CN103106991B - Based on high-coercive force high-stability neodymium iron boron magnet and the preparation method of crystal boundary reconstruct - Google Patents
Based on high-coercive force high-stability neodymium iron boron magnet and the preparation method of crystal boundary reconstruct Download PDFInfo
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 34
- 239000013078 crystal Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 106
- RZJQYRCNDBMIAG-UHFFFAOYSA-N [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] Chemical class [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] RZJQYRCNDBMIAG-UHFFFAOYSA-N 0.000 claims abstract description 62
- 238000000034 method Methods 0.000 claims abstract description 48
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 36
- 238000005275 alloying Methods 0.000 claims abstract description 35
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 230000008569 process Effects 0.000 claims abstract description 20
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011812 mixed powder Substances 0.000 claims abstract description 15
- 238000005516 engineering process Methods 0.000 claims abstract description 11
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- 238000009826 distribution Methods 0.000 claims abstract description 8
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
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- 239000011858 nanopowder Substances 0.000 claims description 41
- 239000000203 mixture Substances 0.000 claims description 31
- 230000001681 protective effect Effects 0.000 claims description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 13
- 238000003801 milling Methods 0.000 claims description 12
- 238000005496 tempering Methods 0.000 claims description 12
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 10
- 229910045601 alloy Inorganic materials 0.000 claims description 10
- 239000000956 alloy Substances 0.000 claims description 10
- 238000005266 casting Methods 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 229910052779 Neodymium Inorganic materials 0.000 claims description 8
- 229910052737 gold Inorganic materials 0.000 claims description 8
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 229910052771 Terbium Inorganic materials 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
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- 229910052691 Erbium Inorganic materials 0.000 claims description 6
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 6
- 229910052689 Holmium Inorganic materials 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
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- 238000000227 grinding Methods 0.000 claims description 6
- 229910052745 lead Inorganic materials 0.000 claims description 6
- 229910052748 manganese Inorganic materials 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- 229910052758 niobium Inorganic materials 0.000 claims description 6
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- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 229910052720 vanadium Inorganic materials 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 5
- 230000001629 suppression Effects 0.000 claims description 5
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 3
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
The invention discloses a kind of high-coercive force high-stability neodymium iron boron magnet based on crystal boundary reconstruct and preparation method thereof.Its key step comprises: master alloying, crystal-boundary phase alloy powder be design and preparation, Grain-Boundary Phase nano modification, mixed powder, magnetic field die mould, isostatic pressed, sintering and heat treatment separately.The present invention is based on crystal boundary reconstruct new technology, the rich new Grain-Boundary Phase of heavy rare earth of Application of composite and nano modification technology, namely redesign and the new Grain-Boundary Phase of the rich heavy rare earth of synthesis, in magnet sintering and temper process, realize magnetic hardening by heavy rare earth element to the diffusion in main phase grain boundary layer, do not add or add less the condition of heavy rare earth in principal phase under, prepare low cost high-coercivity magnet; Optimized distribution and the grain boundary form of Grain-Boundary Phase by nano modification method, pinning domain wall suppresses counter magnetic field forming core, inhibiting grain growth, thus the high-coercive force high stability realizing neodymium iron boron magnetic body simultaneously.Preparation method's technique provided by the invention is simple, and cost is lower, is applicable to large-scale mass production.
Description
Technical field
The present invention relates to a kind of high-coercive force high-stability neodymium iron boron magnet based on crystal boundary reconstruct and preparation method.
Background technology
Nd-Fe-B has the incomparable advantage of the other types such as high energy product, high performance-price ratio permanent magnetic material, is current most widely used rare earth permanent-magnetic material.By 2015, the world demand amount of neodymium iron boron product will up to 200,000 tons, and as seen in the time that future is longer, NdFeB material still can take on important role in modern information technologies industry.
The key technical indexes weighing Nd-Fe-B permanent magnetic performance comprises remanent magnetism
b r, maximum magnetic energy product (
bH)
max, coercive force
h cand Curie temperature
t c.Through effort for many years, the theoretical and optimum preparation condition based on comparatively ripe design of alloy,
b rreaching 1.555T, is more than 96% of theoretical value; (
bH)
maxreaching 474kJ/m3, is more than 92% of theoretical value.And
h calthough achieve certain lifting, be still only 1/10 ~ 1/3 of theoretical value, make the temperature stability of magnet poor, greatly limit the application of magnet in the field such as precision instrumentation, Aero-Space.Therefore, improve neodymium iron boron coercive force, the temperature stability promoting magnet is the key expanding range of application further, is need a difficult problem of capturing badly.
Add doping type element, by crystal grain thinning, improve the coercive force that micro-structural etc. can increase magnet to a certain extent, but amplification can not be very high, and the magnetic diluting effect that large addition causes can make the magnetic property of magnet reduce.Add the heavy rare earth elements such as Dy, Tb, form the RE of high anisotropy field
2fe
14b compound replaces Nd
2fe
14b is that improving magnet HCJ the most direct is also the most frequently used method.But, the neodymium iron boron product of current commercialization, heavy rare earth adopts traditional melting addition manner, heavy rare earth addition up to 5-10wt.% not only substantially increases the production cost of magnet, consume valuable heavy rare earth resource, and the heavy rare earth element indexs such as can making the remanent magnetism of magnet and maximum magnetic energy product that is coupled with the antiferromagnetism of Fe declines rapidly.Therefore, under the condition of low heavy rare earth addition, realizing coercitive significantly lifting of magnet becomes extremely urgent key subject, and magnetic material worker has carried out a large amount of correlative studys.With TDK, Hitachi, enterprise and the Osaka University such as SHIN-ETSU HANTOTAI's chemical industry, University of tsukuba, the R&D institutions such as Kyoto University are that main research staff has carried out and carries out magnetic hardening to improve forming core field, reverse farmland thus to promote the coercitive research of magnet to main phase grain boundary layer, mainly by sputtering, vapour deposition, the means such as slurry coating form rich Dy in magnet surface, the metal of Tb or fluoride, oxide surface layer, then Dy is made by long high-temperature heat treatment, Tb is expanded by crystal boundary and oozes in magnet, and the shell structurre of rich heavy rare earth is formed on main phase grain border, increase the forming core field, reverse farmland of grain boundary layer, thus coercive force is improved while maintenance remanent magnetism.Obtain same coercive force improvement value by this grain boundary decision method, required heavy rare earth content is only about 1/3 of traditional adding method.At home, the unit such as Zhejiang University, Shanghai Communications University, University of Science & Technology, Beijing, Beijing University of Technology has also carried out NdF
3, DyF
3, the doping such as Dy nano particle improves coercitive research.But the technology expanding strengthening grain boundary layers such as oozing has considerable restraint to magnet thickness, is only applicable to the magnet of less than several millimeters thickness, and complex process, and long high temperature diffusion annealing more significantly increases energy consumption and production cost.Therefore, the method is only applicable to the magnet of a small amount of special purpose, is difficult to realize large-scale industrialization and produces and application.
Coercive force is the magnetic parameter of pair of magnets microstructure sensitivity, and large quantity research characterizes: undesirable microstructure formula causes the actual coercive force of magnet well below the major reason of its theoretical value.It is generally acknowledged: the rich Nd Grain-Boundary Phase thin layer that a layer thickness is about 2-4nm surrounds Nd
2fe
14b main phase grain, makes there is not magnetic exchange coupling effect between the crystal grain that isolates toward each other; The Nd contacted with rich-Nd phase thin layer
2fe
14, there is not epitaxial loayer in the composition of B grain surface layer and structure and intra-die uniformity; Nd
2fe
14b crystal grain is tiny, be evenly distributed, regular shape almost spherical, and grain orientation height is consistent and chemical composition is consistent with even structure.Under traditional handicraft, rich neodymium Grain-Boundary Phase is self-assembling formation, is difficult to realize effective regulation and control.But the appearance of pairing gold process and development enable us to carry out artificial design and synthesis to Grain-Boundary Phase, improve the physicochemical property of Grain-Boundary Phase, control its tissue and distribution, thus provide a kind of huge possibility for realizing above-mentioned ideal structure.
In recent years, this seminar utilizes pairing gold process can carry out the feature of Composition Design and preparation respectively to principal phase and Grain-Boundary Phase, for the institutional framework root realizing the lifting of neodymium iron boron coercive force, " crystal boundary reconstruct " ideamonger is proposed, engineer and the new Grain-Boundary Phase synthesizing rich heavy rare earth element, in magnet sintering and tempering heat treatment process, realize magnetic hardening by heavy rare earth element to the diffusion in main phase grain boundary layer, thus prepare low cost high-coercivity magnet do not add or add less the condition of heavy rare earth in principal phase under.This method is neither subject to the restriction of magnet size and shape, eliminates again and expands the long-time high temperature diffusion annealing needed for technology such as oozing, increases production process and energy consumption hardly.Simultaneously, nanometer powder is added in new Grain-Boundary Phase, by distribution and the grain boundary form of nano modification technical optimization Grain-Boundary Phase, pinning domain wall suppresses counter magnetic field forming core to promote coercive force, grain growth in effective suppression sintering process promotes comprehensive magnetic energy, thus realizes the high-coercive force high stability of neodymium iron boron magnetic body.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of high-coercive force high-stability neodymium iron boron magnet based on crystal boundary reconstruct and preparation method are provided.
High-coercive force high-stability neodymium iron boron magnet based on crystal boundary reconstruct is: be calculated in mass percent comprise 90 ~ 97% master alloying and 3 ~ 10% through the crystal-boundary phase alloy of nano-powder, the crystal-boundary phase alloy wherein through nano-powder comprises 90 ~ 99.999% crystal-boundary phase alloy and 0.001 ~ 10% nano powder.
Master alloying is in atomic percentage, and its composition is (Nd
arE
1-a)
xfe
100-x-y-zm
yb
z, Nd is neodymium element, and RE is rare earth element in other group of the lanthanides except Nd or Sc, Y; Fe is ferro element, and M is one or more in Nb, V, Ti, Co, Cr, Mo, Mn, Ni, Ga, Zr, Ta, Ag, Au, Al, Pb, Cu, Si element, and B is boron element; A, x, y, z meet following relation: 0.9≤a≤1,12≤x≤16,0≤y≤1.5,5.5≤z≤6.5.
Crystal-boundary phase alloy is in atomic percentage, and its composition is R
100-um'
ur is one or more in Gd, Tb, Dy, Ho, Er, and M' is one or more in Fe, Nb, V, Ti, Co, Cr, Mo, Mn, Ni, Zr, Ta, Ag, Au, Pb, Si, Ca, W, B, Mg, Cu, Al, Zn, Ga, Bi, Sn, In element; U meets: 0<u<100.
Described nano powder is: nano metal powder, nano-oxide powder, nano nitride powder or nano-carbide powder, wherein, nano metal powder is: Cu and alloy, Zn and alloy thereof, Ti and alloy, Mg alloy or Ni alloy, nano-oxide powder is: SiO
2, Dy
2o
3, ZnO, MgO, CuO, Fe
2o
3, Al
2o
3, Y
2o
3or TiO
2, nano nitride powder is AlN, TiN, ZrN or Si
3n
4, nano-carbide powder is TiC, SiC, Fe
3c, NbC, ZrC, WC or VC, the average particulate diameter of nanometer powder is 1 ~ 100nm.
Preparation method based on the high-coercive force high-stability neodymium iron boron magnet of crystal boundary reconstruct is: the rich new Grain-Boundary Phase of heavy rare earth of Application of composite and nano modification method, namely the new Grain-Boundary Phase with the rich heavy rare earth of synthesis is redesigned, in magnet sintering and temper process, realize magnetic hardening by heavy rare earth element to the diffusion in main phase grain boundary layer, do not add or add less the condition of heavy rare earth in principal phase under, prepare low cost high-coercivity magnet; In new Grain-Boundary Phase, add nanometer powder simultaneously, distribution and the grain boundary form of Grain-Boundary Phase is optimized by nano modification method, pinning domain wall suppresses counter magnetic field forming core to promote coercive force, grain growth in effective suppression sintering process promotes comprehensive magnetic energy, thus realizes the high-coercive force high stability of neodymium iron boron magnetic body.
Concrete steps based on the preparation method of the high-coercive force high-stability neodymium iron boron magnet of crystal boundary reconstruct are:
1) adopted by master alloying the quick-fried and airflow milling three kinds of techniques of rapid hardening slab, hydrogen to prepare the master alloying powder that average particulate diameter is 3 ~ 10 μm, described master alloying is in atomic percentage, and its composition is (Nd
arE
1-a)
xfe
100-x-y-zm
yb
z;
2) crystal-boundary phase alloy adopted casting technique to make ingot casting or adopt rapid hardening slab technique to make rapid hardening thin slice or adopt rapid quenching technique to make rapid tempering belt, and adopt airflow milling or mechanical ball grinding process to prepare crystal-boundary phase alloy powder that average particulate diameter is 1 ~ 10 μm, described crystal-boundary phase alloy is in atomic percentage, and its composition is R
100-um'
u, R is one or more in Gd, Tb, Dy, Ho, Er;
3) crystal-boundary phase alloy powder is mixed under aviation gasoline or benzinum protective medium with the nano powder of interpolation in batch mixer, obtain the crystal-boundary phase alloy powder through nano-powder, wherein, the nano powder weight of interpolation accounts for 0.001 ~ 10% of total powder weight;
4) mix in batch mixer under aviation gasoline or benzinum protective medium by master alloying powder with through the crystal-boundary phase alloy powder of nano-powder, obtain mixed-powder, wherein, the crystal-boundary phase alloy powder weight through nano-powder accounts for 3 ~ 10% of total powder weight;
5) mixed-powder orientation die mould under the magnetic field of 1.5 ~ 3T, and be pressed into green compact through the isostatic cool pressing of 17MPa;
6) adopt high vacuum positive pressure sintering furnace that green compact are sintered 2 ~ 5h at 1050 ~ 1125 DEG C, between 880 ~ 950 DEG C, carry out one-level tempering, then carry out second annealing between 480 ~ 650 DEG C, obtain neodymium iron boron magnetic body.
The beneficial effect that the present invention compared with prior art has: 1) the present invention is based on crystal boundary reconstruct new technology, design initiatively and regulation and control can be carried out to Grain-Boundary Phase composition, prepare new Grain-Boundary Phase and substitute traditional rich neodymium phase, improve tissue and the distribution of Grain-Boundary Phase, improve its physicochemical property; 2) the rich new Grain-Boundary Phase of heavy rare earth of Application of composite of the present invention and nano modification technology, namely the new Grain-Boundary Phase with the rich heavy rare earth of synthesis is redesigned, in magnet sintering and temper process, realize magnetic hardening by heavy rare earth element to the diffusion in main phase grain boundary layer, thus prepare low cost high-coercivity magnet do not add or add less the condition of heavy rare earth in principal phase under; In new Grain-Boundary Phase, add nanometer powder simultaneously, by distribution and the grain boundary form of nano modification technical optimization Grain-Boundary Phase, pinning domain wall suppresses counter magnetic field forming core to promote coercive force, grain growth in effective suppression sintering process promotes comprehensive magnetic energy, thus realizes the high-coercive force high stability of neodymium iron boron magnetic body; 3) the present invention realizes the diffusion of heavy rare earth element in main phase grain boundary layer, simultaneously, the high potential nano-powder particles of adding has large specific area, comparatively easily realize being uniformly distributed, the electrochemistry that can reduce between Grain-Boundary Phase and principal phase is poor, reduce the motive power of electrochemical corrosion course, thus promote intrinsic corrosion stability; 4) nanometer powder that the present invention adds has high reactivity, is conducive to the sintering densification of magnet; Meanwhile, nano powder is evenly distributed on the surface of the Grain-Boundary Phase powder through airflow milling, effectively can improve the physicochemical property of Grain-Boundary Phase, realize being uniformly distributed of nano modification Grain-Boundary Phase; These are conducive to the raising of magnet density, and therefore magnet provided by the invention can improve remanent magnetism to a certain extent
b rwith maximum magnetic energy product (
bH)
max; 5) preparation method's technique provided by the invention is simple, and cost is lower, is applicable to large-scale mass production.
Embodiment
High-coercive force high-stability neodymium iron boron magnet based on crystal boundary reconstruct is: be calculated in mass percent comprise 90 ~ 97% master alloying and 3 ~ 10% through the crystal-boundary phase alloy of nano-powder, the crystal-boundary phase alloy wherein through nano-powder comprises 90 ~ 99.999% crystal-boundary phase alloy and 0.001 ~ 10% nano powder.
Master alloying is in atomic percentage, and its composition is (Nd
arE
1-a)
xfe
100-x-y-zm
yb
z, Nd is neodymium element, and RE is rare earth element in other group of the lanthanides except Nd or Sc, Y; Fe is ferro element, and M is one or more in Nb, V, Ti, Co, Cr, Mo, Mn, Ni, Ga, Zr, Ta, Ag, Au, Al, Pb, Cu, Si element, and B is boron element; A, x, y, z meet following relation: 0.9≤a≤1,12≤x≤16,0≤y≤1.5,5.5≤z≤6.5.
Crystal-boundary phase alloy is in atomic percentage, and its composition is R
100-um'
ur is one or more in Gd, Tb, Dy, Ho, Er, and M' is one or more in Fe, Nb, V, Ti, Co, Cr, Mo, Mn, Ni, Zr, Ta, Ag, Au, Pb, Si, Ca, W, B, Mg, Cu, Al, Zn, Ga, Bi, Sn, In element; U meets: 0<u<100.
Described nano powder is: nano metal powder, nano-oxide powder, nano nitride powder or nano-carbide powder, wherein, nano metal powder is: Cu and alloy, Zn and alloy thereof, Ti and alloy, Mg alloy or Ni alloy, nano-oxide powder is: SiO
2, Dy
2o
3, ZnO, MgO, CuO, Fe
2o
3, Al
2o
3, Y
2o
3or TiO
2, nano nitride powder is AlN, TiN, ZrN or Si
3n
4, nano-carbide powder is TiC, SiC, Fe
3c, NbC, ZrC, WC or VC, the average particulate diameter of nanometer powder is 1 ~ 100nm.
Preparation method based on the high-coercive force high-stability neodymium iron boron magnet of crystal boundary reconstruct is: the rich new Grain-Boundary Phase of heavy rare earth of Application of composite and nano modification method, namely the new Grain-Boundary Phase with the rich heavy rare earth of synthesis is redesigned, in magnet sintering and temper process, realize magnetic hardening by heavy rare earth element to the diffusion in main phase grain boundary layer, do not add or add less the condition of heavy rare earth in principal phase under, prepare low cost high-coercivity magnet; In new Grain-Boundary Phase, add nanometer powder simultaneously, distribution and the grain boundary form of Grain-Boundary Phase is optimized by nano modification method, pinning domain wall suppresses counter magnetic field forming core to promote coercive force, grain growth in effective suppression sintering process promotes comprehensive magnetic energy, thus realizes the high-coercive force high stability of neodymium iron boron magnetic body.
Concrete steps based on the preparation method of the high-coercive force high-stability neodymium iron boron magnet of crystal boundary reconstruct are:
1) adopted by master alloying the quick-fried and airflow milling three kinds of techniques of rapid hardening slab, hydrogen to prepare the master alloying powder that average particulate diameter is 3 ~ 10 μm, described master alloying is in atomic percentage, and its composition is (Nd
arE
1-a)
xfe
100-x-y-zm
yb
z;
2) crystal-boundary phase alloy adopted casting technique to make ingot casting or adopt rapid hardening slab technique to make rapid hardening thin slice or adopt rapid quenching technique to make rapid tempering belt, and adopt airflow milling or mechanical ball grinding process to prepare crystal-boundary phase alloy powder that average particulate diameter is 1 ~ 10 μm, described crystal-boundary phase alloy is in atomic percentage, and its composition is R
100-um'
u, R is one or more in Gd, Tb, Dy, Ho, Er;
3) crystal-boundary phase alloy powder is mixed under aviation gasoline or benzinum protective medium with the nano powder of interpolation in batch mixer, obtain the crystal-boundary phase alloy powder through nano-powder, wherein, the nano powder weight of interpolation accounts for 0.001 ~ 10% of total powder weight;
4) mix in batch mixer under aviation gasoline or benzinum protective medium by master alloying powder with through the crystal-boundary phase alloy powder of nano-powder, obtain mixed-powder, wherein, the crystal-boundary phase alloy powder weight through nano-powder accounts for 3 ~ 10% of total powder weight;
5) mixed-powder orientation die mould under the magnetic field of 1.5 ~ 3T, and be pressed into green compact through the isostatic cool pressing of 17MPa;
6) adopt high vacuum positive pressure sintering furnace that green compact are sintered 2 ~ 5h at 1050 ~ 1125 DEG C, between 880 ~ 950 DEG C, carry out one-level tempering, then carry out second annealing between 480 ~ 650 DEG C, obtain neodymium iron boron magnetic body.
Below in conjunction with instantiation, the present invention will be further described, but the present invention is not limited only to following examples.
Embodiment 1:
1) adopted by master alloying the quick-fried and airflow milling three kinds of techniques of rapid hardening slab, hydrogen to prepare master alloying powder, described master alloying is in atomic percentage, and its composition is Nd
12.6fe
81.3b
6.1;
2) adopt casting technique to make ingot casting crystal-boundary phase alloy, and adopt mechanical ball grinding process to prepare crystal-boundary phase alloy powder, described crystal-boundary phase alloy is in atomic percentage, and its composition is Dy
71.5fe
28.5;
3) crystal-boundary phase alloy powder is mixed under aviation gasoline protective medium with the nano-oxide CuO powder of interpolation in batch mixer, obtain the crystal-boundary phase alloy powder through nano-powder, wherein, the nano-oxide CuO powder average particulate diameter added is about 55nm, accounts for 0.05% of total powder weight;
4) mix in batch mixer under aviation gasoline protective medium by master alloying powder with through the crystal-boundary phase alloy powder of nano-powder, obtain mixed-powder, wherein, the crystal-boundary phase alloy powder weight through nano-powder accounts for 6% of total powder weight;
5) mixed-powder orientation die mould under the magnetic field of 3T, and be pressed into green compact through the isostatic cool pressing of 17MPa;
6) adopt high vacuum positive pressure sintering furnace by green compact at 1080 DEG C of sintering 4h, carry out one-level tempering at 880 DEG C, then carry out second annealing at 520 DEG C and obtain neodymium iron boron magnetic body;
The magnet prepared is put into VSM and measures its magnetic property, result is as follows:
b r=1.45T,
h cj=2316kA/m, (
bH)
max=438kJ/m
3, magnet maximum operating temperature reaches 240 DEG C.
Embodiment 2:
1) adopted by master alloying the quick-fried and airflow milling three kinds of techniques of rapid hardening slab, hydrogen to prepare master alloying powder, described master alloying is in atomic percentage, and its composition is Nd
13.18fe
80.81al
0.24nb
0.07b
5.70;
2) crystal-boundary phase alloy adopted rapid hardening slab technique to make rapid hardening thin slice, and adopt mechanical ball grinding process to prepare crystal-boundary phase alloy powder, described crystal-boundary phase alloy is in atomic percentage, and its composition is Dy
32.50fe
62.00cu
5.50;
3) by the nano-oxide SiO of crystal-boundary phase alloy powder and interpolation
2powder mixes under benzinum protective medium in batch mixer, obtains the crystal-boundary phase alloy powder through nano-powder, wherein, and the nano-oxide SiO of interpolation
2powder average particulate diameter is about 20nm, accounts for 0.001% of total powder weight;
4) mix in batch mixer under benzinum protective medium by master alloying powder with through the crystal-boundary phase alloy powder of nano-powder, obtain mixed-powder, wherein, the crystal-boundary phase alloy powder weight through nano-powder accounts for 4% of total powder weight;
5) mixed-powder orientation die mould under the magnetic field of 1.5T, and be pressed into green compact through the isostatic cool pressing of 17MPa;
6) adopt high vacuum positive pressure sintering furnace that green compact are sintered 4h at 1084 DEG C, carry out one-level tempering at 900 DEG C, then carry out second annealing at 630 DEG C, obtain neodymium iron boron magnetic body;
The magnet prepared is put into VSM and measures its magnetic property, result is as follows:
b r=1.37T,
h cj=2146kA/m, (
bH)
max=358kJ/m
3, magnet maximum operating temperature reaches 240 DEG C.
Embodiment 3:
1) adopted by master alloying the quick-fried and airflow milling three kinds of techniques of rapid hardening slab, hydrogen to prepare master alloying powder, described master alloying is in atomic percentage, and its composition is (Nd
0.9pr
0.1)
16fe
76al
0.2co
0.3ga
0.8si
0.15zr
0.05b
6.5;
2) adopt rapid quenching technique to make rapid tempering belt crystal-boundary phase alloy, and adopt airflow milling technique to prepare crystal-boundary phase alloy powder, described crystal-boundary phase alloy is in atomic percentage, and its composition is Tb
72fe
28;
3) by the nano-oxide Dy of crystal-boundary phase alloy powder and interpolation
2o
3powder mixes under benzinum protective medium in batch mixer, obtains the crystal-boundary phase alloy powder through nano-powder, wherein, and the nano-oxide Dy of interpolation
2o
3powder average particulate diameter is about 40nm, accounts for 10% of total powder weight;
4) mix in batch mixer under benzinum protective medium by master alloying powder with through the crystal-boundary phase alloy powder of nano-powder, obtain mixed-powder, wherein, the crystal-boundary phase alloy powder weight through nano-powder accounts for 3% of total powder weight;
5) mixed-powder orientation die mould under the magnetic field of 2T, and be pressed into green compact through the isostatic cool pressing of 17MPa;
6) adopt high vacuum positive pressure sintering furnace that green compact are sintered 5h at 1050 DEG C, carry out one-level tempering at 950 DEG C, then carry out second annealing at 650 DEG C, obtain neodymium iron boron magnetic body;
The magnet prepared is put into VSM and measures its magnetic property, result is as follows:
b r=1.30T,
h cj=2900kA/m, (
bH)
max=368kJ/m
3, magnet maximum operating temperature reaches 250 DEG C.
Embodiment 4:
1) adopted by master alloying the quick-fried and airflow milling three kinds of techniques of rapid hardening slab, hydrogen to prepare master alloying powder, described master alloying is in atomic percentage, and its composition is Nd
12fe
81.6al
0.2ga
0.6zn
0.1b
5.5;
2) adopt casting technique to make ingot casting crystal-boundary phase alloy, and adopt mechanical ball grinding process to prepare crystal-boundary phase alloy powder, described crystal-boundary phase alloy is in atomic percentage, and its composition is Gd
70cu
30;
3) crystal-boundary phase alloy powder is mixed under aviation gasoline protective medium with the nano metal Cu powder of interpolation in batch mixer, obtain the crystal-boundary phase alloy powder through nano-powder, wherein, the nano metal Cu powder average particulate diameter of interpolation is about 48nm, accounts for 0.02% of total powder weight;
4) mix in batch mixer under aviation gasoline protective medium by master alloying powder with through the crystal-boundary phase alloy powder of nano-powder, obtain mixed-powder, wherein, the crystal-boundary phase alloy powder weight through nano-powder accounts for 10% of total powder weight;
5) mixed-powder orientation die mould under the magnetic field of 2T, and be pressed into green compact through the isostatic cool pressing of 17MPa;
6) adopt high vacuum positive pressure sintering furnace that green compact are sintered 2h at 1125 DEG C, carry out one-level tempering at 880 DEG C, then carry out second annealing at 650 DEG C, obtain neodymium iron boron magnetic body.
The magnet prepared is put into VSM and measures its magnetic property, result is as follows:
b r=1.35T,
h cj=1956kA/m, (
bH)
max=322kJ/m
3, magnet maximum operating temperature reaches 250 DEG C.
Claims (3)
1. the high-coercive force high-stability neodymium iron boron magnet based on crystal boundary reconstruct, it is characterized in that being calculated in mass percent comprise 90 ~ 97% master alloying and 3 ~ 10% through the crystal-boundary phase alloy of nano-powder, the crystal-boundary phase alloy wherein through nano-powder comprises 90 ~ 99.999% crystal-boundary phase alloy and 0.001 ~ 10% nano powder; Described nano powder is: nano metal powder, nano-oxide powder, nano nitride powder or nano-carbide powder, wherein, nano metal powder is: Cu and alloy, Zn and alloy thereof, Ti and alloy, Mg alloy or Ni alloy, nano-oxide powder is: SiO
2, Dy
2o
3, ZnO, MgO, CuO, Fe
2o
3, Al
2o
3, Y
2o
3or TiO
2, nano nitride powder is AlN, TiN, ZrN or Si
3n
4, nano-carbide powder is TiC, SiC, Fe
3c, NbC, ZrC, WC or VC, the average particulate diameter of nanometer powder is 1 ~ 100nm;
Master alloying is in atomic percentage, and its composition is (Nd
arE
1-a)
xfe
100-x-y-zm
yb
z, Nd is neodymium element, and RE is rare earth element in other group of the lanthanides except Nd or Sc, Y; Fe is ferro element, and M is one or more in Nb, V, Ti, Co, Cr, Mo, Mn, Ni, Ga, Zr, Ta, Ag, Au, Al, Pb, Cu, Si element, and B is boron element; A, x, y, z meet following relation: 0.9≤a≤1,12≤x≤16,0≤y≤1.5,5.5≤z≤6.5;
Crystal-boundary phase alloy is in atomic percentage, and its composition is R
100-um'
ur is one or more in Gd, Tb, Dy, Ho, Er, and M' is one or more in Fe, Nb, V, Ti, Co, Cr, Mo, Mn, Ni, Zr, Ta, Ag, Au, Pb, Si, Ca, W, B, Mg, Cu, Al, Zn, Ga, Bi, Sn, In element; U meets: 0<u<100.
2. the preparation method of the high-coercive force high-stability neodymium iron boron magnet based on crystal boundary reconstruct as claimed in claim 1, it is characterized in that: the rich new Grain-Boundary Phase of heavy rare earth of Application of composite and nano modification technology, namely the new Grain-Boundary Phase with the rich heavy rare earth of synthesis is redesigned, in magnet sintering and temper process, realize magnetic hardening by heavy rare earth element to the diffusion in main phase grain boundary layer, do not add or add less the condition of heavy rare earth in principal phase under, prepare low cost high-coercivity magnet; In new Grain-Boundary Phase, add nanometer powder simultaneously, distribution and the grain boundary form of Grain-Boundary Phase is optimized by nano modification method, pinning domain wall suppresses counter magnetic field forming core to promote coercive force, grain growth in effective suppression sintering process promotes comprehensive magnetic energy, thus realizes the high-coercive force high stability of neodymium iron boron magnetic body.
3. the preparation method of a kind of high-coercive force high-stability neodymium iron boron magnet based on crystal boundary reconstruct according to claim 2, is characterized in that its concrete steps are:
1) adopted by master alloying the quick-fried and airflow milling three kinds of techniques of rapid hardening slab, hydrogen to prepare the master alloying powder that average particulate diameter is 3 ~ 10 μm, described master alloying is in atomic percentage, and its composition is (Nd
arE
1-a)
xfe
100-x-y-zm
yb
z;
2) crystal-boundary phase alloy adopted casting technique to make ingot casting or adopt rapid hardening slab technique to make rapid hardening thin slice or adopt rapid quenching technique to make rapid tempering belt, and adopt airflow milling or mechanical ball grinding process to prepare crystal-boundary phase alloy powder that average particulate diameter is 1 ~ 10 μm, described crystal-boundary phase alloy is in atomic percentage, and its composition is R
100-um'
u, R is one or more in Gd, Tb, Dy, Ho, Er;
3) crystal-boundary phase alloy powder is mixed under aviation gasoline or benzinum protective medium with the nano powder of interpolation in batch mixer, obtain the crystal-boundary phase alloy powder through nano-powder, wherein, the nano powder weight of interpolation accounts for 0.001 ~ 10% of total powder weight;
4) mix in batch mixer under aviation gasoline or benzinum protective medium by master alloying powder with through the crystal-boundary phase alloy powder of nano-powder, obtain mixed-powder, wherein, the crystal-boundary phase alloy powder weight through nano-powder accounts for 3 ~ 10% of total powder weight;
5) mixed-powder orientation die mould under the magnetic field of 1.5 ~ 3T, and be pressed into green compact through the isostatic cool pressing of 17MPa;
6) adopt high vacuum positive pressure sintering furnace that green compact are sintered 2 ~ 5h at 1050 ~ 1125 DEG C, carry out one-level tempering at 880 ~ 950 DEG C, then carry out second annealing at 480 ~ 650 DEG C, obtain neodymium iron boron magnetic body.
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