CN103106991A - High-coercivity and high-stability neodymium iron boron magnet and preparation method based on crystal boundary reconstruction - Google Patents
High-coercivity and high-stability neodymium iron boron magnet and preparation method based on crystal boundary reconstruction Download PDFInfo
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Abstract
The invention discloses a high-coercivity and high-stability neodymium iron boron magnet and a preparation method based on crystal boundary reconstruction. The preparation method comprises the steps of separating design and preparation of main alloy and crystal boundary phase alloy powder, nano-modification of crystal boundary phase, powder mixing, magnetic field profiling, isostatic pressing, sintering and thermal treatment. According to the high-coercivity and high-stability neodymium iron boron magnet and the preparation method is based on crystal boundary reconstruction and combines with a rich heavy rear earth novel crystal boundary phase and nano-modification technology, namely the rich heavy rare earth novel crystal boundary phase is redesigned and synthesized, in the process of magnetic sintering and tempering, magnetic hardening is achieved through spread of the heavy rare earth element to the boundary layers of the principle phase crystal grain, and thus a high-coercivity magnetic is prepared under the condition that no or less heavy rear earth is added in the principle phase. Meanwhile the distribution of the crystal boundary and the form of the crystal grain boundary are optimized through a nano-modification method, a pinning domain wall restrains counter magnetic field nucleation and crystal grain growth, and thus high coercivity and high stability of the neodymium iron boron is achieved. The high-coercivity and high-stability neodymium iron boron magnet and preparation method based on crystal boundary reconstruction is simple in process, low in cost and suitable for large-scale volume production.
Description
Technical field
The present invention relates to a kind of high-coercive force high stability neodymium iron boron magnetic body and preparation method based on crystal boundary reconstruct.
Background technology
Nd-Fe-B has the incomparable advantages of other types permanent magnetic material such as high energy product, high performance-price ratio, is present most widely used rare earth permanent-magnetic material.By 2015, the world demand amount of neodymium iron boron product will be up to 200,000 tons, and as seen in the long time in future, NdFeB material still can be taken on important role in the modern information technologies industry.
The key technical indexes of weighing the Nd-Fe-B permanent magnetic performance comprises remanent magnetism
B r, maximum magnetic energy product (
BH)
max, coercive force
H cAnd Curie temperature
T cThrough effort for many years, based on comparatively ripe design of alloy theory and optimum preparation condition,
B rReach 1.555T, be more than 96% of theoretical value; (
BH)
maxReach 474kJ/m3, be more than 92% of theoretical value.And
H cAlthough realized certain lifting, but still only be 1/10 ~ 1/3 of theoretical value, make the temperature stability of magnet relatively poor, greatly limited the application of magnet in fields such as precision instrumentation, Aero-Space.Therefore, improve the neodymium iron boron coercive force, the temperature stability that promotes magnet is the key that further enlarges range of application, is to need a difficult problem of capturing badly.
Add the 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 be very not 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
14The B compound replaces Nd
2Fe
14B is that improving the magnet HCJ the most direct is also the most frequently used method.But, present commercial neodymium iron boron product, heavy rare earth adopts traditional melting addition manner, heavy rare earth addition up to 5-10wt.% has not only greatly increased the production cost of magnet, consumed valuable heavy rare earth resource, and the antiferromagnetism coupling of heavy rare earth element and Fe can make the indexs such as the remanent magnetism of magnet and maximum magnetic energy product descend rapidly.Therefore, under the condition of low heavy rare earth addition, realize that coercitive significantly lifting of magnet becomes extremely urgent key subject, the magnetic material worker has carried out a large amount of correlative studys.with TDK, Hitachi, enterprise and Osaka universities such as SHIN-ETSU HANTOTAI's chemical industry, University of tsukuba, thereby the R﹠D institutions such as Kyoto University are main research staff to have carried out and magnetic hardening is carried out in the main phase grain boundary layer promotes the coercitive research of magnet to improve forming core field, reverse farmland, mainly by sputter, vapour deposition, the means such as slurry coating form rich Dy in magnet surface, the metal of Tb or fluoride, oxide surface layer, then make Dy by long high-temperature heat treatment, Tb expands in the magnet by crystal boundary and oozes, and form the shell structurre of rich heavy rare earth on the main phase grain border, increase the forming core field, reverse farmland of grain boundary layer, thereby improve coercive force when keeping remanent magnetism.Obtain same coercive force improvement value with this crystal boundary diffusion method, needed heavy rare earth content is only 1/3 left and right of traditional adding method.At home, the units such as Zhejiang University, Shanghai Communications University, University of Science ﹠ Technology, Beijing, Beijing University of Technology have also carried out NdF
3, DyF
3, the doping such as Dy nano particle improves coercitive research.But, expand to ooze and wait the technology of reinforcement grain boundary layer to magnet thickness, considerable restraint to be arranged, be only applicable to the magnet of thickness below several millimeters, and complex process, long high temperature diffusion annealing has significantly increased 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 production 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: a layer thickness approximately rich Nd Grain-Boundary Phase thin layer of 2-4nm is surrounded Nd
2Fe
14The B main phase grain makes isolated toward each other intergranule not have the magnetic exchange-coupling interaction; With the contacted Nd of rich Nd phase thin layer
2Fe
14There is not epitaxial loayer in the inner uniformity of the composition of B grain surface layer and structure and crystal grain; Nd
2Fe
14B crystal grain is tiny, be evenly distributed, the regular shape almost spherical, and the 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 effectively regulation and control.But the appearance of pairing gold process and development make us carry out artificial design and synthetic to Grain-Boundary Phase, improve the physicochemical property of Grain-Boundary Phase, control its tissue and distribution, thereby for realizing that above-mentioned ideal structure provides a kind of huge possibility.
In recent years, this seminar utilizes the pairing gold process to carry out respectively the characteristics of Composition Design and preparation to principal phase and Grain-Boundary Phase, for the institutional framework root that realizes that the neodymium iron boron coercive force promotes, " crystal boundary reconstruct " ideamonger is proposed, artificial design and the new Grain-Boundary Phase that synthesizes rich heavy rare earth element, realize magnetic hardening by heavy rare earth element to the diffusion in main phase grain boundary layer in magnet sintering and tempering heat treatment process, thereby do not add or add less the low-cost high-coercive force magnet of preparation under the condition of heavy rare earth in principal phase.This method neither is subjected to the restriction of magnet size and shape, has save again to expand the required long-time high temperature diffusion annealing of technology such as to ooze, and increases hardly production process and energy consumption.Simultaneously, add nanometer powder in new Grain-Boundary Phase, distribution and grain boundary form by nano modification technical optimization Grain-Boundary Phase, the pinning domain wall suppresses the counter magnetic field forming core and promotes coercive force, the grain growth that effectively suppresses in sintering process promotes the comprehensive magnetic energy, thereby realizes the high-coercive force high stability of neodymium iron boron magnetic body.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of high-coercive force high stability neodymium iron boron magnetic body and preparation method based on crystal boundary reconstruct is provided.
High-coercive force high stability neodymium iron boron magnetic body based on crystal boundary reconstruct is: be calculated in mass percent and comprise 90 ~ 97% master alloying and 3 ~ 10% crystal-boundary phase alloy through nano-powders, wherein the crystal-boundary phase alloy 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, RE is rare earth element or Sc, the Y in other group of the lanthanides except Nd; 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 satisfy 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 satisfies: 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 thereof, Zn and alloy thereof, Ti and alloy thereof, 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, the nano nitride powder is AlN, TiN, ZrN or Si
3N
4, the nano-carbide powder is TiC, SiC, Fe
3C, NbC, ZrC, WC or VC, the average particulate diameter of nanometer powder are 1 ~ 100nm.
Preparation method based on the high-coercive force high stability neodymium iron boron magnetic body of crystal boundary reconstruct is: the rich new Grain-Boundary Phase of heavy rare earth of Application of composite and nano modification method, i.e. redesign and the new Grain-Boundary Phase that synthesizes rich heavy rare earth, realize magnetic hardening by heavy rare earth element to the diffusion in main phase grain boundary layer in magnet sintering and temper process, do not add or add less the low-cost high-coercive force magnet of preparation under the condition of heavy rare earth in principal phase; Add nanometer powder simultaneously in new Grain-Boundary Phase, optimize distribution and the grain boundary form of Grain-Boundary Phase by the nano modification method, the pinning domain wall suppresses the counter magnetic field forming core and promotes coercive force, the grain growth that effectively suppresses in sintering process promotes the comprehensive magnetic energy, thereby 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 magnetic body of crystal boundary reconstruct are:
1) master alloying is adopted the rapid hardening slab, hydrogen is quick-fried and three kinds of techniques of airflow milling prepare the master alloying powder that average particulate diameter is 3 ~ 10 μ m, described master alloying is in atomic percentage, its composition is (Nd
aRE
1-a)
xFe
100-x-y-zM
yB
z
2) crystal-boundary phase alloy is adopted casting technique make ingot casting or adopt rapid hardening slab technique to make the 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 the crystal-boundary phase alloy powder that average particulate diameter is 1 ~ 10 μ m, 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) nano powder with crystal-boundary phase alloy powder and interpolation mixes in batch mixer under aviation gasoline or benzinum protective medium, 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) the crystal-boundary phase alloy powder with master alloying powder and process nano-powder mixes in batch mixer under aviation gasoline or benzinum protective medium, 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 is orientated die mould under the magnetic field of 1.5 ~ 3T, and is pressed into green compact through the isostatic cool pressing of 17MPa;
6) employing high vacuum positive pressure sintering furnace at 1050 ~ 1125 ℃ of sintering 2 ~ 5h, carries out green compact the one-level tempering, then carry out second annealing between 480 ~ 650 ℃ between 880 ~ 950 ℃, obtains 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, can carry out design and regulation and control initiatively to the 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, i.e. redesign and the new Grain-Boundary Phase that synthesizes rich heavy rare earth, realize magnetic hardening by heavy rare earth element to the diffusion in main phase grain boundary layer in magnet sintering and temper process, thereby do not add or add less the low-cost high-coercive force magnet of preparation under the condition of heavy rare earth in principal phase; Add nanometer powder simultaneously in new Grain-Boundary Phase, distribution and grain boundary form by nano modification technical optimization Grain-Boundary Phase, the pinning domain wall suppresses the counter magnetic field forming core and promotes coercive force, the grain growth that effectively suppresses in sintering process promotes the comprehensive magnetic energy, thereby realizes the high-coercive force high stability of neodymium iron boron magnetic body; 3) the present invention realizes that heavy rare earth element is in the diffusion in main phase grain boundary layer, simultaneously, the high potential nano-powder particles of adding has large specific area, easily realize evenly distributing, the electrochemistry that can dwindle between Grain-Boundary Phase and principal phase is poor, reduce the motive power of electrochemical corrosion course, thereby promote the intrinsic corrosion stability; 4) nanometer powder of the present invention's interpolation has high reactivity, is conducive to the sintering densification of magnet; Simultaneously, nano powder is evenly distributed on the surface through the Grain-Boundary Phase powder of airflow milling, can effectively improve the physicochemical property of Grain-Boundary Phase, realizes the even distribution 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 rAnd maximum magnetic energy product (
BH)
max5) preparation method's technique provided by the invention is simple, and cost is lower, is fit to large-scale mass production.
Embodiment
High-coercive force high stability neodymium iron boron magnetic body based on crystal boundary reconstruct is: be calculated in mass percent and comprise 90 ~ 97% master alloying and 3 ~ 10% crystal-boundary phase alloy through nano-powders, wherein the crystal-boundary phase alloy 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, RE is rare earth element or Sc, the Y in other group of the lanthanides except Nd; 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 satisfy 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 satisfies: 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 thereof, Zn and alloy thereof, Ti and alloy thereof, 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, the nano nitride powder is AlN, TiN, ZrN or Si
3N
4, the nano-carbide powder is TiC, SiC, Fe
3C, NbC, ZrC, WC or VC, the average particulate diameter of nanometer powder are 1 ~ 100nm.
Preparation method based on the high-coercive force high stability neodymium iron boron magnetic body of crystal boundary reconstruct is: the rich new Grain-Boundary Phase of heavy rare earth of Application of composite and nano modification method, i.e. redesign and the new Grain-Boundary Phase that synthesizes rich heavy rare earth, realize magnetic hardening by heavy rare earth element to the diffusion in main phase grain boundary layer in magnet sintering and temper process, do not add or add less the low-cost high-coercive force magnet of preparation under the condition of heavy rare earth in principal phase; Add nanometer powder simultaneously in new Grain-Boundary Phase, optimize distribution and the grain boundary form of Grain-Boundary Phase by the nano modification method, the pinning domain wall suppresses the counter magnetic field forming core and promotes coercive force, the grain growth that effectively suppresses in sintering process promotes the comprehensive magnetic energy, thereby 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 magnetic body of crystal boundary reconstruct are:
1) master alloying is adopted the rapid hardening slab, hydrogen is quick-fried and three kinds of techniques of airflow milling prepare the master alloying powder that average particulate diameter is 3 ~ 10 μ m, described master alloying is in atomic percentage, its composition is (Nd
aRE
1-a)
xFe
100-x-y-zM
yB
z
2) crystal-boundary phase alloy is adopted casting technique make ingot casting or adopt rapid hardening slab technique to make the 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 the crystal-boundary phase alloy powder that average particulate diameter is 1 ~ 10 μ m, 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) nano powder with crystal-boundary phase alloy powder and interpolation mixes in batch mixer under aviation gasoline or benzinum protective medium, 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) the crystal-boundary phase alloy powder with master alloying powder and process nano-powder mixes in batch mixer under aviation gasoline or benzinum protective medium, 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 is orientated die mould under the magnetic field of 1.5 ~ 3T, and is pressed into green compact through the isostatic cool pressing of 17MPa;
6) employing high vacuum positive pressure sintering furnace at 1050 ~ 1125 ℃ of sintering 2 ~ 5h, carries out green compact the one-level tempering, then carry out second annealing between 480 ~ 650 ℃ between 880 ~ 950 ℃, obtains neodymium iron boron magnetic body.
The present invention will be further described below in conjunction with instantiation, but the present invention is not limited only to following examples.
Embodiment 1:
1) master alloying is adopted the rapid hardening slab, hydrogen is quick-fried and three kinds of techniques of airflow milling prepare the master alloying powder, described master alloying is in atomic percentage, its composition is Nd
12.6Fe
81.3B
6.1
2) adopt casting technique to make ingot casting crystal-boundary phase alloy, and adopt the mechanical ball grinding process to prepare the crystal-boundary phase alloy powder, described crystal-boundary phase alloy is in atomic percentage, and its composition is Dy
71.5Fe
28.5
3) the nano-oxide CuO powder with crystal-boundary phase alloy powder and interpolation mixes in batch mixer under the aviation gasoline protective medium, obtain the crystal-boundary phase alloy powder through nano-powder, wherein, the nano-oxide CuO powder average particulate diameter that adds is about 55nm, accounts for 0.05% of total powder weight;
4) the crystal-boundary phase alloy powder with master alloying powder and process nano-powder mixes in batch mixer under the aviation gasoline protective medium, obtains mixed-powder, and wherein, the crystal-boundary phase alloy powder weight of process nano-powder accounts for 6% of total powder weight;
5) mixed-powder is orientated die mould under the magnetic field of 3T, and is pressed into green compact through the isostatic cool pressing of 17MPa;
6) adopt the high vacuum positive pressure sintering furnace with green compact at 1080 ℃ of sintering 4h, carry out the one-level tempering at 880 ℃, then carry out second annealing at 520 ℃ and obtain neodymium iron boron magnetic body;
The magnet for preparing is put into VSM measure its magnetic property, result is as follows:
B r=1.45T,
H cj=2316kA/m, (
BH)
max=438kJ/m
3, the magnet maximum operating temperature reaches 240 ℃.
Embodiment 2:
1) master alloying is adopted the rapid hardening slab, hydrogen is quick-fried and three kinds of techniques of airflow milling prepare the master alloying powder, described master alloying is in atomic percentage, its composition is Nd
13.18Fe
80.81Al
0.24Nb
0.07B
5.70
2) crystal-boundary phase alloy is adopted rapid hardening slab technique make the rapid hardening thin slice, and adopt the mechanical ball grinding process to prepare the 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) with the nano-oxide SiO of crystal-boundary phase alloy powder and interpolation
2Powder mixes in batch mixer under the benzinum protective medium, obtains the crystal-boundary phase alloy powder through nano-powder, wherein, and the nano-oxide SiO of interpolation
2The powder average particulate diameter is about 20nm, accounts for 0.001% of total powder weight;
4) the crystal-boundary phase alloy powder with master alloying powder and process nano-powder mixes in batch mixer under the benzinum protective medium, obtains mixed-powder, and wherein, the crystal-boundary phase alloy powder weight of process nano-powder accounts for 4% of total powder weight;
5) mixed-powder is orientated die mould under the magnetic field of 1.5T, and is pressed into green compact through the isostatic cool pressing of 17MPa;
6) employing high vacuum positive pressure sintering furnace at 1084 ℃ of sintering 4h, carries out green compact the one-level tempering at 900 ℃, then carries out second annealing at 630 ℃, obtains neodymium iron boron magnetic body;
The magnet for preparing is put into VSM measure its magnetic property, result is as follows:
B r=1.37T,
H cj=2146kA/m, (
BH)
max=358kJ/m
3, the magnet maximum operating temperature reaches 240 ℃.
Embodiment 3:
1) master alloying is adopted the rapid hardening slab, hydrogen is quick-fried and three kinds of techniques of airflow milling prepare the master alloying powder, described master alloying is in atomic percentage, 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 the crystal-boundary phase alloy powder, described crystal-boundary phase alloy is in atomic percentage, and its composition is Tb
72Fe
28
3) with the nano-oxide Dy of crystal-boundary phase alloy powder and interpolation
2O
3Powder mixes in batch mixer under the benzinum protective medium, obtains the crystal-boundary phase alloy powder through nano-powder, wherein, and the nano-oxide Dy of interpolation
2O
3The powder average particulate diameter is about 40nm, accounts for 10% of total powder weight;
4) the crystal-boundary phase alloy powder with master alloying powder and process nano-powder mixes in batch mixer under the benzinum protective medium, obtains mixed-powder, and wherein, the crystal-boundary phase alloy powder weight of process nano-powder accounts for 3% of total powder weight;
5) mixed-powder is orientated die mould under the magnetic field of 2T, and is pressed into green compact through the isostatic cool pressing of 17MPa;
6) employing high vacuum positive pressure sintering furnace at 1050 ℃ of sintering 5h, carries out green compact the one-level tempering at 950 ℃, then carries out second annealing at 650 ℃, obtains neodymium iron boron magnetic body;
The magnet for preparing is put into VSM measure its magnetic property, result is as follows:
B r=1.30T,
H cj=2900kA/m, (
BH)
max=368kJ/m
3, the magnet maximum operating temperature reaches 250 ℃.
Embodiment 4:
1) master alloying is adopted the rapid hardening slab, hydrogen is quick-fried and three kinds of techniques of airflow milling prepare the master alloying powder, described master alloying is in atomic percentage, 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 the mechanical ball grinding process to prepare the crystal-boundary phase alloy powder, described crystal-boundary phase alloy is in atomic percentage, and its composition is Gd
70Cu
30
3) the nano metal Cu powder with crystal-boundary phase alloy powder and interpolation mixes in batch mixer under the aviation gasoline protective medium, 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) the crystal-boundary phase alloy powder with master alloying powder and process nano-powder mixes in batch mixer under the aviation gasoline protective medium, obtains mixed-powder, and wherein, the crystal-boundary phase alloy powder weight of process nano-powder accounts for 10% of total powder weight;
5) mixed-powder is orientated die mould under the magnetic field of 2T, and is pressed into green compact through the isostatic cool pressing of 17MPa;
6) employing high vacuum positive pressure sintering furnace at 1125 ℃ of sintering 2h, carries out green compact the one-level tempering at 880 ℃, then carries out second annealing at 650 ℃, obtains neodymium iron boron magnetic body.
The magnet for preparing is put into VSM measure its magnetic property, result is as follows:
B r=1.35T,
H cj=1956kA/m, (
BH)
max=322kJ/m
3, the magnet maximum operating temperature reaches 250 ℃.
Claims (4)
1. high-coercive force high stability neodymium iron boron magnetic body based on crystal boundary reconstruct, it is characterized in that being calculated in mass percent and comprise 90 ~ 97% master alloying and 3 ~ 10% crystal-boundary phase alloy through nano-powders, wherein the crystal-boundary phase alloy 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, RE is rare earth element or Sc, the Y in other group of the lanthanides except Nd; 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 satisfy 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 satisfies: 0＜u＜100.
2. a kind of high-coercive force high stability neodymium iron boron magnetic body based on crystal boundary reconstruct according to claim 1, it is characterized in that 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 thereof, Zn and alloy thereof, Ti and alloy thereof, 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, the nano nitride powder is AlN, TiN, ZrN or Si
3N
4, the nano-carbide powder is TiC, SiC, Fe
3C, NbC, ZrC, WC or VC, the average particulate diameter of nanometer powder are 1 ~ 100nm.
3. the preparation method of the high-coercive force high stability neodymium iron boron magnetic body based on crystal boundary reconstruct as claimed in claim 1 or 2, it is characterized in that: the rich new Grain-Boundary Phase of heavy rare earth of Application of composite and nano modification technology, i.e. redesign and the new Grain-Boundary Phase that synthesizes rich heavy rare earth, realize magnetic hardening by heavy rare earth element to the diffusion in main phase grain boundary layer in magnet sintering and temper process, do not add or add less the low-cost high-coercive force magnet of preparation under the condition of heavy rare earth in principal phase; Add nanometer powder simultaneously in new Grain-Boundary Phase, optimize distribution and the grain boundary form of Grain-Boundary Phase by the nano modification method, the pinning domain wall suppresses the counter magnetic field forming core and promotes coercive force, the grain growth that effectively suppresses in sintering process promotes the comprehensive magnetic energy, thereby realizes the high-coercive force high stability of neodymium iron boron magnetic body.
4. the preparation method of a kind of high-coercive force high stability neodymium iron boron magnetic body based on crystal boundary reconstruct according to claim 3 is characterized in that its concrete steps are:
1) master alloying is adopted the rapid hardening slab, hydrogen is quick-fried and three kinds of techniques of airflow milling prepare the master alloying powder that average particulate diameter is 3 ~ 10 μ m, described master alloying is in atomic percentage, its composition is (Nd
aRE
1-a)
xFe
100-x-y-zM
yB
z
2) crystal-boundary phase alloy is adopted casting technique make ingot casting or adopt rapid hardening slab technique to make the 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 the crystal-boundary phase alloy powder that average particulate diameter is 1 ~ 10 μ m, 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) nano powder with crystal-boundary phase alloy powder and interpolation mixes in batch mixer under aviation gasoline or benzinum protective medium, 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) the crystal-boundary phase alloy powder with master alloying powder and process nano-powder mixes in batch mixer under aviation gasoline or benzinum protective medium, 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 is orientated die mould under the magnetic field of 1.5 ~ 3T, and is pressed into green compact through the isostatic cool pressing of 17MPa;
6) employing high vacuum positive pressure sintering furnace at 1050 ~ 1125 ℃ of sintering 2 ~ 5h, carries out green compact the one-level tempering at 880 ~ 950 ℃, then carries out second annealing at 480 ~ 650 ℃, obtains neodymium iron boron magnetic body.
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