CN103632835A - Rapid forming method of high-performance Nd-Fe-B magnetic body - Google Patents

Rapid forming method of high-performance Nd-Fe-B magnetic body Download PDF

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CN103632835A
CN103632835A CN201310638198.1A CN201310638198A CN103632835A CN 103632835 A CN103632835 A CN 103632835A CN 201310638198 A CN201310638198 A CN 201310638198A CN 103632835 A CN103632835 A CN 103632835A
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magnetic body
performance
neodymium
forming method
iron
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CN103632835B (en
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崔熙贵
崔承云
程晓农
许晓静
张洁
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Dongtai Chengdong science and Technology Pioneer Park Management Co.,Ltd.
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Jiangsu University
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Abstract

The invention discloses a rapid forming method of a high-performance Nd-Fe-B magnetic body, and relates to a preparation method of a permanent magnetic material. The rapid forming method comprises the steps of (1) weighing raw materials of each element according to the composition of a magnetic body, and mixing the raw materials; (2) preparing an Nd-Fe-B alloy strip through a rapid-hardening strip casting technology; (3) carrying out layer-by-layer magnetic-field-assisted laser melting deposition on the Nd-Fe-B alloy strip under protective atmosphere or vacuum, and preparing an Nd-Fe-B magnetic body; (4) carrying out thermal deformation on the Nd-Fe-B magnetic body, and strengthening a magnetic texture; (5)carrying out vacuum low-temperature tempering on the Nd-Fe-B magnetic body which is subjected to the thermal deformation, improving a grain boundary structure, and improving the performance of the magnetic body. The rapid forming method disclosed by the invention is suitable for preparing a large-size Nd-Fe-B magnetic body, and the prepared Nd-Fe-B magnetic body is small in grain, uniform in Nd-rich phase distribution, high in density, low in oxygen content and beneficial for improving the performance of the magnetic body. The preparation method disclosed by the invention is simple in technology, short in process, easy to operate and suitable for large-scale batch production.

Description

A kind of quick forming method of high-performance neodymium-iron-boron magnet
Technical field
The present invention relates to permanent magnetic material preparing technical field, 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 industries field, especially be suitablely applied to require in 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 of preparing high-performance neodymium-iron-boron magnet, and the maximum magnetic energy product of the Sintered NdFeB magnet making by this technique has at present approached 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 is difficult for realizing effective refinement of crystal grain.This is not only bad for the raising of neodymium iron boron magnetic body combination property, and wastes energy, and has increased production cost.
Based on this, simply cast-thermal deformation technique of preparation technology has caused widely to be paid close attention to, and it also becomes one of important method of manufacturing neodymium iron boron magnetic body.But the neodymium iron boron ingot casting that casting technique obtains exists and organize thick, lack of homogeneity, easily form α-Fe soft magnetism, equate problem, seriously restricted the raising of magnet magnetic property.Neodymium iron boron ingot structure 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, essential its microstructure, the especially ingot structure optimized.Desirable neodymium iron boron ingot structure is normally: Nd 2fe 14b Hard Magnetic phase crystal grain is tiny; Without α-Fe soft magnetism, separate out mutually and the rich neodymium of crystal boundary distributes even as far as possible mutually.For this reason, need to develop a kind of new neodymium-iron-boron preparation process, guaranteeing to have under the prerequisite of good institutional framework, simplify preparation technology, boost productivity, reduce production costs.
For the problems referred to above, the present invention proposes to adopt combination process that rapid hardening belt-rejecting technology, magnetic field assistant laser melt deposition technology combine with thermal deformation technique with laying successively and the mode that is successively orientated melt deposition, to prepare fast the method for high-performance neodymium-iron-boron magnet.Rapid hardening belt-rejecting technology can effectively suppress separating out of α-Fe soft magnetism phase, refinement principal phase Nd 2fe 14the institutional framework of B, makes rich neodymium be uniformly distributed in mutually principal phase interface; It not only provides magnetic field assistant laser melt deposition band used, and for subsequent technique, carries out tissue and 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 makes tiny, without α-Fe soft magnetism, separate out mutually, and having kept the mutually equally distributed feature of rich neodymium in rapid hardening strip, it is applicable to preparing the neodymium iron boron magnetic body of 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 has further been strengthened magnet texture on the basis of magnetic field orientating, has improved magnet density.The combination of above-mentioned three kinds of techniques not only can obtain the magnet institutional framework of optimization, and has simplified preparation technology, has reduced production cost.
Summary of the invention
The object of the invention is the problem existing for solving prior art, a kind of quick forming method of high-performance neodymium-iron-boron magnet is provided, it is characterized in that adopting the combination process inhibition soft magnetism that rapid hardening belt-rejecting technology, magnetic field assistant laser melt deposition technology combine with thermal deformation technique to form mutually, crystal grain thinning tissue, the rich neodymium of homogenizing distributes mutually, induction forms magnetic texture, prepares fast high-performance neodymium-iron-boron magnet.
The technical scheme that the present invention addresses the above problem is: adopt combination process that rapid hardening belt-rejecting technology, magnetic field assistant laser melt deposition technology combine with thermal deformation technique to prepare fast high-performance neodymium-iron-boron magnet with laying successively and the mode that is successively orientated melt deposition, obtain the heterogeneous microstructure of optimizing, improve magnet combination property.The steps include:
1) according to magnet composition, weigh each element raw material, by its mixing;
2) by rapid hardening belt-rejecting technology, make Nd Fe B alloys strip;
3) Nd Fe B alloys strip is successively carried out under protective atmosphere or vacuum to magnetic field assistant laser melt deposition, make neodymium iron boron magnetic body;
4) neodymium iron boron magnetic body is carried out to thermal deformation, strengthening magnetic texture;
5) thermal deformation neodymium iron boron magnetic body is carried out to 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, 14≤a+b≤18 wherein, 0.1≤b≤5,6≤c≤8,0.1≤d≤4, R is one or more in Pr, Dy, Tb, Ho, Gd element, 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 ℃, and pressure is 50-300MPa.
Described low tempering temperatures is 480-650 ℃, and tempering time is 0.5-4h.
Major advantage of the present invention is: by rapid hardening belt-rejecting technology, can effectively suppress separating out of α-Fe soft magnetism phase, refinement principal phase Nd 2fe 14the institutional framework of B, the rich neodymium of homogenizing crystal boundary distributes mutually, for magnetic field assistant laser melt deposition provides band and carries out tissue and prepare; The processing flexibility of magnetic field assistant laser melt deposition technology is good, be applicable to preparing the neodymium iron boron magnetic body of all size and shape, not only can induce and form certain magnetic texture, and the advantage of its rapid solidification be conducive to obtain main phase grain tiny, without the neodymium iron boron magnetic body of α-Fe soft magnetism phase, and can keep the rich neodymium crystal boundary that hands down to be uniformly distributed; Thermal deformation technique can further be strengthened magnet magnetic texture, improves magnet density.These three kinds of techniques cooperatively interact and not only can obtain the magnet institutional framework of optimization, realize the preparation of high-performance neodymium-iron-boron magnet, and have simplified preparation technology, have improved productivity ratio, have reduced production cost.Therefore, the present invention can effectively suppress the formation of α-Fe soft magnetism phase, and refinement main phase grain reduces oxygen content, rich neodymium is uniformly distributed mutually and grain orientation good, prepare high-performance neodymium-iron-boron magnet, further expand its practical ranges.This technical process is simple, and flow process is short, and easy operating is suitable for large-scale batch production.Therefore, by the present invention, can prepare fast high-performance neodymium-iron-boron magnet.
Embodiment
In the present invention, high-performance neodymium-iron-boron magnet is to adopt combination process that rapid hardening belt-rejecting technology, magnetic field assistant laser melt deposition technology combine with thermal deformation technique to be prepared from fast with laying successively and the mode that is successively orientated melt deposition.First will by magnet, become the mixed material of assignment system to carry out vacuum melting; by rapid hardening belt-rejecting technology, make Nd Fe B alloys strip; 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 to thermal deformation; further strengthen magnetic texture; finally thermal deformation neodymium iron boron magnetic body is carried out to vacuum and low temperature tempering, further optimize magnet heterogeneous microstructure, improve magnet performance.The neodymium iron boron magnetic body crystal grain that adopts the present invention to make is tiny, Grain-Boundary Phase is evenly distributed, magnetic texture is good, and oxygen content is low, has realized 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, by its mixing;
2) by rapid hardening belt-rejecting technology, make Nd Fe B alloys strip, copper roller rotating speed is 1.0m/s;
3) Nd Fe B alloys strip is successively carried out to 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%, makes neodymium iron boron magnetic body;
4) neodymium iron boron magnetic body is carried out at 700 ℃ to thermal deformation, pressure is 100MPa, strengthening magnetic texture;
5) thermal deformation neodymium iron boron magnetic body is carried out at 650 ℃ to the tempering of 0.5h vacuum and low temperature, improve grain boundary structure, improve magnet performance.
The neodymium iron boron magnetic body that adopts the present invention to prepare is compared with casting-thermal deformation technique, and maximum magnetic energy product improves approximately 13%.
Embodiment 2:
1) according to magnet composition Nd 14dy 2fe 73co 2.5b 7cu 1.5weigh each element raw material, by its mixing;
2) by rapid hardening belt-rejecting technology, make Nd Fe B alloys strip, copper roller rotating speed is 1.6m/s;
3) Nd Fe B alloys strip is successively carried out under vacuum to magnetic field assistant laser melt deposition, 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%, makes neodymium iron boron magnetic body;
4) neodymium iron boron magnetic body is carried out at 650 ℃ to thermal deformation, pressure is 300MPa, strengthening magnetic texture;
5) thermal deformation neodymium iron boron magnetic body is carried out at 480 ℃ to the tempering of 2h vacuum and low temperature, improve grain boundary structure, improve magnet performance.
The neodymium iron boron magnetic body that adopts the present invention to prepare is compared with casting-thermal deformation technique, and coercive force improves approximately 7%.
Embodiment 3:
1) according to magnet composition Nd 12pr 1ho 1fe 79.9b 6zr 0.1weigh each element raw material, by its mixing;
2) by rapid hardening belt-rejecting technology, make Nd Fe B alloys strip, copper roller rotating speed is 2m/s;
3) Nd Fe B alloys strip is successively carried out under vacuum to magnetic field assistant laser melt deposition, 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%, makes neodymium iron boron magnetic body;
4) neodymium iron boron magnetic body is carried out at 1000 ℃ to thermal deformation, pressure is 200MPa, strengthening magnetic texture;
5) thermal deformation neodymium iron boron magnetic body is carried out at 580 ℃ to the tempering of 4h vacuum and low temperature, improve grain boundary structure, improve magnet performance.
The neodymium iron boron magnetic body that adopts the present invention to prepare is compared with casting-thermal deformation technique, and coercive force improves approximately 11%.
Embodiment 4:
1) according to magnet composition Nd 13pr 2gd 2fe 72.5ni 1b 8sn 1ti 0.5weigh each element raw material, by its mixing;
2) by rapid hardening belt-rejecting technology, make Nd Fe B alloys strip, copper roller rotating speed is 1.2m/s;
3) Nd Fe B alloys strip is successively carried out to 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%, makes neodymium iron boron magnetic body;
4) neodymium iron boron magnetic body is carried out at 900 ℃ to thermal deformation, pressure is 50MPa, strengthening magnetic texture;
5) thermal deformation neodymium iron boron magnetic body is carried out at 600 ℃ to the tempering of 3h vacuum and low temperature, improve grain boundary structure, improve magnet performance.
The neodymium iron boron magnetic body that adopts the present invention to prepare is compared with casting-thermal deformation technique, and maximum magnetic energy product improves approximately 10%.
Embodiment 5:
1) according to magnet composition Nd 15tb 0.1fe 76.9b 6.5cu 1ga 0.5weigh each element raw material, by its mixing;
2) by rapid hardening belt-rejecting technology, make Nd Fe B alloys strip, copper roller rotating speed is 1.6m/s;
3) Nd Fe B alloys strip is successively carried out under vacuum to magnetic field assistant laser melt deposition, 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%, makes neodymium iron boron magnetic body;
4) neodymium iron boron magnetic body is carried out at 800 ℃ to thermal deformation, pressure is 150MPa, strengthening magnetic texture;
5) thermal deformation neodymium iron boron magnetic body is carried out at 520 ℃ to the tempering of 1h vacuum and low temperature, improve grain boundary structure, improve magnet performance.
The neodymium iron boron magnetic body that adopts the present invention to prepare is compared with casting-thermal deformation technique, and coercive force improves approximately 8%.

Claims (6)

1. the quick forming method of a high-performance neodymium-iron-boron magnet, it is characterized in that, adopt rapid hardening to get rid of complex method that band, magnetic field assistant laser melt deposition combine with thermal deformation and prepare fast high-performance neodymium-iron-boron magnet with laying successively and the mode that is successively orientated melt deposition; Its key step is:
A) according to magnet composition, weigh each element raw material, by its mixing;
B) by rapid hardening, get rid of band method and make Nd Fe B alloys strip;
C) by Nd Fe B alloys strip laying successively, under protective gas or vacuum, Nd Fe B alloys strip is successively carried out to magnetic field assistant laser melt deposition, make neodymium iron boron magnetic body;
D) neodymium iron boron magnetic body is carried out to thermal deformation, strengthening magnetic texture;
E) thermal deformation neodymium iron boron magnetic body is carried out to 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, 14≤a+b≤18 wherein, 0.1≤b≤5,6≤c≤8,0.1≤d≤4, R is one or more in Pr, Dy, Tb, Ho, Gd element, 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 C) in the magnetic field intensity in magnetic field be 10-20T.
4. the quick forming method of a kind of high-performance neodymium-iron-boron magnet according to claim 1, it is characterized in that, described step C) laser in is continuous laser, 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%.
5. 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 ℃, and pressure is 50-300MPa.
6. 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 ℃, tempering time is 0.5-4h.
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CN104599802A (en) * 2014-12-03 2015-05-06 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
CN105632749A (en) * 2015-12-29 2016-06-01 江苏大学 Preparation method for high-performance anisotropic nano-composite magnet
CN105779886A (en) * 2014-12-24 2016-07-20 肇庆三环京粤磁材有限责任公司 Vacuum smelting method of neodymium iron boron alloy
CN107096918A (en) * 2017-04-18 2017-08-29 西北工业大学 A kind of method for preparing texturing high tenacity block materials
CN107768063A (en) * 2017-11-24 2018-03-06 周慧媛 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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Cited By (9)

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Publication number Priority date Publication date Assignee Title
CN104599802A (en) * 2014-12-03 2015-05-06 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
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CN105632749A (en) * 2015-12-29 2016-06-01 江苏大学 Preparation method for high-performance anisotropic nano-composite magnet
CN107096918A (en) * 2017-04-18 2017-08-29 西北工业大学 A kind of method for preparing texturing high tenacity block materials
CN107096918B (en) * 2017-04-18 2019-02-12 西北工业大学 A method of preparing texturing high tenacity block materials
CN107768063A (en) * 2017-11-24 2018-03-06 周慧媛 A kind of high-performance permanent magnet alloy material
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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Record date: 20231102

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EE01 Entry into force of recordation of patent licensing contract

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