-performance neodymium-iron-boron magnet fast in the mode of successively laying and successively orientation melt deposition; Its key step is:
A) weigh each element raw material according to magnet composition, mixed;
B) get rid of band method by rapid hardening and obtain Nd Fe B alloys strip;
C) by Nd Fe B alloys strip successively laying, under protective gas or vacuum, Nd Fe B alloys strip is successively carried out magnetic field assistant laser melt deposition, obtained neodymium iron boron magnetic body; The magnetic field intensity in described magnetic field is 10-20T, and described laser is continuous laser, and the parameter of Laser Melting Deposition is: laser power 300-5000W, sweep speed 10-100mm/s, spot diameter 0.2-1mm, overlapping rate 20%-80%;
D) neodymium iron boron magnetic body is carried out thermal deformation, strengthening magnetic texture;
E) thermal deformation neodymium iron boron magnetic body is carried out vacuum and low temperature tempering, improve grain boundary structure, improve magnet performance.
2. the quick forming method of a kind of high-performance neodymium-iron-boron magnet according to claim 1, is characterized in that, described steps A) in the atomic percent of magnet composition be Nd
ar
bfe
100-a-b-c-db
cm
d, wherein 14≤a+b≤18,0.1≤b≤5,6≤c≤8,0.1≤d≤4, R is one or more in Pr, Dy, Tb, Ho, Gd element, and M is one or more in Al, Cu, Ga, Mg, Zn, Sn, Si, Co, Ni, Nb, Zr, Ti, W, V, Hf element.
3. the quick forming method of a kind of high-performance neodymium-iron-boron magnet according to claim 1, is characterized in that, described step D) in Deformation Parameters be: temperature is 650-1000 DEG C, and pressure is 50-300MPa.
4. the quick forming method of a kind of high-performance neodymium-iron-boron magnet according to claim 1, is characterized in that, described step e) in vacuum and low temperature temperature be 480-650 DEG C, tempering time is 0.5-4h.
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| CN104599802B (en) * | 2014-12-03 | 2017-07-04 | 中国科学院宁波材料技术与工程研究所 | Rare earth permanent-magnetic material and preparation method thereof |
| CN105779886B (en) * | 2014-12-24 | 2019-02-01 | 肇庆三环京粤磁材有限责任公司 | Nd Fe B alloys vacuum smelting method |
| CN105632749B (en) * | 2015-12-29 | 2017-12-05 | 江苏大学 | A kind of preparation method of high-performance anisotropy Nanocomposite magnet |
| CN107096918B (en) * | 2017-04-18 | 2019-02-12 | 西北工业大学 | A method of preparing texturing high tenacity block materials |
| CN107768063B (en) * | 2017-11-24 | 2019-09-10 | 宁波合力磁材技术有限公司 | A kind of high-performance permanent magnet alloy material |
| CN108269683A (en) * | 2017-11-28 | 2018-07-10 | 宁波金鸡强磁股份有限公司 | A kind of method for improving neodymium iron boron magnetic body magnetic property |
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| CN102218531A (en) * | 2011-05-18 | 2011-10-19 | 山西众恒磁性材料有限公司 | Hybrid preparation method of high-performance sintered NdFeB permanent magnet |
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| CN102623166A (en) * | 2012-04-17 | 2012-08-01 | 江苏大学 | Preparation method for high performance as cast condition neodymium iron boron magnet |
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Application publication date: 20140312 Assignee: Dongtai tepusong Machinery Equipment Co.,Ltd. Assignor: Dongtai Chengdong science and Technology Pioneer Park Management Co.,Ltd. Contract record no.: X2023980043158 Denomination of invention: A Rapid Prototyping Method for High Performance Neodymium Iron Boron Magnets Granted publication date: 20160302 License type: Common License Record date: 20231012 |
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Application publication date: 20140312 Assignee: Dongtai Donggao Electronic Information Technology Co.,Ltd. Assignor: Dongtai Chengdong science and Technology Pioneer Park Management Co.,Ltd. Contract record no.: X2023980045160 Denomination of invention: A Rapid Prototyping Method for High Performance Neodymium Iron Boron Magnets Granted publication date: 20160302 License type: Common License Record date: 20231102 |
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Application publication date: 20140312 Assignee: Dongtai Gaoxin Mechanical Equipment Co.,Ltd. Assignor: Dongtai Chengdong science and Technology Pioneer Park Management Co.,Ltd. Contract record no.: X2023980046304 Denomination of invention: A Rapid Prototyping Method for High Performance Neodymium Iron Boron Magnets Granted publication date: 20160302 License type: Common License Record date: 20231110 |