CN103903823A - Rare earth permanent magnetic material and preparation method thereof - Google Patents

Rare earth permanent magnetic material and preparation method thereof Download PDF

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CN103903823A
CN103903823A CN201210577008.5A CN201210577008A CN103903823A CN 103903823 A CN103903823 A CN 103903823A CN 201210577008 A CN201210577008 A CN 201210577008A CN 103903823 A CN103903823 A CN 103903823A
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rare earth
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CN103903823B (en
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王会杰
胡元虎
赵家成
丁海浩
唐国团
郭林
陈福峰
沈是茂
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NINGBO JINJI STRONG MAGNETIC MATERIAL CO Ltd
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Abstract

The invention provides a rare earth permanent magnetic material and a preparation method thereof. The rare earth permanent magnetic material is characterized in that the rare earth permanent magnetic material is formed in the mode that a composite-structure blank composed of a magnetic phase blank and a non-magnetic phase covering the surface of the magnetic phase blank is pressed and sintered and undergoes tempering heat treatment. During preparation, firstly the magnetic phase blank is prepared in a forming stage, then non-magnetic phase mixtures comprising heavy rare earth compounds are applied to the end face of the blank, then sintering and tempering processing are carried out, and in the heat processing process, by means of grain boundary diffusion, a sintered magnet with low heavy rare earth content and high coercivity is obtained. Compared with an existing grain boundary diffusion technique, production efficiency is improved after the technique is adopted. By means of the method, heavy rare earth elements are in grain boundary of gains in the sintered magnet, and accordingly coercivity is improved and meanwhile residual magnetism is reduced to the smallest degree. By means of the method, a large magnet can be prepared, the defect that a large magnet cannot be prepared in a traditional sintered magnet grain boundary diffusion technique is overcome, and preparation and machining cost of the magnet is reduced.

Description

A kind of rare earth permanent-magnetic material and preparation method thereof
Technical field
The invention belongs to the manufacturing technology field of rare earth permanent-magnetic material, specifically a kind of low heavy rare earth high-coercive force rare earth permanent magnetic material and preparation method thereof.
Background technology
As important Metallic Functional Materials, sintered NdFeB magnet has a wide range of applications in various fields such as space flight navigation, information electronic, the energy, traffic, communication, health cares.In a lot of fields, as needed sintered NdFeB magnet to there is higher coercive force in electric automobile, hybrid vehicle and field of wind power generation, to meet the instructions for use under uniform temperature.Conventionally the way adopting is at present to add heavy rare earth element Dy, and Tb part replaces Nd and puies forward heavy alloyed coercive force and temperature stability.
Be different from light rare earth element, heavy rare earth element and transition element have the magnetic moment of arranged anti-parallel, and therefore a large amount of heavy rare earth elements replace the significantly magnetic property of reduction sintered magnet of light rare earth element.Due to the scarcity of heavy rare earth element, high-coercive force magnet has higher cost in addition.The coercive force mechanism of sintered NdFeB magnet is Nucleation Mechanism, and the forming core field of its grain boundaries reverse magnetic domain has determined the coercive force of magnet, Dy, and Tb part replaces Nd and can improve the forming core of grain boundaries reverse magnetic domain, thereby improves magnet coercive force.Add Dy according to conventional method, when Tb, the loss of remanent magnetism is that inevitably, because Dy, Tb has more entered crystal grain inside except entering crystal boundary, has reduced magnet saturation magnetization.
Research shows that it is to obtain a kind of effective way that has high-coercive force and high surplus sintered magnet concurrently that the magnet after sintering is carried out to crystal boundary diffusion again.
Patent CN200810179949.7 has introduced and has arranged alloy powder on sintered magnet surface, and powder is rare earth intermetallic compound, heat treatment temperature be 20 ℃ ~ (Ts-10) ℃, the sintering temperature that Ts is sintered magnet.Sintered magnet comprises the least part that is equal to or less than 20mm.Patent CN200810179949.7 has introduced a kind of annealing device, utilizes heavy rare earth (Tb, Dy, Ho) hydride, between 700 ℃ ~ 1000 ℃, heavy rare earth element RH is diffused into sintered magnet inside.Patent TW200822154, WO2012121351 have introduced one and first Tb, Dy element evaporation have been arrived to magnet surface, the technology that then (800 ℃ ~ 1000 ℃) carry out crystal boundary diffusion below sintering temperature.
At present there is obvious weak point in crystal boundary diffusion technique: (1), owing to utilizing in crystal boundary diffusion technique the Elements Diffusion degree of depth limited, heavy rare earth element cannot be diffused into large-size magnet inside.Therefore utilize crystal boundary diffusion technique to be suitable for preparing thickness sheet magnet (US2010282371, US20080245442), direction of orientation thickness can only be controlled within the scope of 3.5 ~ 10mm, and therefore this technology is not suitable for bulk magnet.(2) current heavy rare earth element crystal boundary diffusion technique for sintering after magnet, magnet will carry out machining before DIFFUSION TREATMENT, after DIFFUSION TREATMENT, because magnet size and surface roughness change and need to again process, processing cost is high.(3) crystal boundary diffusion technique adopts heavy rare earth element compound or metalwork compound adopt excessive coating, and the recovery of residue rare earth compound is also the key factor that affects this technical costs control.
Summary of the invention
First technical problem to be solved by this invention is to provide a kind of rare earth permanent-magnetic material, adopts heavy rare earth compound to be combined and to obtain with Magnetic Phase blank, has the feature of high remanent magnetism and high-coercive force concurrently.
First technical problem to be solved by this invention is to provide a kind of preparation method of the rare earth permanent-magnetic material that has high remanent magnetism and high-coercive force concurrently, and preparation technology is simple, can prepare bulk magnet.
The present invention solves the technical scheme that above-mentioned first technical problem adopts: a kind of rare earth permanent-magnetic material, it is characterized in that this rare earth permanent-magnetic material by Magnetic Phase blank and be coated on that the composite construction blank that the non-magnetic phase on Magnetic Phase blank surface forms is repressed, sintering, tempering heat treatment obtain, wherein the composition of Magnetic Phase blank is R x-M y-B z, R is at least one element in rare earth element; M is selected from Fe, Co, Ni, Mn, Cr, Al, Sn, Ga, Ti, Zn, Zr, Mo, Ag, W, the one or more transition elements in Nb and Cu; B is boron element, x, and y, z represents that atomic percent number and scope are: 12<x<20,5<z<7, all the other are y; Non-magnetic phase is the mixture of heavy rare-earth oxide, fluoride, chloride or hydride and Cu powder.
As preferably, the thickness 4mm ~ 30mm of Magnetic Phase blank in described composite construction blank, non-magnetic phase thickness is 0.1mm ~ 1mm.
Finally, the heavy rare earth in described non-magnetic phase refers to Tb, Dy, Ho, and heavy rare-earth oxide, fluoride, chloride or hydride are 1:1 ~ 10:1 with the mixed weight ratio of Cu powder.
The present invention solves the technical scheme that above-mentioned second technical problem adopt: a kind of preparation method of rare earth permanent-magnetic material, is characterized in that comprising the following steps:
1) prepare composite construction blank: wherein blank is made up of Magnetic Phase and non-magnetic phase, Magnetic Phase composition is R x-M y-B z, wherein R is at least one element in rare earth element; M is selected from Fe, Co, Ni, Mn, Cr, Al, Sn, Ga, Ti, Zn, Zr, Mo, Ag, W, the one or more transition elements in Nb and Cu; B is boron element, x, and y, z represents that atomic percent number and scope are: 12<x<20,5<Z<7, all the other are y; Non-magnetic phase is the mixture of heavy rare-earth oxide, fluoride, chloride or hydride and Cu powder; First-selection is prepared Magnetic Phase blank and non-magnetic phase powder, then non-magnetic phase powder is applied to the surface of Magnetic Phase blank, or non-magnetic phase powder is dispersed in organic solvent, and the slurry obtaining is applied in to Magnetic Phase blank surface, obtains composite construction blank;
2) composite construction blank is suppressed, then in vacuum or inert gas, carried out sintering and tempering heat treatment, obtain sintered magnet; Maybe multiple being superimposed of this composite construction blank suppressed, then carry out sintering and tempering heat treatment, obtain bulk sintered magnet.
As improvement, the preparation process of described Magnetic Phase blank is: the magnetic that alloy fragmentation is become to particle mean size 1 ~ 5um, this magnetic is orientated in the magnetic field of 1T ~ 5T, apply the pressure parallel or vertical with being orientated field simultaneously and carry out moulding, pressure is 50MPa ~ 100Mpa, Magnetic Phase blank single-sheet thickness 4mm~30mm.
As improvement, described alloy is to adopt strip casting, alloy preparation is become to the rapid-hardening flake of thickness 0.1mm ~ 0.5mm is prepared, and described magnetic is to adopt after Mechanical Crushing or hydrogen fragmentation, then carries out that airflow milling powder obtains.
As improvement, described non-magnetic phase is by heavy rare earth Tb, Dy, Ho oxide, fluoride, chloride or hydride are ground to the powder below 500um, and be evenly mixed to get with the Cu powder that diameter is 1um ~ 50um, described heavy rare-earth oxide, fluoride, chloride or hydride are with the mixed weight of Cu powder than being 1:1 ~ 10:1, and in described composite construction blank, non-magnetic phase thickness is 0.1mm ~ 1mm.
As preferably, the pressing pressure of described composite construction blank is 100MPa ~ 300Mpa; Pressing pressure when the multiple stacks of described composite construction blank are suppressed is 100MPa ~ 300MPa.
Preferred again, described sintering process adopts vacuum-sintering, and vacuum degree is 1 × 10 -1pa ~ 1 × 10 -5pa, sintering temperature is 1000 ℃ ~ 1200 ℃, sintering time 120 ~ 240 minutes.
Finally, described tempering heat treatment is to adopt two sections of tempering process, first stage 850~950 ℃ of insulations 60~240 minutes, 400~650 ℃ of insulations of second stage 60 ~ 180 minutes.
Compared with prior art, the invention has the advantages that: heavy rare earth compound is applied to the blank surface obtaining after the die mould of magnetic field in powder compacting process, then carries out sintering, realize the effect of heavy rare earth element in crystal boundary diffusion.Preparation method's technique of the present invention is simple, and the production efficiency raising that is improved, and the crystal boundary annex of the element of this diffusion alloy crystal grain in sintered magnet make coercive force improve simultaneously remanent magnetism and decline minimumly, and the magnet making has high remanent magnetism and high-coercive force concurrently; And can prepare the bulk magnet that thickness is greater than 100mm, overcome conventional sintering magnet crystal boundary diffusion technique and can only prepare the defect that thickness direction is less than 20mm magnet, reduce preparation and the processing cost of magnet.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1 and comparative example 1
Carry out proportioning according to component ratio, adopt purity to be greater than Nd, Fe, Co, Nb, Cu and the BFe alloy of 99% (percentage by weight).Intermediate frequency (IF) smelting in argon gas atmosphere, then casts in molten steel and rolls on the water-cooled copper roller of speed for 1.5m/s, is prepared into rapid hardening thin slice.Rapid hardening thin slice average thickness 0.25mm, composition is Nd 13.5fe balco 1nb 0.2cu 0.3b 5.5(atomic percent).
Utilize the first particle for 0.5mm left and right by alloy coarse crushing of hydrogen fragmentation or Mechanical Crushing, then utilize airflow milling powder, alloy fragmentation is become to the fine powder of particle mean size 3.8um, this magnetic is orientated in the magnetic field of 2T, apply the pressure vertical with being orientated field simultaneously and carry out moulding, pressure is 70MPa, obtains the blank that thickness direction is 8mm.
Non-magnetic phase powder preparation method is for passing through Dy 2o 3be milled to 2um left and right, and be evenly mixed to get Dy with the Cu powder that diameter is 10um 2o 3compare for 9:1 with Cu powder mixing ratio weight.
The surface that this non-magnetic phase powder is applied to Magnetic Phase blank, obtains composite construction blank.In composite construction, non-magnetic phase thickness is 0.2mm.This compound blank is waited to static pressure, and pressure is 150MPa.
In vacuum or inert gas, this composite blank is carried out to sintering, sintering process adopts vacuum-sintering, and vacuum degree is 5 × 10 -3pa, sintering temperature is 1070 ℃, sintering time is 150min.Magnet after sintering is carried out to temper, utilize two sections of tempering process, first stage 900 ℃ of insulations 120 minutes, then 520 ℃ of insulations 120 minutes.
As a comparison, prepare the blank that does not adopt compound coating structure, become magnet according to same preparation technology's preparation.
Alloying component non-magnetic phase composition and Magnetic Phase thickness and non-magnetic phase thickness etc. in embodiment 1 and comparative example 1 in table 1, are gathered.Table 2 has been listed the magnetic property of comparative example 1 and embodiment 1 magnet.As seen from the data in Table 2, embodiment 1 has 20mT to decline with respect to the remanent magnetism of comparative example 1, and coercive force significantly promotes.
Table 1
Table 2
? Br(T) Hcj(kAm -1) (BH)m(kJ/m 3)
Embodiment 1 1.42 1130 390
Comparative example 1 1.44 680 401
Embodiment 2 and comparative example 2
Carry out proportioning according to component ratio, adopt purity to be greater than Nd, Fe, Co, Nb, Cu and the BFe alloy of 99% (percentage by weight).Intermediate frequency (IF) smelting in 0.04MPA argon gas atmosphere, then casts in molten steel and rolls on the water-cooled copper roller of speed for 2m/s, is prepared into rapid hardening thin slice, rapid hardening thin slice average thickness 0.23mm, and composition is Nd 13.5fe balco 1nb 0.2cu 0.3b 5.5(atomic percent).
Utilize the first particle for 0.5mm left and right by alloy coarse crushing of hydrogen fragmentation or Mechanical Crushing, then utilize airflow milling powder, alloy fragmentation is become to the fine powder of particle mean size 3.8um, this magnetic is orientated in the magnetic field of 2T, apply the pressure parallel or vertical with being orientated field simultaneously and carry out moulding, pressure is 70MPa, obtains the blank that thickness direction is 8mm.
Non-magnetic phase powder preparation method is to be milled to 3um left and right by fluoridizing terbium, and is evenly mixed to get with the Cu powder that diameter is 10um, and dysprosium fluoride is 9:1 with Cu powder mixing ratio weight ratio.
This non-magnetic phase powder is applied on the end face of Magnetic Phase blank, obtains composite construction blank.In composite construction, non-magnetic phase thickness is 0.2mm.This compound blank is waited to static pressure, and pressure is 150MPa.
In vacuum or inert gas, this composite blank is carried out to sintering, sintering process adopts vacuum-sintering, and vacuum degree is 5 × 10 -3pa, sintering temperature is 1070 ℃, sintering time is 150min.Magnet after sintering is carried out to temper, utilize two sections of tempering process, first stage 900 ℃ of insulations 120 minutes, then 520 ℃ of insulations 120 minutes.
As a comparison, prepare the blank that does not adopt compound coating structure, become magnet according to same preparation technology's preparation.
Alloying component non-magnetic phase composition and Magnetic Phase thickness and non-magnetic phase thickness etc. in embodiment 2 and comparative example 2 in table 3, are gathered.Table 4 has been listed the magnetic property of comparative example 2 and embodiment 2 magnets.As seen from the data in Table 4, embodiment 2 has 10mT to decline with respect to the remanent magnetism of comparative example 2, and coercive force significantly promotes.
Table 3
Figure BDA00002654221100051
Table 4
? Br(T) Hcj(kAm -1) (BH)m(kJ/m 3)
Embodiment 2 1.43 1430 394
Comparative example 2 1.44 680 401
Embodiment 3 and comparative example 3
Carry out proportioning according to component ratio, adopt purity to be greater than Nd, Fe, Co, Nb, Cu and the BFe alloy of 99% (percentage by weight).Intermediate frequency (IF) smelting in 0.04MPA argon gas atmosphere, then casts in molten steel and rolls on the water-cooled copper roller of speed for 2m/s, is prepared into rapid hardening thin slice.Rapid hardening thin slice average thickness 0.23mm, composition is Nd 13.5fe balco 1nb 0.2cu 0.3b 5.5(atomic percent).
Utilize the first particle for 0.5mm left and right by alloy coarse crushing of hydrogen fragmentation or Mechanical Crushing, then utilize airflow milling powder, alloy fragmentation is become to the fine powder of particle mean size 3.8um, this magnetic is orientated in the magnetic field of 2T, apply the pressure parallel or vertical with being orientated field simultaneously and carry out moulding, pressure is 70MPa, obtains the blank that thickness direction is 8mm.
Non-magnetic phase powder preparation method is to be milled to 3um left and right by fluoridizing terbium, and is evenly mixed to get with the Cu powder that diameter is 10um, and holmium fluoride is 9:1 with Cu powder mixing ratio weight ratio.
This non-magnetic phase powder is applied on the end face of Magnetic Phase blank, obtains composite construction blank.In composite construction, non-magnetic phase thickness is 0.2mm.This compound blank is waited to static pressure, and pressure is 150MPa.
In vacuum or inert gas, this composite blank is carried out to sintering, sintering process adopts vacuum-sintering, and vacuum degree is 5 × 10 -3pa, sintering temperature is 1070 ℃, sintering time is 150min.Magnet after sintering is carried out to temper, utilize two sections of tempering process, first stage 900 ℃ of insulations 120 minutes, then 520 ℃ of insulations 120 minutes.
As a comparison, prepare the blank that does not adopt compound coating structure, become magnet according to same preparation technology's preparation.
Alloying component non-magnetic phase composition and Magnetic Phase thickness and non-magnetic phase thickness etc. in embodiment 3 and comparative example 3 in table 5, are gathered.Table 6 has been listed the magnetic property of comparative example 3 and embodiment 3 magnets.As seen from the data in Table 6, embodiment 3 has 20mT to decline with respect to the remanent magnetism of comparative example 3, and coercive force significantly promotes.
Table 5
Figure BDA00002654221100061
Table 6
? Br(T) Hcj(kAm -1) (BH)m(kJ/m 3)
Embodiment 3 1.42 930 392
Comparative example 3 1.44 680 401
Embodiment 4 and comparative example 4
Carry out proportioning according to component ratio, adopt purity to be greater than Nd, Fe, Co, Nb, Cu and the BFe alloy of 99% (percentage by weight).Intermediate frequency (IF) smelting in 0.04MPa argon gas atmosphere, then casts in molten steel and rolls on the water-cooled copper roller of speed for 1m/s, is prepared into rapid hardening thin slice.Rapid hardening thin slice average thickness 0.3mm, composition is Nd 13.5fe balco 1nb 0.2cu 0.3b 5.5(atom very).
Utilize the first particle for 0.5mm left and right by alloy coarse crushing of hydrogen fragmentation or Mechanical Crushing, then utilize airflow milling powder, alloy fragmentation is become to the fine powder of particle mean size 3.8um, this magnetic is orientated in the magnetic field of 2T, apply the pressure parallel or vertical with being orientated field simultaneously and carry out moulding, pressure is 70MPa, obtains the blank that thickness direction is 8mm.
Non-magnetic phase powder preparation method is to be milled to 3um left and right by fluoridizing terbium, and is evenly mixed to get with the Cu powder that diameter is 10um, and dysprosium fluoride is 9:1 with Cu powder mixing ratio weight ratio.
This non-magnetic phase powder is applied on the end face of Magnetic Phase blank, obtains composite construction blank.In composite construction, non-magnetic phase thickness is 0.2mm.By this, composite construction 10 is stacked adds up, and then this multilayer blank is waited to static pressure, and pressure is 150MPa.
In vacuum or inert gas, this composite blank is carried out to sintering, sintering process adopts vacuum-sintering, and vacuum degree is 5 × 10 -3pa, sintering temperature is 1070 ℃, sintering time is 150min.Magnet after sintering is carried out to temper, utilize two sections of tempering process, first stage 900 ℃ of insulations 120 minutes, then 520 ℃ of insulations 120 minutes.
As a comparison, prepare the blank that does not adopt compound coating structure, become magnet according to same preparation technology's preparation.
Alloying component non-magnetic phase composition and Magnetic Phase thickness and non-magnetic phase thickness and magnet total height in embodiment 4 and comparative example 4 in table 7, are gathered.Table 8 has been listed the magnetic property of comparative example 4 and embodiment 4 magnets.As seen from the data in Table 8, embodiment 4 has 10mT to decline with respect to the remanent magnetism of comparative example 4, and coercive force significantly promotes.
Table 7
Figure BDA00002654221100071
Table 8
? Br(T) Hcj(kAm -1) (BH)m(kJ/m 3)
Embodiment 4 1.43 1430 399
Comparative example 4 1.44 680 401
Embodiment 5-10 and comparative example 5
According to embodiment 1, with different Magnetic Phases and non-magnetic phase composition, thickness, and adopt different sintering temperatures.Table 9 shows different principal phase compositions, non-magnetic phase composition, Single Magnetic phase thickness, non-magnetic phase thickness and sintering process.Table 10 shows magnet magnetic property.
Table 9
Figure BDA00002654221100072
Figure BDA00002654221100081
Table 10
? Br(T) Hcj(kAm -1) (BH)m(kJ/m 3)
Embodiment 5 1.42 1430 385
Embodiment 6 1.42 1530 392
Embodiment 7 1.41 1730 380
Embodiment 8 1.41 1330 390
Embodiment 9 13.5 2210 346
Embodiment 10 13.6 2030 352
Comparative example 5 1.44 680 401
As seen from the data in Table 10, embodiment 5 ~ 10 has the decline of 20 ~ 90mT with respect to the remanent magnetism of comparative example 5, and coercive force significantly promotes.

Claims (10)

1. a rare earth permanent-magnetic material, it is characterized in that this rare earth permanent-magnetic material by Magnetic Phase blank and be coated on that the composite construction blank that the non-magnetic phase on Magnetic Phase blank surface forms is repressed, sintering, tempering heat treatment obtain, wherein the composition of Magnetic Phase blank is R x-M y-B z, R is at least one element in rare earth element; M is selected from Fe, Co, Ni, Mn, Cr, Al, Sn, Ga, Ti, Zn, Zr, Mo, Ag, W, the one or more transition elements in Nb and Cu; B is boron element, x, and y, z represents that atomic percent number and scope are: 12<x<20,5<z<7, all the other are y; Non-magnetic phase is the mixture of heavy rare-earth oxide, fluoride, chloride or hydride and Cu powder.
2. rare earth permanent-magnetic material according to claim 1, is characterized in that the thickness 4mm ~ 30mm of Magnetic Phase blank in described composite construction blank, and non-magnetic phase thickness is 0.1mm ~ 1mm.
3. rare earth permanent-magnetic material according to claim 1, is characterized in that the heavy rare earth in described non-magnetic phase refers to Tb, Dy, Ho, and heavy rare-earth oxide, fluoride, chloride or hydride are 1:1 ~ 10:1 with the mixed weight ratio of Cu powder.
4. a preparation method for rare earth permanent-magnetic material, is characterized in that comprising the following steps:
1) prepare composite construction blank: this composite construction blank blank is made up of Magnetic Phase and non-magnetic phase, and Magnetic Phase composition is R x-M y-B z, wherein R is at least one element in rare earth element; M is selected from Fe, Co, Ni, Mn, Cr, Al, Sn, Ga, Ti, Zn, Zr, Mo, Ag, W, the one or more transition elements in Nb and Cu; B is boron element, x, and y, z represents that atomic percent number and scope are: 12<x<20,5<Z<7, all the other are y; Non-magnetic phase is the mixture of heavy rare-earth oxide, fluoride, chloride or hydride and Cu powder; First-selection is prepared Magnetic Phase blank and non-magnetic phase powder, non-magnetic phase powder is applied to the surface of Magnetic Phase blank, or non-magnetic phase powder is dispersed in organic solvent, and the slurry obtaining is applied in to Magnetic Phase blank surface, obtains composite construction blank;
2) composite construction blank is suppressed, then in vacuum or inert gas, carried out sintering and tempering heat treatment, obtain sintered magnet; Maybe multiple being superimposed of this composite construction blank suppressed, then carry out sintering and tempering heat treatment, obtain bulk sintered magnet.
5. preparation method according to claim 4, the preparation process that it is characterized in that described Magnetic Phase blank is: the magnetic that alloy fragmentation is become to particle mean size 1 ~ 5um, this magnetic is orientated in the magnetic field of 1T ~ 5T, apply the pressure parallel or vertical with being orientated field simultaneously and carry out moulding, pressure is 50MPa ~ 100Mpa, Magnetic Phase blank single-sheet thickness 4mm ~ 30mm.
6. preparation method according to claim 5, it is characterized in that described alloy is to adopt strip casting, alloy preparation is become to the thick rapid-hardening flake of thickness 0.1 ~ 0.5mm and be prepared, described magnetic is to adopt after Mechanical Crushing or hydrogen fragmentation, then carries out that airflow milling powder obtains.
7. preparation method according to claim 4, it is characterized in that described non-magnetic phase is by heavy rare earth Tb, Dy, Ho oxide, fluoride, chloride or hydride are ground to the powder below 500um, and be evenly mixed to get with the Cu powder that diameter is 5um ~ 50um, described heavy rare-earth oxide, fluoride, chloride or hydride are with the mixed weight of Cu powder than being 1:1 ~ 10:1, and in described composite construction blank, non-magnetic phase thickness is 0.1mm ~ 1mm.
8. preparation method according to claim 4, the pressing pressure that it is characterized in that described composite construction blank is 100MPa ~ 300Mpa; Pressing pressure when the multiple stacks of described composite construction blank are suppressed is 100MPa ~ 300MPa.
9. preparation method according to claim 4, is characterized in that described sintering process adopts vacuum-sintering, and vacuum degree is 1 × 10 -1pa ~ 1 × 10 -5pa, sintering temperature is 1000 ℃ ~ 1200 ℃, sintering time 120 ~ 240 minutes.
10. preparation method according to claim 4, is characterized in that described tempering heat treatment is to adopt two sections of tempering process, first stage 850~950 ℃ of insulations 60~240 minutes, 400~650 ℃ of insulations of second stage 60 ~ 180 minutes.
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CN114864268A (en) * 2022-06-07 2022-08-05 安徽吉华新材料有限公司 Preparation method of high-coercivity regenerative magnet

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US10115507B2 (en) 2013-11-27 2018-10-30 Xiamen Tungsten Co., Ltd. Low-B bare earth magnet
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US10381139B2 (en) 2014-03-31 2019-08-13 Xiamen Tungsten Co., Ltd. W-containing R—Fe—B—Cu sintered magnet and quenching alloy
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CN105185497A (en) * 2015-08-28 2015-12-23 包头天和磁材技术有限责任公司 Preparation method of permanent magnet material
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CN105551789A (en) * 2016-02-04 2016-05-04 宁波韵升股份有限公司 Manufacturing method of rare earth permanent magnet
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CN106952721A (en) * 2017-03-15 2017-07-14 宁波金鸡强磁股份有限公司 A kind of method that high temperature compression improves rare earth permanent-magnetic material performance
CN107240469A (en) * 2017-07-06 2017-10-10 京磁材料科技股份有限公司 One kind improves the coercitive preparation method of ndfeb magnet
CN108269664A (en) * 2017-12-29 2018-07-10 中国科学院宁波材料技术与工程研究所 Rare-earth iron-boron permanent-magnet material and preparation method thereof
CN112119475A (en) * 2018-04-30 2020-12-22 星林尖端产业(株) Method for producing rare earth sintered permanent magnet
CN112119475B (en) * 2018-04-30 2022-08-09 星林尖端产业(株) Method for producing rare earth sintered permanent magnet
CN109935462A (en) * 2019-03-12 2019-06-25 宁波雄海稀土速凝技术有限公司 The preparation method and its neodymium iron boron magnetic body of grain boundary decision heavy rare earth neodymium iron boron magnetic body
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