CN107146671A - A kind of method of raising Y base sintered magnet magnetic properties - Google Patents
A kind of method of raising Y base sintered magnet magnetic properties Download PDFInfo
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- CN107146671A CN107146671A CN201710329955.5A CN201710329955A CN107146671A CN 107146671 A CN107146671 A CN 107146671A CN 201710329955 A CN201710329955 A CN 201710329955A CN 107146671 A CN107146671 A CN 107146671A
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- base sintered
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- ZLHLYESIHSHXGM-UHFFFAOYSA-N 4,6-dimethyl-1h-imidazo[1,2-a]purin-9-one Chemical compound N=1C(C)=CN(C2=O)C=1N(C)C1=C2NC=N1 ZLHLYESIHSHXGM-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000009792 diffusion process Methods 0.000 claims abstract description 52
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 37
- 239000000956 alloy Substances 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 8
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 11
- 238000002604 ultrasonography Methods 0.000 claims description 8
- 229910052779 Neodymium Inorganic materials 0.000 claims description 7
- 229910052684 Cerium Inorganic materials 0.000 claims description 6
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052771 Terbium Inorganic materials 0.000 claims description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims description 5
- 229910052772 Samarium Inorganic materials 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- 229910052693 Europium Inorganic materials 0.000 claims description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 2
- 229910052689 Holmium Inorganic materials 0.000 claims description 2
- 229910052765 Lutetium Inorganic materials 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 2
- 229910052775 Thulium Inorganic materials 0.000 claims description 2
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052787 antimony Inorganic materials 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 150000004678 hydrides Chemical class 0.000 claims description 2
- 239000011812 mixed powder Substances 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052706 scandium Inorganic materials 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 229910000906 Bronze Inorganic materials 0.000 claims 1
- 239000010974 bronze Substances 0.000 claims 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 11
- 239000002344 surface layer Substances 0.000 abstract description 4
- 230000005389 magnetism Effects 0.000 abstract description 2
- 230000005415 magnetization Effects 0.000 abstract description 2
- 239000000725 suspension Substances 0.000 description 24
- 150000002910 rare earth metals Chemical class 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 239000011521 glass Substances 0.000 description 6
- 229910001172 neodymium magnet Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052727 yttrium Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910000583 Nd alloy Inorganic materials 0.000 description 1
- 229910017557 NdF3 Inorganic materials 0.000 description 1
- 229910019322 PrF3 Inorganic materials 0.000 description 1
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/008—Ferrous alloys, e.g. steel alloys containing tin
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/60—Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur
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- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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Abstract
The invention provides a kind of method of raising Y base sintered magnet magnetic properties.By treating comprising Pr or/and Nd elements, diffusion-alloyed powder is uniformly mixed this method with organic solvent, obtains treating diffusion alloy liquid;It will treat that diffusion alloy liquid is attached to Y base sintered magnets surface, it is subsequently placed in progress grain boundary decision heat treatment in vacuum sintering furnace, Pr or/and Nd elements diffusions are made to enter the main phase grain top layer of Y base sintered magnets, finally carry out temper, enhance the magnetocrystalline anisotropy field of main phase grain surface layer, the reversion forming core at Grain Surface in reverse magnetization process is prevented, the magnetic properties such as remanent magnetism, maximum magnetic energy product and the coercivity of Y base sintered magnets is improved, obtains high performance Y bases sintered magnet.
Description
Technical field
The invention belongs to field of rare-earth permanent magnetic, more particularly to a kind of method of raising Y base rear earth permanent magnet performances.
Background technology
Rare-earth Nd-Fe-B permanent magnetic material is developed in the early 1980s, because it has high coercivity and maximum magnetic flux
Energy product, high comprehensive performance and be referred to as " magnetic king ".Since the advent of the world, in instrument and meter, microwave communication, wind-power electricity generation, electronic
The industry-by-industry of the national economy such as automobile, electronic information is used widely.With the fast development of human society, 2016 complete
The annual production of ball rare-earth permanent magnet has reached about 150,000 tons, and shows staggering growth trend.Due to Nd-Fe-B permanent magnet
In the rare earth element containing 30wt.% or so, therefore, with the continuous growth of Nd-Fe-B permanent magnet yield, rare earth element disappears
Consumption is also aggravated year by year.
Up to now, prepare Nd-Fe-B permanent magnet and still largely use LREE Nd, Pr and heavy rare earth element Dy, Tb
Deng.On the one hand, because LREE Nd, Pr and heavy rare earth element Dy, Tb etc. price are high, the valency of neodymium iron boron magnetic body is caused
Lattice remain high;On the other hand, rare earth element in the earth's crust content arrangement be followed successively by Ce, Y, La, Nd, Pr, Sm, Gd, Dy,
Tb ..., and a large amount of of rare-earth permanent magnet are used so that Pr, Nd, Dy, Tb are consumed rapidly, causes high abundance rare earth La, Ce, Y big
Amount overstocks, and causes rare earth resources to utilize unbalanced.Therefore, high abundance rare earth element La and Ce and Y how is made full use of to prepare high property
Energy rare-earth permanent magnet, is paid high attention to by rare earth permanent magnet circle.
The 2 of the formation of high abundance rare earth element:14:In 1 phase, Y2Fe14B has higher intrinsic magnetic properties can (Ha=
26kOe, 4 π Ms=14.1kG, Tc=565K), and the price of Y element is relatively low.Therefore high abundance rare earth is prepared with Y element
Permanent-magnet material, has broad application prospects.Patent document CN201611108740.2 is on the basis of Nd-Ce-Fe-B in magnetic
Ce elements are substituted with Y element in body, high abundance rare earth (Ce+Y) is obtained and accounts for total amount of rare earth 50wt.%, coercivity Hcj=9.7kOe,
Maximum magnetic energy product (BH)m> 29MGOe high abundance rare-earth permanent magnet.Simultaneously its temperature stability is studied, obtain α=-
0.1516% DEG C, β=- 0.5145% DEG C, its temperature stability is far above Ce base magnets.Magnet microstructure study is found,
There is Element segregation phenomenon in magnet containing Y, and core shell structure, i.e. Y element are formed in main phase grain and be mainly gathered in magnet master
The nucleus of phase crystal grain, Nd and Ce elements are concentrated mainly in the shell region of main phase grain and Grain-Boundary Phase.This structure class
It is similar to the shell structurre in recent years in the higher grain boundary decision formation of Nd-Fe-B fields attention rate, the Nd with high magnetic characteristics
Element aggregation improves the anisotropy field of main phase grain in main phase grain outer layer.
However, using in the shell structurre that is directly formed in main phase grain by the way of addition Y, NdPr elements in shell and
The difference of core content only has 1wt.% or so, and the raising effect to main phase grain magnetocrystalline anisotropy is limited.
The content of the invention
For the above-mentioned state of the art, the invention provides a kind of method of raising Y base sintered magnet magnetic properties, this method is adopted
With grain boundary decision method by Pr or/and Nd alloy diffusion enter sintering Y base sintered magnets in, improve main phase grain surface layer Nd or/
With the content of Pr elements, so that the magnetocrystalline anisotropy field on enhancing magnet main phase grain top layer, prevent in reverse magnetization process in crystalline substance
The reversion forming core of grain surface layer, obtains the Y base sintered magnets of high magnetic characteristics.
The technical scheme is that:A kind of method of raising Y base sintered magnet magnetic properties, will include Pr or/and Nd members
Plain treats that diffusion-alloyed powder is uniformly mixed with organic solvent, obtains treating diffusion alloy liquid;It will treat that diffusion alloy liquid is attached to Y bases
Sintered magnet surface, is subsequently placed in progress grain boundary decision heat treatment in vacuum sintering furnace, Pr or/and Nd elements diffusions is entered Y
The main phase grain top layer of base sintered magnet, finally carries out temper;
The composition of described Y base sintered magnets is:ReαYβBγMxFe100-α-β-γ-x
Wherein, Y is the rare earth element that there must be;
Re is rare earth element, including La, Ce, Pr, Nd, Pm, Sm, Eu, Tb, Dy, Ho, Er, Tm, Yb, Lu and Sc etc. in
One or more of elements;
M is addition element, the one or more member in Co, Cu, Nb, Ti, Zn, Ga, Al, Zr, Sn, Sb, Ta and W etc.
Element;
α, β, γ, x, y be each element weight percentage, the < β≤33.5,28.5 of 0≤α < 33.5,0≤alpha+beta≤
33.5,0.85≤γ≤1.1,0≤x≤2.
It is described to treat that diffusion-alloyed powder includes Pr or/and Nd elements, can be Pr or/and Nd hydride, oxide,
One or more mixed-powders in fluoride, chloride and sulfide etc..
Described organic solvent is not limited, including the one or more in ethanol, ethylene glycol, propane diols, polyvinyl alcohol etc.
Mixed liquor.
Preferably, the described granularity for treating diffusion-alloyed powder is less than 0.5 μm.
Preferably, described treats diffusion-alloyed powder with organic solvent according to mass ratio 1:1~2:1 mixing.
Preferably, described is treated into diffusion alloy liquid carries out ultrasonic disperse, mixture homogeneity is improved;Further preferably exist
The lower scattered 5~30min of 40W~80W ultrasounds.
Treat that diffusion alloy liquid is attached to the method on Y base sintered magnets surface and do not limited, including coating, submergence etc..
Preferably, in vacuum < 10-3Grain boundary decision heat treatment is carried out under the conditions of Pa.
Preferably, the treatment temperature of grain boundary decision heat treatment is 700 DEG C~900 DEG C.
Preferably, the processing time of grain boundary decision heat treatment is 2h~10h.
Preferably, temper is in vacuum < 10-3Carried out under the conditions of Pa.
Preferably, the treatment temperature of temper is 450 DEG C~700 DEG C.
Preferably, the processing time of temper is 2h~4h;
Embodiment
Below with reference to example, the present invention will be further described, and example of the invention is merely to illustrate the technology of the present invention
Scheme, and the non-limiting present invention.
Embodiment 1:
(1) granularity is less than to 0.5 μm of NdH3Alloy powder is with ethanol according to mass ratio 1:1 mixing, is stirred with glass bar,
Alloy powder is set to be blended completely with organic solvent;
(2) mixed liquor for obtaining step (1) disperses 30min under 50W ultrasounds, obtains diffusion alloy suspension;
(3) it is [Nd by nominal composition0.5(Ce0.35Y0.15)]30.5Al0.1Cu0.1Fe68.3B1Y base sintered magnets be totally submerged
In the suspension that step (2) is obtained, then take out, make magnet surface that there is one layer of suspension of covering;
(4) magnet of the surface covered with suspension is positioned over shady place, treats that it is dried;
(5) magnet that the surface covering obtained step (4) needs diffusion alloy is placed in vacuum sintering furnace, in vacuum
< 10-3Heat diffusion treatment 4h at Pa, 900 DEG C of diffusion heat temperature, obtains thermal diffusion magnet;
(6) magnet for obtaining step (5) is placed in vacuum sintering furnace, in vacuum < 10-3Pa, 700 DEG C of temperature is next time
Fire processing 2h, obtains final magnet.
Embodiment 2:
(1) granularity is less than to 0.5 μm of PrH3Alloy powder is with ethanol according to mass ratio 1:1 mixing, is stirred with glass bar,
Alloy powder is set to be blended completely with organic solvent;
(2) mixed liquor for obtaining step (1) disperses 30min under 50W ultrasounds, obtains diffusion alloy suspension;
(3) it is [Nd by nominal composition0.5(Ce0.35Y0.15)]30.5Al0.1Cu0.1Fe68.3B1Y base sintered magnets be totally submerged
In the suspension that step (2) is obtained, then take out, make magnet surface that there is one layer of suspension of covering;
(4) magnet of the surface covered with suspension is positioned over shady place, treats that it is dried;
(5) magnet that the surface covering obtained step (4) needs diffusion alloy is placed in vacuum sintering furnace, in vacuum
< 10-3Heat diffusion treatment 4h at Pa, 900 DEG C of diffusion heat temperature, obtains thermal diffusion magnet;
(6) magnet for obtaining step (5) is placed in vacuum sintering furnace, in vacuum < 10-3Pa, 700 DEG C of temperature is next time
Fire processing 2h, obtains final magnet.
Embodiment 3:
(1) granularity is less than to 0.5 μm of NdF3Alloy powder is with ethanol according to mass ratio 1:1 mixing, is stirred with glass bar,
Alloy powder is set to be blended completely with organic solvent;
(2) mixed liquor for obtaining step (1) disperses 30min under 50W ultrasounds, obtains diffusion alloy suspension;
(3) it is [Nd by nominal composition0.5(Ce0.35Y0.15)]30.5Al0.1Cu0.1Fe68.3B1Y base sintered magnets be totally submerged
In the suspension that step (2) is obtained, then take out, make magnet surface that there is one layer of suspension of covering;
(4) magnet of the surface covered with suspension is positioned over shady place, treats that it is dried;
(5) magnet that the surface covering obtained step (4) needs diffusion alloy is placed in vacuum sintering furnace, in vacuum
< 10-3Heat diffusion treatment 4h at Pa, 900 DEG C of diffusion heat temperature, obtains thermal diffusion magnet;
(6) magnet for obtaining step (5) is placed in vacuum sintering furnace, in vacuum < 10-3Pa, 700 DEG C of temperature is next time
Fire processing 2h, obtains final magnet.
Embodiment 4:
(1) granularity is less than to 0.5 μm of PrF3Alloy powder is with ethanol according to mass ratio 1:1 mixing, is stirred with glass bar,
Alloy powder is set to be blended completely with organic solvent;
(2) mixed liquor for obtaining step (1) disperses 30min under 50W ultrasounds, obtains diffusion alloy suspension;
(3) it is [Nd by nominal composition0.5(Ce0.35Y0.15)]30.5Al0.1Cu0.1Fe68.3B1Y base sintered magnets be totally submerged
In the suspension that step (2) is obtained, then take out, make magnet surface that there is one layer of suspension of covering;
(4) magnet of the surface covered with suspension is positioned over shady place, treats that it is dried;
(5) magnet that the surface covering obtained step (4) needs diffusion alloy is placed in vacuum sintering furnace, in vacuum
< 10-3Heat diffusion treatment 4h at Pa, 900 DEG C of diffusion heat temperature, obtains thermal diffusion magnet;
(6) magnet for obtaining step (5) is placed in vacuum sintering furnace, in vacuum < 10-3Pa, 700 DEG C of temperature is next time
Fire processing 2h, obtains final magnet.
Embodiment 5:
(1) granularity is less than to 0.5 μm of Nd2O3Alloy powder is with ethanol according to mass ratio 1:1 mixing, is stirred with glass bar,
Alloy powder is set to be blended completely with organic solvent;
(2) mixed liquor for obtaining step (1) disperses 30min under 50W ultrasounds, obtains diffusion alloy suspension;
(3) it is [Nd by nominal composition0.5(Ce0.35Y0.15)]30.5Al0.1Cu0.1Fe68.3B1Y base sintered magnets be totally submerged
In the suspension that step (2) is obtained, then take out, make magnet surface that there is one layer of suspension of covering;
(4) magnet of the surface covered with suspension is positioned over shady place, treats that it is dried;
(5) magnet that the surface covering obtained step (4) needs diffusion alloy is placed in vacuum sintering furnace, in vacuum
< 10-3Heat diffusion treatment 4h at Pa, 900 DEG C of diffusion heat temperature, obtains thermal diffusion magnet;
(6) magnet for obtaining step (5) is placed in vacuum sintering furnace, in vacuum < 10-3Pa, 700 DEG C of temperature is next time
Fire processing 2h, obtains final magnet.
Embodiment 6:
(1) granularity is less than to 0.5 μm of Pr2O3Alloy powder is with ethanol according to mass ratio 1:1 mixing, is stirred with glass bar,
Alloy powder is set to be blended completely with organic solvent;
(2) mixed liquor for obtaining step (1) disperses 30min under 50W ultrasounds, obtains diffusion alloy suspension;
(3) it is [Nd by nominal composition0.5(Ce0.35Y0.15)]30.5Al0.1Cu0.1Fe68.3B1Y base sintered magnets be totally submerged
In the suspension that step (2) is obtained, then take out, make magnet surface that there is one layer of suspension of covering;
(4) magnet of the surface covered with suspension is positioned over shady place, treats that it is dried;
(5) magnet that the surface covering obtained step (4) needs diffusion alloy is placed in vacuum sintering furnace, in vacuum
< 10-3Heat diffusion treatment 4h at Pa, 900 DEG C of diffusion heat temperature, obtains thermal diffusion magnet;
(6) magnet for obtaining step (5) is placed in vacuum sintering furnace, in vacuum < 10-3Pa, 700 DEG C of temperature is next time
Fire processing 2h, obtains final magnet.
Comparative example 1:
(1) it is [Nd by nominal composition0.5(Ce0.35Y0.15)]30.5Al0.1Cu0.1Fe68.3B1Y base sintered magnets be placed in vacuum
In sintering furnace, in vacuum < 10-3Heat diffusion treatment 4h at Pa, 900 DEG C of diffusion heat temperature, obtains thermal diffusion magnet;
(2) magnet for obtaining step (1) is placed in vacuum sintering furnace, in vacuum < 10-3Pa, 700 DEG C of temperature is next time
Fire processing 2h, obtains final magnet.
The magnetic property table of comparisons of obtained magnet is as shown in table 1 below in above-described embodiment 1-6 and comparative example 1.From
It is can be seen that in table 1 compared with comparative example 1, when the surface attachment in Y base sintered magnets includes Pr or/and Nd elements
Aluminium alloy, is heat-treated by grain boundary decision, Pr or/and Nd elements diffusions is entered magnet main phase grain top layer, is improved principal phase
The concentration of Pr or/and Nd elements at Grain Surface, enhances the magnetocrystalline anisotropy field of main phase grain surface layer, prevents magnetic reversal
During reversion forming core at Grain Surface, improve remanent magnetism, maximum magnetic energy product and the coercivity of Y base sintered magnets, obtain
Obtained high performance magnet.
Table 1:The magnetic property table of comparisons of each embodiment and comparative example
Although introducing and describing the embodiment of the present invention, the invention is not limited in this, but may be used also
Implemented with the other modes in the range of the technical scheme defined in appended claims.
Claims (10)
1. a kind of method of raising Y base sintered magnet magnetic properties, it is characterized in that:By treating comprising Pr or/and Nd elements, diffusion is closed
Bronze end is uniformly mixed with organic solvent, obtains treating diffusion alloy liquid;It will treat that diffusion alloy liquid is attached to Y base sintered magnet tables
Face, is subsequently placed in progress grain boundary decision heat treatment in vacuum sintering furnace, Pr or/and Nd elements diffusions is entered Y base sintered magnets
Main phase grain top layer, finally carry out temper;
The composition of described Y base sintered magnets is:ReαYβBγMxFe100-α-β-γ-x
Wherein, Y is the rare earth element that there must be;
Re be one kind in rare earth element, including La, Ce, Pr, Nd, Pm, Sm, Eu, Tb, Dy, Ho, Er, Tm, Yb, Lu and Sc or
Several elements;
M is addition element, one or more of elements in Co, Cu, Nb, Ti, Zn, Ga, Al, Zr, Sn, Sb, Ta and W;
α, β, γ, x, y be each element weight percentage, the < β≤33.5,28.5 of 0≤α < 33.5,0≤alpha+beta≤33.5,
0.85≤γ≤1.1,0≤x≤2.
2. the method for Y base sintered magnet magnetic properties is improved as claimed in claim 1, it is characterized in that:Described treats diffusion alloy
Powder is one or more mixed powders in Pr or/and Nd hydride, oxide, fluoride, chloride and sulfide
End.
3. the method for Y base sintered magnet magnetic properties is improved as claimed in claim 1, it is characterized in that:Described organic solvent bag
Include one or more kinds of mixed liquors in ethanol, ethylene glycol, propane diols, polyvinyl alcohol.
4. the method for Y base sintered magnet magnetic properties is improved as claimed in claim 1, it is characterized in that:Described treats diffusion alloy
The granularity of powder is less than 0.5 μm.
5. the method for Y base sintered magnet magnetic properties is improved as claimed in claim 1, it is characterized in that:Described treats diffusion alloy
Powder is with organic solvent according to mass ratio 1:1~2:1 mixing;
Preferably, described is treated into diffusion alloy liquid carries out ultrasonic disperse, mixture homogeneity is improved;Further preferably in 40W
The lower scattered 5~30min of~80W ultrasounds.
6. the method for Y base sintered magnet magnetic properties is improved as claimed in claim 1, it is characterized in that:Treat that diffusion alloy liquid adheres to
Method on Y base sintered magnets surface includes coating and/or submerged.
7. the method for Y base sintered magnet magnetic properties is improved as claimed in claim 1, it is characterized in that:In vacuum < 10-3Pa bars
Grain boundary decision heat treatment is carried out under part.
8. the method for the raising Y base sintered magnet magnetic properties as described in any claim in claim 1 to 7, it is characterized in that:
The treatment temperature of grain boundary decision heat treatment is 700 DEG C~900 DEG C.
9. the method for the raising Y base sintered magnet magnetic properties as described in any claim in claim 1 to 7, it is characterized in that:
The processing time of grain boundary decision heat treatment is 2h~10h.
10. the method for the raising Y base sintered magnet magnetic properties as described in any claim in claim 1 to 7, its feature
It is:The treatment temperature of temper is 450 DEG C~700 DEG C;
Preferably, the processing time of temper is 2h~4h;
Preferably, temper is in vacuum < 10-3Carried out under the conditions of Pa.
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CN110400669A (en) * | 2019-06-28 | 2019-11-01 | 宁波合盛磁业有限公司 | A kind of high performance neodymium iron boron of low heavy rare earth and preparation method thereof |
CN110473685A (en) * | 2019-08-27 | 2019-11-19 | 安徽省瀚海新材料股份有限公司 | A method of neodymium iron boron magnetic body is prepared using rare earth alloy modification |
CN111063536A (en) * | 2019-12-31 | 2020-04-24 | 浙江大学 | Grain boundary diffusion method suitable for bulk rare earth permanent magnet material |
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JP2015153813A (en) * | 2014-02-12 | 2015-08-24 | トヨタ自動車株式会社 | Method for producing rare earth magnet |
CN106128680A (en) * | 2016-08-24 | 2016-11-16 | 江西金力永磁科技股份有限公司 | A kind of modified neodymium iron boron magnetic body and preparation method thereof |
CN106252009A (en) * | 2016-07-26 | 2016-12-21 | 浙江大学 | A kind of high-performance richness La/Ce/Y rare-earth permanent magnet based on rare earth hydride interpolation and preparation method thereof |
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JP2015153813A (en) * | 2014-02-12 | 2015-08-24 | トヨタ自動車株式会社 | Method for producing rare earth magnet |
CN106252009A (en) * | 2016-07-26 | 2016-12-21 | 浙江大学 | A kind of high-performance richness La/Ce/Y rare-earth permanent magnet based on rare earth hydride interpolation and preparation method thereof |
CN106128680A (en) * | 2016-08-24 | 2016-11-16 | 江西金力永磁科技股份有限公司 | A kind of modified neodymium iron boron magnetic body and preparation method thereof |
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CN110400669A (en) * | 2019-06-28 | 2019-11-01 | 宁波合盛磁业有限公司 | A kind of high performance neodymium iron boron of low heavy rare earth and preparation method thereof |
CN110473685A (en) * | 2019-08-27 | 2019-11-19 | 安徽省瀚海新材料股份有限公司 | A method of neodymium iron boron magnetic body is prepared using rare earth alloy modification |
CN110473685B (en) * | 2019-08-27 | 2020-09-11 | 安徽省瀚海新材料股份有限公司 | Method for preparing neodymium-iron-boron magnet by modifying rare earth alloy |
CN111063536A (en) * | 2019-12-31 | 2020-04-24 | 浙江大学 | Grain boundary diffusion method suitable for bulk rare earth permanent magnet material |
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