CN102496437A - Anisotropic nanocrystal complex-phase compact block neodymium-iron-boron permanent-magnet material and preparation method thereof - Google Patents

Anisotropic nanocrystal complex-phase compact block neodymium-iron-boron permanent-magnet material and preparation method thereof Download PDF

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CN102496437A
CN102496437A CN201110386059.5A CN201110386059A CN102496437A CN 102496437 A CN102496437 A CN 102496437A CN 201110386059 A CN201110386059 A CN 201110386059A CN 102496437 A CN102496437 A CN 102496437A
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hot pressing
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CN102496437B (en
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陈仁杰
唐旭
唐鑫
尹文宗
李东
闫阿儒
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Ningbo Institute of Material Technology and Engineering of CAS
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Abstract

The invention relates to an anisotropic nanocrystal complex-phase compact block neodymium-iron-boron permanent-magnet material which is characterized by comprising a nanocrystal-structure hard magnetic phase and a soft magnetic phase, wherein the hard magnetic phase is a (Nd,R)2Fe17B phase, and R is selected from at least one of La, Ce, Pr, Gd, Tb and Dy; and the soft magnetic phase is at least one of alpha-Fe alpha-FeCo or Fe3B. The invention also discloses a preparation method of the permanent-magnet material. Compared with the prior art, the permanent-magnet material has the following advantages: due to the introduction of the soft magnetic phase, the coercive force of the nano complex-phase magnet is far lower than that of the single hard magnetic phase magnet, and the liquid phase is diffused into the nano complex-phase magnet and positioned at the grain boundary, thereby obviously enhancing the coercive force of the magnet.

Description

The nanocrystalline complex phase densification of anisotropy block Nd-Fe-Bo permanent magnet material and preparation method thereof
Technical field
The present invention relates to a kind of permanent magnetic material, the invention still further relates to the preparation method of this permanent magnetic material.
Background technology
From third generation rare earth permanent-magnetic material-Nd eighties in last century 2Fe 14Since B found, the researchers of countries in the world carried on further investigation, the new rare-earth permanent magnetic material that the expectation discovery has excellent permanent magnetism performance.The development novel high-performance permanent magnetic material that is found to be of nanometer complex phase permanent material has been opened up new thinking, has important scientific meaning and huge economic.Isotropic nanocrystalline complex phase permanent material is representative with the high magnetic energy fast quenching magnetic of wheat lattice elder brother magnetic exploitation at present; Form with bonded permanent magnet is able to extensive use; Because this magnetic shows magnetic isotropy; And density is not high after making bonded permanent magnet, causes the magnet magnetic property not high, well below the anisotropic sintered Nd-Fe-B permanent magnetic material of densification.The macroscopic view magnetic anisotropy is the necessary condition that obtains high permanent magnetism performance, how to realize that the magnetic anisotropy of nanometer complex phase rare earth permanent magnetism material is current to remain physically and technical huge challenge.
Hot pressing/thermal deformation technology is the effective means of preparation block theoretical density anisotropy nanometer permanent magnet.It is generally acknowledged, because tetragonal Nd 2Fe 14The anisotropy of B crystal grain modulus of elasticity and strain energy; Dissolving-deposition-diffusion-the creep process that takes place in the high rare-earth content neodymium iron boron hot flowage; Make magnet form the sheet crystal structure; Obtain strong magnetic anisotropy, the existence of rich rare earth liquid phase obtains texture to high rare-earth content magnet hot pressing/thermal deformation and has important function.In order in anisotropy hot pressing/heat distortion magnet, to introduce soft/Hard Magnetic multiphase structure; U.S. Dayton university; Korea S Pukyong national university adopts modes such as rich rare earth quenched powder mixes with poor rare earth quenched powder, soft magnetism particle interpolation mutually, plated film to attempt with the researchers of research institutions such as U.S. Delaware university, has obtained certain progress.Micro-Structure Analysis shows; Macroscopic anisotropy comes from the formation of the Hard Magnetic phase texture that has the zone generation of rich rare earth liquid phase; The orientation and poor rare earth zone does not wherein deform basically; So desire obtains excellent orientation, then the content of soft magnetism phase receives very big restriction, and this is unfavorable for the performance of the advantage of soft/Hard Magnetic built-up magnet.
Do not rely on rich rare earth liquid phase, directly content of rare earth is lower than the nanocrystalline complex phase magnet that is just dividing and carries out hot pressing/Thermal Deformation and show that magnet also can obtain anisotropy to a certain degree.At this moment, Hard Magnetic phase texture derives from the shearing deformation that takes place under the pressure effect, i.e. Nd 2Fe 14The anisotropy of B crystal grain modulus of elasticity causes the slippage and the rotation of crystal face, realizes the texture of crystal grain.Yet the degree of orientation of magnet and magnetic property are starkly lower than high rare earth hot pressing/thermal deformation Nd 2Fe 14The level of B magnet, and along with the soft magnetism phase content increases, the degree of orientation and the magnetic property of magnet descend rapidly, need higher pressure simultaneously, harsh to process conditions and equipment requirements.In the recent period, the domestic researcher of University On The Mountain Of Swallows through strong pressure (~310MPa) effect noncrystal substrate hot flowage is down separated out nanocrystalline multiphase structure, and the texture of forming core realization Hard Magnetic phase according to qualifications takes place simultaneously.This noncrystal substrate that utilizes is realized anisotropy, and keeps the research of soft or hard magnetic phase crystal grain boundary coherence still to be in the initial exploration stage, and the magnet magnetic property of preparation and single-phase hot pressing/heat distortion magnet still have big gap at present.
Introduce the rich rare earth liquid phase of an amount of low melting point if in the nanocrystalline complex phase magnet of poor rare earth, adopt the method for crystal boundary diffusion; Can realize that then soft or hard magnetic and liquid phase coexist; Satisfy the needed deformation orientation condition of hot pressing/thermal deformation technology, the block magnet of anisotropy nanometer complex phase that preparation is fine and close.The present invention proposes a kind of low melting point liquid phase alloy that utilizes and diffuses into the fast quenching magnetic along crystal boundary; Improving the deformation orientation ability of poor rare-earth nano-crystal complex phase fast quenching magnetic in thermal deformation process, thereby preparation has the brilliant complex phase permanent material of the densification lumpy nanometer of macroscopic anisotropy.
Summary of the invention
Technical problem to be solved by this invention is the nanocrystalline complex phase densification of the anisotropy block Nd-Fe-Bo permanent magnet material that a kind of high-coercive force is provided to the above-mentioned state of the art.
Another technical problem to be solved by this invention provides a kind of preparation method that can significantly improve the nanocrystalline complex phase densification of the coercitive anisotropy of magnet block Nd-Fe-Bo permanent magnet material.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: the nanocrystalline complex phase densification of a kind of anisotropy block Nd-Fe-Bo permanent magnet material; It is characterized in that hard magnetic that this permanent magnetic material includes nanocrystalline structure mutually with soft magnetism mutually; Aforesaid hard magnetic be mutually (Nd, R) 2Fe 14The B phase, wherein R is selected from least a among La, Ce, Pr, Gd, Tb and the Dy, and aforesaid soft magnetism is at least a among α-Fe, α-FeCo or the Fe3B mutually, and soft magnetism is 2~40% with the mutually shared volume ratio scope of permanent magnetism.
The preparation method of the nanocrystalline complex phase densification of a kind of anisotropy block Nd-Fe-Bo permanent magnet material comprises the steps:
1. utilize rapid quenching technique to prepare Nd 2Fe 14B/ α-Fe base, Nd 2Fe 14B/Fe 3B base or Nd 2Fe 14B/ α-FeCo base nanometer crystal complex phase quick quenching band, and be broken into the principal phase powder that particle diameter is no more than 300 μ m;
2. be that composition prepares the low melting point liquid phase alloy RM that fusing point is lower than 800 ℃ with rare earth element and magnesium-yttrium-transition metal; And be broken into the liquid phase powder that particle diameter is no more than 50 μ m; Or this low melting point liquid phase alloy processed target; R wherein is selected from least a among La, Ce, Pr, Nd, Gd, Tb and the Dy, and M is at least a among Al, Cu, Ga, Co, the Sn;
3. evenly be coated on the principal phase powder surface with liquid phase alloy and principal phase powder, or with the liquid phase alloy, obtain mixed-powder;
4. mixed-powder is carried out hot pressing under vacuum or protective atmosphere and prepare the block blank, or mixed-powder is carried out earlier the elevated temperature heat DIFFUSION TREATMENT carry out hot pressing again and prepare the block blank in vacuum or under protective atmosphere;
5. the block blank is carried out thermal deformation orientation preparation anisotropy magnet, or the hot pressing blank is carried out earlier the elevated temperature heat DIFFUSION TREATMENT carry out thermal deformation again and prepare anisotropy magnet under vacuum or protective atmosphere.
Further, described liquid phase alloy and main-phase alloy mass ratio range are 0.5: 99.5~15: 85.
Further, the hot pressing preparation condition of step in 4. is following: 500~850 ℃ of hot pressing temperatures, and pressure 100~500MPa, vacuum degree is higher than 1 * 10 -2Carry out hot pressing under the Pa condition and prepare the block blank.
Further, the elevated temperature heat DIFFUSION TREATMENT condition of step in 4. is following: temperature 500-850 ℃, and temperature retention time 30~120 minutes, vacuum degree was higher than 1 * 10 when vacuum condition was handled down -2Protection gas was argon gas when Pa, protective atmosphere environment handled down, and air pressure is lower than 0.2Mpa.
Further, the condition of the thermal deformation orientation preparation of step in 5. is following: 700~850 ℃ of heat distortion temperatures, and pressure 100~500MPa, vacuum degree is higher than 1 * 10 -2Pa, or charge into protection gas argon pressure about 10 after vacuumizing 2Pa.
Compared with prior art, the invention has the advantages that: generally speaking, only tens microns of commercial neodymium iron boron fast quenching magnetic thickness carry out Liquid Phase Diffusion to quenched powder, can be easy to realize sufficient diffusion effect; On the basis that can soft or hard magnetic coexists mutually through Liquid Phase Diffusion, introduce sufficient liquid phase alloy, satisfy hot pressing/required liquid phase of hot flowage orientation, obtain the texture of hard magnetic phase, realize the macroscopic anisotropy of magnet; Utilize the magnet of hot pressing/thermal deformation prepared to have fine and close structure, density is high, and has anisotropy, and its magnetic property is far above present nanometer complex phase bonded permanent magnet; Because magnet has soft/hard magnetic phase nanometer coupled structure, the rare earth consumption is few, helps the saving of rare earth resources; Because the introducing of soft magnetism phase, the coercive force of nanometer complex phase magnet be far below the coercive force of single hard magnetic phase magnet, Liquid Phase Diffusion is advanced in the nanometer complex phase magnet and is positioned at the crystal boundary place, can significantly improve the magnet coercive force.
Description of drawings
Fig. 1 is the electronic scanning displaing micro picture of the final magnet section of preparation among the embodiment 2.
Embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Embodiment 1:
1, utilize fast melt-quenching technology preparation nanometer complex phase quick quenching band, and be broken into the powder of particle diameter 150 μ m, alloying component is Nd21.452Pr0.42Fe74.294Co0.674B0.98Al0.479Cu0.11Nb1.591 (a quality percentage composition);
2, utilize fast melt-quenching technology preparation fusing point to be lower than 800 ℃ low melting point Nd90Cu10 liquid phase alloy, be broken into the powder of 50 μ m;
3, multiphase alloy powder and liquid phase alloy powder are mixed with 95: 5 mass ratioes;
4, place mould to put into vacuum hotpressing stove in powder and be evacuated to 6 * 10 -3Behind the Pa, be warming up to 700 ℃, pressurization 270MPa, taking-up is cooled off in pressurize after 1 minute;
5, place mould to put into vacuum hotpressing stove the hot pressing blank and be evacuated to 6 * 10 -3Behind the Pa, charge into 10 2The Pa argon gas is warming up to 850 ℃, pressurization 10 5The MPa orientation that deforms, taking-up is cooled off in pressurize after 0.5 minute, obtain anisotropy nanometer complex phase permanent material.
Embodiment 2:
1, utilize fast melt-quenching technology preparation nanometer complex phase quick quenching band, and be broken into the powder of particle diameter 150 μ m, alloying component is Nd21.452Pr0.42Fe74.294Co0.674B0.98Al0.479Cu0.11Nb1.591 (a quality percentage composition);
2, utilize fast melt-quenching technology preparation fusing point to be lower than 800 ℃ low melting point Nd90Cu10 liquid phase alloy, be broken into the powder of 50 μ m;
3, multiphase alloy powder and liquid phase alloy powder are mixed with 92: 8 mass ratioes;
4, place mould to put into vacuum hotpressing stove in powder and be evacuated to 6 * 10 -3Behind the Pa, be warming up to 700 ℃, pressurization 270MPa, taking-up is cooled off in pressurize after 40 seconds;
5, place mould to put into vacuum hotpressing stove the hot pressing blank and be evacuated to 6 * 10 -3Behind the Pa, charge into 10 2The Pa argon gas is warming up to 850 ℃, pressurization 10 5The MPa orientation that deforms, taking-up is cooled off in pressurize after 0.5 minute, obtain anisotropy nanometer complex phase permanent material.
The microstructure use emission scan electron microscope observation of final magnet, shown in accompanying drawing 1, its crystal grain forms sheet crystal structure uniformly, explains that magnet has taken place to form macroscopic anisotropy than the significant deformation orientation in thermal deformation process.
Embodiment 3:
1, utilize fast melt-quenching technology preparation nanometer complex phase quick quenching band, and be broken into the powder of particle diameter 150 μ m, alloying component is Nd21.452Pr0.42Fe74.294Co0.674B0.98Al0.479Cu0.11Nb1.591 (a quality percentage composition);
2, utilize fast melt-quenching technology preparation fusing point to be lower than 800 ℃ low melting point Nd90Cu10 liquid phase alloy, be broken into the powder of 50 μ m;
3, multiphase alloy powder and liquid phase alloy powder are mixed with 92: 8 mass ratioes;
4, place mould to put into vacuum hotpressing stove in powder and be evacuated to 6 * 10 -3Behind the Pa, be warming up to 700 ℃, pressurization 270MPa, taking-up is cooled off in pressurize after 1 minute;
5, with hot pressing blank timeliness 30 minutes under 400 ℃ of vacuum environments;
6, place mould to put into vacuum hotpressing stove the hot pressing blank and be evacuated to 6 * 10 -3Behind the Pa, charge into 10 2The Pa argon gas is warming up to 850 ℃, pressurization 10 5The MPa orientation that deforms, taking-up is cooled off in pressurize after 0.5 minute, obtain anisotropy nanometer complex phase permanent material.
Embodiment 4:
1, utilize fast melt-quenching technology preparation nanometer complex phase quick quenching band, and be broken into the powder of particle diameter 150 μ m, alloying component is Nd21.452Pr0.42Fe74.294Co0.674B0.98Al0.479Cu0.11Nb1.591 (a quality percentage composition);
2, utilize fast melt-quenching technology preparation low melting point Nd90Cu10 liquid phase alloy, be broken into the powder of 50 μ m;
3, multiphase alloy powder and liquid phase alloy powder are mixed with 90: 10 mass ratioes;
4, place mould to put into vacuum hotpressing stove in powder and be evacuated to 6 * 10 -3Behind the Pa, be warming up to 700 ℃, pressurization 270MPa, taking-up is cooled off in pressurize after 1 minute;
5, place mould to put into vacuum hotpressing stove the hot pressing blank and be evacuated to 6 * 10 -3Behind the Pa, charge into 10 2The Pa argon gas is warming up to 850 ℃, the pressurization 105MPa orientation that deforms, and taking-up is cooled off in pressurize after 0.5 minute, acquisition anisotropy nanometer complex phase permanent material.
Table 1 for each embodiment preparation anisotropy nanometer complex phase magnet magnetic property
Magnet type Remanent magnetism (kGs) HCJ Hcj (kOe) Magnetic energy product (MGOe)
Embodiment 1 9.79 9.72 20.10
Embodiment 2 10.95 13.64 26.30
Embodiment 3 10.61 14.76 24.86
Embodiment 4 10.92 14.83 27.70
Can know from the foregoing description; Through low melting point Liquid Phase Diffusion method; Strengthen the texture of nanometer complex phase neodymium iron boron base fast quenching magnetic in thermal deformation process and formed ability, successfully prepared the block magnet of the densification anisotropy with soft/hard magnetic phase nano composite structure.

Claims (6)

1. the nanocrystalline complex phase densification of anisotropy block Nd-Fe-Bo permanent magnet material, it is characterized in that hard magnetic that this permanent magnetic material includes nanocrystalline structure mutually with soft magnetism mutually, aforesaid hard magnetic be mutually (Nd, R) 2Fe 14The B phase, wherein R is selected from least a among La, Ce, Pr, Gd, Tb and the Dy, and aforesaid soft magnetism is α-Fe, α-FeCo or Fe mutually 3At least a among the B, soft magnetism is 2~40% with the mutually shared volume ratio scope of permanent magnetism.
2. the preparation method of the nanocrystalline complex phase densification of the described anisotropy of claim 1 a block Nd-Fe-Bo permanent magnet material is characterized in that comprising the steps:
1. utilize rapid quenching technique to prepare Nd 2Fe 14B/ α-Fe base, Nd 2Fe 14B/Fe 3B base or Nd 2Fe 14B/ α-FeCo base nanometer crystal complex phase quick quenching band, and be broken into the principal phase powder that particle diameter is no more than 300 μ m;
2. be that composition prepares the low melting point liquid phase alloy RM that fusing point is lower than 800 ℃ with rare earth element and magnesium-yttrium-transition metal; And be broken into the liquid phase powder that particle diameter is no more than 50 μ m; Or this low melting point liquid phase alloy processed target; R wherein is selected from least a among La, Ce, Pr, Nd, Gd, Tb and the Dy, and M is at least a among Al, Cu, Ga, Co, the Sn;
3. evenly be coated on the principal phase powder surface with liquid phase alloy and principal phase powder, or with the liquid phase alloy, obtain mixed-powder;
4. mixed-powder is carried out hot pressing under vacuum or protective atmosphere and prepare the block blank, or mixed-powder is carried out earlier the elevated temperature heat DIFFUSION TREATMENT carry out hot pressing again and prepare the block blank in vacuum or under protective atmosphere;
5. the block blank is carried out thermal deformation orientation preparation anisotropy magnet, or the hot pressing blank is carried out earlier the elevated temperature heat DIFFUSION TREATMENT carry out thermal deformation again and prepare anisotropy magnet under vacuum or protective atmosphere.
3. preparation method according to claim 2 is characterized in that described liquid phase alloy and main-phase alloy mass ratio range are 0.5: 99.5~15: 85.
4. preparation method according to claim 2 is characterized in that the hot pressing preparation condition during step is 4. is following: 500~850 ℃ of hot pressing temperatures, and pressure 100~500MPa, vacuum degree is higher than 1 * 10 -2Carry out hot pressing under the Pa condition and prepare the block blank.
5. preparation method according to claim 2 is characterized in that the elevated temperature heat DIFFUSION TREATMENT condition during step is 4. is following: temperature 500-850 ℃, and temperature retention time 30~120 minutes, vacuum degree was higher than 1 * 10 when vacuum condition was handled down -2Protection gas was argon gas when Pa, protective atmosphere environment handled down, and air pressure is lower than 0.2Mpa.
6. preparation method according to claim 2 is characterized in that the condition of the thermal deformation orientation preparation during step is 5. is following: 700~850 ℃ of heat distortion temperatures, and pressure 100~500MPa, vacuum degree is higher than 1 * 10 -2Pa, or charge into protection gas argon pressure about 10 after vacuumizing 2Pa.
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CN103123839A (en) * 2013-01-30 2013-05-29 浙江大学 Rare earth permanent magnet produced by applying abundant rare earth cerium (Ce) and preparation method thereof
CN103258609A (en) * 2013-05-14 2013-08-21 深圳大学 Anisotropism nanometer rare earth permanent magnetic material and preparation method thereof
CN103310933A (en) * 2013-05-10 2013-09-18 安徽大地熊新材料股份有限公司 Method for preparing sintered Nd-Fe-B under high pressure
CN103489619A (en) * 2013-10-14 2014-01-01 北京科技大学 Method for preparing dense fine-grain neodymium iron boron sintering magnet
CN103794324A (en) * 2014-02-26 2014-05-14 江门市新会区宇宏科技有限责任公司 Method for preparing nanocrystalline complex phase permanent magnetic powder
CN104584147A (en) * 2012-07-10 2015-04-29 罗伯特·博世有限公司 Magnetic material, use thereof and method for the production thereof
CN104707990A (en) * 2013-12-11 2015-06-17 北京中科三环高技术股份有限公司 Method for improving coercive force of neodymium iron boron quick-quenching nanocrystalline magnetic powder
CN105321648A (en) * 2015-10-20 2016-02-10 浙江英洛华磁业有限公司 Thermal deformation composite permanent magnet and preparation method therefor
CN105321646A (en) * 2015-11-25 2016-02-10 中国科学院宁波材料技术与工程研究所 Nanocrystalline thermal deformation rare-earth permanent magnet with high coercivity and preparation method of nanocrystalline thermal deformation rare-earth permanent magnet
CN105355411A (en) * 2015-11-25 2016-02-24 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
CN105869876A (en) * 2016-04-06 2016-08-17 中国科学院宁波材料技术与工程研究所 Rare-earth permanent magnet and fabrication method thereof
WO2017041741A1 (en) * 2015-09-10 2017-03-16 燕山大学 Permanent magnet material and preparation method thereof
CN108987016A (en) * 2018-07-13 2018-12-11 杭州电子科技大学 A kind of preparation process of nano-crystal neodymium iron boron magnetic body
US10629341B2 (en) 2016-08-22 2020-04-21 Ford Global Technologies, Llc Magnetic phase coupling in composite permanent magnet
CN111627631A (en) * 2020-03-19 2020-09-04 中国科学院宁波材料技术与工程研究所 Preparation method of nano composite permanent magnetic material

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CN103123839B (en) * 2013-01-30 2015-04-22 浙江大学 Rare earth permanent magnet produced by applying abundant rare earth cerium (Ce) and preparation method thereof
CN103123839A (en) * 2013-01-30 2013-05-29 浙江大学 Rare earth permanent magnet produced by applying abundant rare earth cerium (Ce) and preparation method thereof
CN103310933A (en) * 2013-05-10 2013-09-18 安徽大地熊新材料股份有限公司 Method for preparing sintered Nd-Fe-B under high pressure
CN103258609A (en) * 2013-05-14 2013-08-21 深圳大学 Anisotropism nanometer rare earth permanent magnetic material and preparation method thereof
CN103489619A (en) * 2013-10-14 2014-01-01 北京科技大学 Method for preparing dense fine-grain neodymium iron boron sintering magnet
CN103489619B (en) * 2013-10-14 2016-01-20 北京科技大学 The preparation method of the thin brilliant sintered NdFeB magnet of a kind of densification
CN104707990A (en) * 2013-12-11 2015-06-17 北京中科三环高技术股份有限公司 Method for improving coercive force of neodymium iron boron quick-quenching nanocrystalline magnetic powder
CN104707990B (en) * 2013-12-11 2019-06-14 北京中科三环高技术股份有限公司 A kind of coercitive method of raising neodymium iron boron fast quenching nanocrystalline magnetic
CN103794324A (en) * 2014-02-26 2014-05-14 江门市新会区宇宏科技有限责任公司 Method for preparing nanocrystalline complex phase permanent magnetic powder
WO2017041741A1 (en) * 2015-09-10 2017-03-16 燕山大学 Permanent magnet material and preparation method thereof
US10249418B2 (en) 2015-09-10 2019-04-02 Yanshan University Permanent magnet material and method for preparing the same
CN105321648A (en) * 2015-10-20 2016-02-10 浙江英洛华磁业有限公司 Thermal deformation composite permanent magnet and preparation method therefor
CN105321646A (en) * 2015-11-25 2016-02-10 中国科学院宁波材料技术与工程研究所 Nanocrystalline thermal deformation rare-earth permanent magnet with high coercivity and preparation method of nanocrystalline thermal deformation rare-earth permanent magnet
CN105355411B (en) * 2015-11-25 2019-01-29 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
CN105355411A (en) * 2015-11-25 2016-02-24 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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US10629341B2 (en) 2016-08-22 2020-04-21 Ford Global Technologies, Llc Magnetic phase coupling in composite permanent magnet
CN108987016A (en) * 2018-07-13 2018-12-11 杭州电子科技大学 A kind of preparation process of nano-crystal neodymium iron boron magnetic body
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CN111627631B (en) * 2020-03-19 2022-07-05 中国科学院宁波材料技术与工程研究所 Preparation method of nano composite permanent magnetic material

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