CN107578912A - A kind of preparation method of the neodymium iron boron magnetic body with high-coercive force - Google Patents
A kind of preparation method of the neodymium iron boron magnetic body with high-coercive force Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 15
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 40
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 35
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 33
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 33
- 239000011737 fluorine Substances 0.000 claims abstract description 32
- 238000012545 processing Methods 0.000 claims abstract description 32
- 239000002002 slurry Substances 0.000 claims abstract description 29
- 239000003960 organic solvent Substances 0.000 claims abstract description 24
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 23
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 22
- 238000011282 treatment Methods 0.000 claims abstract description 21
- 230000032683 aging Effects 0.000 claims abstract description 20
- 239000011230 binding agent Substances 0.000 claims abstract description 19
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 16
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 6
- 125000001153 fluoro group Chemical group F* 0.000 claims abstract description 4
- 238000013329 compounding Methods 0.000 claims abstract description 3
- 238000004513 sizing Methods 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims description 29
- 239000002184 metal Substances 0.000 claims description 29
- 230000008569 process Effects 0.000 claims description 25
- 238000005245 sintering Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 18
- 229910052779 Neodymium Inorganic materials 0.000 claims description 12
- -1 ketone compounds Chemical class 0.000 claims description 10
- 238000001802 infusion Methods 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- GETTZEONDQJALK-UHFFFAOYSA-N (trifluoromethyl)benzene Chemical class FC(F)(F)C1=CC=CC=C1 GETTZEONDQJALK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 238000005253 cladding Methods 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 5
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- WRWPPGUCZBJXKX-UHFFFAOYSA-N 1-fluoro-4-methylbenzene Chemical compound CC1=CC=C(F)C=C1 WRWPPGUCZBJXKX-UHFFFAOYSA-N 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 3
- 239000004734 Polyphenylene sulfide Substances 0.000 claims description 2
- 150000001298 alcohols Chemical class 0.000 claims description 2
- 150000001299 aldehydes Chemical class 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229920000069 polyphenylene sulfide Polymers 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims 3
- 150000001336 alkenes Chemical class 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract description 9
- 239000011248 coating agent Substances 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 235000006708 antioxidants Nutrition 0.000 description 31
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 29
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 24
- 238000012360 testing method Methods 0.000 description 22
- 239000011268 mixed slurry Substances 0.000 description 20
- 239000012298 atmosphere Substances 0.000 description 19
- 230000002940 repellent Effects 0.000 description 16
- 239000005871 repellent Substances 0.000 description 16
- 238000005260 corrosion Methods 0.000 description 13
- 230000005389 magnetism Effects 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 229910052786 argon Inorganic materials 0.000 description 12
- 230000007797 corrosion Effects 0.000 description 12
- 239000007789 gas Substances 0.000 description 12
- 238000009792 diffusion process Methods 0.000 description 9
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 9
- 239000004698 Polyethylene Substances 0.000 description 7
- 238000003682 fluorination reaction Methods 0.000 description 7
- 229920000573 polyethylene Polymers 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 210000002615 epidermis Anatomy 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 238000003487 electrochemical reaction Methods 0.000 description 5
- 238000003754 machining Methods 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 5
- FWQVINSGEXZQHB-UHFFFAOYSA-K trifluorodysprosium Chemical compound F[Dy](F)F FWQVINSGEXZQHB-UHFFFAOYSA-K 0.000 description 5
- WRMNZCZEMHIOCP-UHFFFAOYSA-N 2-phenylethanol Chemical compound OCCC1=CC=CC=C1 WRMNZCZEMHIOCP-UHFFFAOYSA-N 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 230000004913 activation Effects 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 230000003321 amplification Effects 0.000 description 4
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 4
- 229910017052 cobalt Inorganic materials 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 238000003801 milling Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000003199 nucleic acid amplification method Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000005554 pickling Methods 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 3
- 150000004678 hydrides Chemical class 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 2
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000006253 efflorescence Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 2
- 206010037844 rash Diseases 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000004876 x-ray fluorescence Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 150000001217 Terbium Chemical class 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- AXRCYOXBQNOKHL-UHFFFAOYSA-N benzene terbium Chemical compound [Tb].C1=CC=CC=C1 AXRCYOXBQNOKHL-UHFFFAOYSA-N 0.000 description 1
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005324 grain boundary diffusion Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- QMEZUZOCLYUADC-UHFFFAOYSA-N hydrate;dihydrochloride Chemical compound O.Cl.Cl QMEZUZOCLYUADC-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910001512 metal fluoride Inorganic materials 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000036647 reaction Effects 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
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- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The present invention relates to a kind of preparation method of the neodymium iron boron magnetic body with high-coercive force, including heavy rare earth powder and antioxidant, binding agent, organic solvent are mixed to prepare into uniform sizing material, heavy rare earth powder is Dy, hydrogenates dysprosium, any one or a few the compounding in Tb, hydrogenation terbium, the mass fraction of heavy rare earth powder is 40 80% in slurry, the mass fraction of antioxidant is 5 20%, the mass fraction of binding agent is 2 10%, and surplus is organic solvent, and antioxidant is fluorine-containing antioxidant；Slurry is covered in the surface of sintered magnet afterwards, the thickness for controlling slurry is 20 100 μm, and processing is then dried；Dried magnet is sintered afterwards, Ageing Treatment, heavy rare earth Dy, Tb etc. usage amount can be reduced by producing the method for the present invention, while overcome requirement and fluoride of the grain boundary decision technology to product size, the oxide coating caducous problem of powder, and manufacturing process is simple.
Description
Technical field
The present invention relates to a kind of preparation method of neodymium iron boron magnetic body, more particularly to a kind of neodymium-iron-boron with high-coercive force
The preparation method of body, belong to the fabricating technology field of magnet.
Background technology
Nd-Fe-B series magnets are because its superior performance is widely used, especially because automobile and electronic application field pair
The demand of energy-saving motor, the market application of sintered NdFeB can further expand.NdFeB material remanent magnetism and coercitive carry
Height is advantageous to its rapid growth in motor market, but coercitive raising is always to sacrifice remanent magnetism as generation in traditional handicraft
Valency, and the heavy rare earth element Dy/Tb of larger specific gravity must be used to improve coercivity, cause the sharp increase of magnet cost.
It is existing it is disclosed maintain high remanent magnetism increase simultaneously coercitive method (K.Machida, H.Kawasaki,
T.Suzuki, M.Ito and T.Horikawa, " GrainBoundary Tailoring of Sintered Nd-Fe-B
Magnets and their Magnetic Properties ", powder powder in 2004 and association of powder powder metallurgy Japan
Powder＆Powder Metallurgy Society spring session publications, page 202) be：It is by sintered magnet machining
Small size, Dy or Tb are applied in magnet surface by sputtering and magnet carried out at a temperature of less than sintering temperature
Heating and thermal insulation processing, so that Dy or Tb are only diffused into crystal boundary.These methods allow Dy or Tb more efficiently in grain boundaries
Concentrate, and successfully increase coercivity in the case of no significantly loss remanent magnetism.When the specific surface area of magnet becomes much larger,
That is magnet becomes more hour, Dy or Tb amount will become much larger, thus this method be suitable only for it is small-sized or thin
Magnet.But, still left problem be to by the related low yield of deposited metal coating such as sputtering.
SHIN-ETSU HANTOTAI etc., which discloses, makes slurry by Tb or Dy oxide, fluoride and oxyfluoride and is coated on sintered magnet
Surface, slurry cladding process, heavy rare earth dvielement RH is made from sintered magnet diffusion into the surface with coating weight once, for coercive force
There is also boundary for the effect of raising.In order to realize that high coercive force improves effect, it is necessary to repeat coating sizing-agent, complex operation,
And the powder of magnetic sheet surface adhesion a large amount of Tb or Dy after handling, it need to machine or clean removal, complex process and cause wave
Take；Slurry coated on magnet surface is still powdery after the drying, easy to fall off, and magnet coercivity can not be carried significantly after processing
It is high.And the shortcomings that only coating metal alloy method is, it is difficult to coat gold in magnet surface with a large amount of and uniform coat weight
Belong to alloy.
In addition, the neodymium chemism in magnet is big, easily it is oxidized, corrosion-resistant, in a humidity environment, magnet surface
Form corrosivity micro cell, increase corrosion rate, the technology of existing increase neodymium iron boron surface anticorrosive ability include plating,
Organic coating and composite coating etc., it is being directed to improving the electrochemical properties of magnet.And it is above-mentioned using heavy rare-earth oxide,
The grain boundary diffusion process of fluoride improves surface treatment of the method for neodymium iron boron magnetic body coercivity and remanent magnetism not to magnet and risen
To favourable effect.
The content of the invention
Deficiency existing for its coercivity of neodymium iron boron magnetic body and remanent magnetism that the present invention produces for existing process, there is provided one
The preparation method of neodymium iron boron magnetic body of the kind with high-coercive force.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：
A kind of preparation method of the neodymium iron boron magnetic body with high-coercive force, comprises the following steps：
1) sintered magnet R1-Fe-B-M is prepared, and is pre-processed；
2) heavy rare earth powder and antioxidant, binding agent, organic solvent are mixed to prepare uniform sizing material, the heavy rare earth powder
End is Dy, hydrogenates dysprosium, any one or a few the compounding in Tb, hydrogenation terbium, and the quality of heavy rare earth powder is divided in the slurry
Number is 40-80%, and the mass fraction of antioxidant is 5-20%, and the mass fraction of binding agent is 2-10%, and surplus is organic molten
Agent, the antioxidant are fluorine-containing antioxidant；
3) slurry obtained by step 2) is covered in the sintered magnet surface of step 1), the thickness for controlling slurry is 20-100
μm, processing is then dried；
4) magnet obtained by step 3) is sintered, Ageing Treatment, produced.
Further, any one between the antioxidant is in two benzotrifluorides, o-fluorotobuene or p-fluorotoluene.
Further, binding agent described in step 2) is any one in butyral, polyethylene or polyphenylene sulfide.
Further, slurry is made to be covered in the method on sintered magnet surface as in spraying process, cladding process, infusion process in step 3)
One kind.
Further, metal Dy described in step 2) or metal Tb purity are more than 98%.
Further, the temperature of sintering is 800-960 DEG C, sintering time 6-16h in step 4), and the temperature of Ageing Treatment is
460-580 DEG C, the time of Ageing Treatment is 2-6h.
Further, organic solvent described in step 2) is one kind in alcohols, aldehydes, ketone compounds.
Further, the temperature of drying process is 60-100 DEG C in step 3).
Further, R1 is a kind of or several in Nd, Pr, Dy, Tb, Ho, Gd in the sintered magnet R1-Fe-B-M
Kind, its total amount is 26%-33wt%；One or more of the M in Ti, Mn, Co, Ga, Ca, Cu, Si, Al, Mg, Zr, Nb, its
Total amount is 0-5wt%；B total amounts are 0.8-1.2wt%；Surplus is Fe.
The beneficial effect of preparation method provided by the invention is：
1) mixed slurry of heavy rare earth powder provided by the invention and antioxidant, binding agent, organic solvent burns in magnet
During knot, relative to the DIFFUSION TREATMENT for directly using fluoride, oxide and oxyfluoride, it is not easy to form fluorination in magnet surface
Layer, oxide layer, reduce machining cost, simplify production technology；And heavy rare earth powder, hydride are compared with fluoride, oxide
It is easier to be diffused into magnet Grain-Boundary Phase, improves magnet coercivity, coercivity increases amount of increase and greatly promoted；
2) it is as follows using the effect of fluorine-containing antioxidant：In magnet diffusion process, first, using fluorine-containing antioxidant,
Serve the effect for preventing that heavy metal powder from aoxidizing；Second, fluorine-containing antioxidant can also play adhesive effect with binding agent, gold
Category powder is difficult for drop-off in magnet surface, and magnet coercivity greatly promotes；3rd, the fluorine chemistry stability in fluorine-containing antioxidant
Height, do not reacted with reactive rare earth element reaction, the displacements for being advantageous to the heavy rare earth element such as Nd and Dy/Tb in diffusion process such as Nd；
And it is different from chlorine element, chlorine is easy to form micro cell reaction in magnet surface, accelerates magnet corrosion, the use of fluorine-containing antioxidant
The generation of electrochemical reaction is avoided, improves magnet corrosion resistance；
3) method of the invention can reduce heavy rare earth Dy, Tb etc. usage amount, while overcome grain boundary decision technology pair
The requirement of product size and fluoride, the hydride coating caducous problem of powder, and manufacturing process is simple.
Embodiment
The principle and feature of the present invention are described below in conjunction with example, the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the present invention.
Metal Tb powder described in 1-4 of the embodiment of the present invention refers to metal Tb with hydrogenating the mixture of both terbiums, metal Dy
Powder refers to metal Dy with hydrogenating the mixture of both dysprosiums, in above-mentioned mixture, metal Tb or metal Dy mass fraction
More than 98%.
Embodiment 1：
1) preparation of sintered magnet：By neodymium, praseodymium, dysprosium, terbium, electrolytic iron, cobalt, copper, gallium, aluminium, zirconium, boron by weight：Nd-
23.8%, Pr-5%, Dy-0.6%, Tb-0.4%, Co-0.5%, Cu-0.13%, Ga-0.1%, Al-0.1%, Zr-
0.12%, B-1% ratio, surplus are iron and inevitable impurity, complete in vacuum melting furnace in an inert atmosphere
Into cast, 1450 DEG C of pouring temperature, chilling roller rotating speed is 60r/min, leads to cooling water in chilling roller, obtained flake thickness is about
0.36mm；Then, scale passes through HD powder, airflow milling, the magnetic that particle mean size is 3.4 μm is made；In normal temperature and magnetic field intensity
It is orientated for 2T in the environment of field and carries out orientation compacting, pressed compact is made；Pressed compact is put into the sintering furnace under Ar atmosphere, 1100 DEG C of burnings
Knot 5h obtains green compact, green compact timeliness 5h at a temperature of 500 DEG C, obtains sintering blank.Sintering blank is processed into by machining
Size is 40mm*20mm*4mm magnet, after the washing of oil removing, pickling, activation and deionized water after drying process, is designated as A0.
2) by 2.4 μm of fluorination terbium powder and ethanol according to weight ratio 2：Uniform mixed slurry is made in 3 ratio.Spraying process
The surface for the sintered magnet A0 being covered in after processing, the thickness of slurry is 100 μm, then 100 DEG C of drying in argon gas atmosphere, after
Sintered 16 hours at 920 DEG C, Ageing Treatment carries out grain boundary decision processing in 2 hours at 580 DEG C, is designated as A1.
3) by 2.4 μm of metal Tb powder, 1.3.5- benzotrichlorides, organic solvent ethanol, according to weight than 4:1:5 ratio
Uniform mixed slurry is made in example, and wherein Tb powder is mixed-powders of the metal Tb with hydrogenating terbium, and metal Tb mass fraction is 99%.
Spraying process is covered in the surface of the sintered magnet A0 after processing, and the thickness of slurry is 100 μm, then 100 DEG C of bakings in argon gas atmosphere
Dry, after being sintered 16 hours at 920 DEG C, Ageing Treatment carries out grain boundary decision processing in 2 hours at 580 DEG C, is designated as A2.
4) by two benzotrifluorides, binding agent butyral, organic solvent ethanol between 2.4 μm of metal Tb powder, antioxidant,
According to weight than 4:1:1:Uniform mixed slurry is made in 4 ratio.Spraying process is covered in the surface of the sintered magnet A0 after processing,
The thickness of slurry is 100 μm, then 100 DEG C of drying in argon gas atmosphere, after being sintered 16 hours at 920 DEG C, the timeliness at 580 DEG C
Processing carries out grain boundary decision processing in 2 hours, is designated as A3.
A1, A2, A3 magnet are taken respectively, 50 μm, the epidermis of 100 μ m thicks are ground off to magnet surface machinery respectively, using XRF
(X-ray fluorescence spectra analysis) tests the Oil repellent of magnet surface, has ground off the A1 of the addition fluorination terbium after 50 μm, magnet surface
Oil repellent be 1.8%, add the A3 of fluorine-containing antioxidant and binding agent, the Oil repellent of magnet surface is 0.8%；Grind off
100 μm magnet A2, A3 does not almost measure Oil repellent, and adds the A1 of fluorination terbium, and the Oil repellent of magnet surface is 1.4%.This
Be because the fluorine and the Tb that are fluorinated in A1 in terbium are to be diffused into inside magnet simultaneously, after product surface has ground off 100 μm, magnet table
Face can still detect the content of fluorine with XRF；And the A3 of fluorine-containing antioxidant and binding agent is added, its fluorine element derives from oxygen
Agent, when 100 DEG C are dry, binding agent evaporation, and antioxidant is remained in magnet surface, but can be volatilized in sintering process
Completely, therefore after progress magnet epidermis processing, F contents are not almost measured with XRF.
The magnetic property and A1, A2, A3 magnet of A0, A1, A2, A3 magnet grind off the survey of the test Oil repellents of the XRF behind top layer
Test result is as shown in table 1：
Table 1 A1, A2, A3 and A0 comparison of magnetic property
| Project | Br | Hcj | (BH)max | Hk/iHc | △Hcj | F contents | F contents |
| Unit | kGs | kOe | MGOe | - | kOe | 50 μm of mill | 100 μm of mill |
| A0 | 14.36 | 15.02 | 49.66 | 0.98 | - | - | - |
| A1 | 14.12 | 24.37 | 48.16 | 0.96 | 9.35 | 1.8% | 1.4% |
| A2 | 14.14 | 25.49 | 48.22 | 0.95 | 10.47 | - | - |
| A3 | 14.13 | 26.58 | 48.19 | 0.94 | 11.56 | 0.8% | - |
By the data in table 1 it will be seen that A1 magnets：Using the mixed slurry of fluorination terbium and organic solvent ethanol,
Its coercivity rises to 24.37kOe from A0 15.02kOe, and wants high by XRF detection, the amount containing F of A1 magnet surfaces
More, because with for the relative simple metal Tb of fluorination terbium diffusion, not only heavy rare earth element terbium can be diffused into magnet crystal boundary, fluorine element
Also it can be diffused into simultaneously inside magnet with terbium, thus have impact on the diffusion effect of heavy rare earth element terbium, and then to magnet coercivity
Lifting have an impact, the lifting of the coercivitys of A1 magnets is about 9.3kOe；A2：Using metal Tb powder and the chloromethanes of 1,3,5- tri-
The mixed slurry of benzene, organic solvent ethanol, its coercivity rise to 25.49kOe from A0 15.02kOe, coercivity amplification compared with
Greatly, 10kOe has been exceeded, and A0 to A2 is from 14.36kGs to 14.14kGs in terms of remanent magnetism, has no obvious reduction；A3：Using
Metal Tb powder and two benzotrifluoride, butyral, the mixed slurry of organic solvent ethanol, coercivity is from A0 15.02kOe
Be raised to 26.58kOe, coercivity amplification is maximum, has exceeded 11.5kOe, and in terms of remanent magnetism A0 to A3 be from 14.36kGs to
14.13kGs, have no obvious reduction；It is well known that using the diffusion technique of simple metal, metal is easy to aoxidize, thus generally adopts
With being not easy to be oxidized and the low metal fluoride of cost substitutes, but above-mentioned the results show, the fluorine in fluoride can be same
Heavy rare earth metal is diffused into inside magnet simultaneously, thus can also produce certain influence to the performance of magnet.
By above-mentioned A1, A2, A3 magnet, do corrosion resistance and test 4 days PCT, test result is as shown in table 2.
2 A1, A2, A3 magnet of table, 4 days PCT compare
| 4 days PCT (mg/cm2) | |
| A1 | 0.8 |
| A2 | 1.6 |
| A3 | 0.3 |
From the test result in table 2, the corrosion resistance of A3 products is best, because A3 products contain due to using
Fluorine antioxidant prevents the oxidation of Tb powder as antioxidant, and A2 products antioxidant is using chloride anti-oxidation
Easily with the neodymium in magnet electrochemical reaction occurs for agent, chlorion, causes magnet to corrode efflorescence, fluorine-containing antioxidant chemical stability
Height, not with neodymium occur electrochemical reaction, magnet will not be caused to corrode, at the same fluorine atom due to molecular mass it is lighter, be easy to volatilize,
Magnet surface is not trapped in, so as to influence the surface characteristic of magnet.
Embodiment 2：
1) by neodymium, dysprosium, terbium, cobalt, copper, aluminium, boron by weight：Nd-30.1%, Dy-0.5%, Co-0.8%, Cu-
0.13%, Al-0.2%, B-1% ratio, surplus are Fe and inevitable impurity, and vacuum in an inert atmosphere melts
Cast, 1450 DEG C of pouring temperature are completed in furnace, chilling roller rotating speed is 65r/min, leads to cooling water, obtained scale in chilling roller
Thickness about 0.32mm；Then, scale passes through HD powder, airflow milling, the magnetic that particle mean size is 3.2 μm is made；In normal temperature and magnetic
Field intensity is to carry out orientation compacting in the environment of 2T is orientated field, and pressed compact is made；Pressed compact is put into the sintering furnace under Ar atmosphere,
1060 DEG C of sintering 6h obtain green compact, green compact timeliness 4h at a temperature of 510 DEG C, obtain sintering blank.Hair will be sintered by machining
Base is processed into the magnet that size is 40mm*20mm*4mm, after the washing of oil removing, pickling, activation and deionized water after drying process,
It is designated as B0；
2) by 2.0 μm of DyF powder and organic solvent-acetone according to weight ratio 3:Uniform mixed slurry is made in 2 ratio.
Cladding process is covered in the surface of the sintered magnet B0 after processing, and the thickness of slurry is 50 μm, then 80 DEG C of drying in argon gas atmosphere,
After being sintered 8 hours at 800 DEG C, Ageing Treatment carries out grain boundary decision processing in 4 hours at 520 DEG C, is designated as B1.
3) by 2.0 μm of metal Dy powder, 1.3.5- benzotrichlorides, organic solvent-acetone, according to weight than 3:1:1 ratio
Uniform mixed slurry is made in example.Cladding process is covered in the surface of the sintered magnet B0 after processing, and the thickness of slurry is 50 μm, so
80 DEG C of drying in argon gas atmosphere afterwards, after being sintered 8 hours at 800 DEG C, Ageing Treatment carries out grain boundary decision in 4 hours at 520 DEG C
Processing, is designated as B2.
4) by 2.0 μm of metal Dy powder, o-fluorotobuene, polyethylene, organic solvent-acetone, according to weight than 30:10:1:
Uniform mixed slurry is made in 9 ratio.Cladding process is covered in the surface of the sintered magnet B0 after processing, and the thickness of slurry is 50
μm, then 80 DEG C of drying in argon gas atmosphere, after being sintered 8 hours at 800 DEG C, Ageing Treatment carries out crystal boundary in 4 hours at 520 DEG C
DIFFUSION TREATMENT, it is designated as B3.
B1, B2, B3 magnet are taken respectively, 50 μm, the epidermis of 100 μ m thicks are ground off to magnet surface machinery respectively, using XRF
(X-ray fluorescence spectra analysis) tests the Oil repellent of magnet surface, has ground off 50 μm of magnet B2 and has not almost measured Oil repellent, has added
Add the B1 of dysprosium fluoride, the Oil repellent of magnet surface is 1.4%, adds the B3 of fluorine-containing antioxidant, and the Oil repellent of magnet surface is
0.2%；100 μm magnet B2, B3 are ground off and have not almost measured Oil repellent, and added the B1 of dysprosium fluoride, the fluorine of magnet surface contains
Measure as 1.1%.Because the fluorine of dysprosium fluoride is diffused into the inside of magnet with dysprosium in B1 magnets simultaneously, product surface is ground off
After 100 μm, magnet surface can still detect the content of fluorine with XRF；And the B3 of fluorine-containing antioxidant and binding agent is added, fluorine member
Antioxidant is usually come from, when 80 DEG C are dry, binding agent evaporation, and antioxidant remains in magnet surface, and sintering process
In can volatilize completely because, carry out magnet epidermis processing after, F contents are not almost measured with XRF.
The magnetic property and B1, B2, B3 magnet of B0, B1, B2, B3 magnet grind off the survey of the test Oil repellents of the XRF behind top layer
Test result is as shown in table 3：
Table 3 B1, B2, B3 and B0 comparison of magnetic property
| Project | Br | Hcj | (BH)max | Hk/iHc | △Hcj | F contents | F contents |
| Unit | kGs | kOe | MGOe | - | kOe | 50 μm of mill | 100 μm of mill |
| B0 | 13.8 | 14.31 | 45.85 | 0.99 | - | - | - |
| B1 | 13.65 | 20.28 | 44.86 | 0.98 | 5.97 | 1.4% | 1.1% |
| B2 | 13.66 | 20.94 | 44.92 | 0.99 | 6.63 | - | - |
| B3 | 13.64 | 21.75 | 44.81 | 0.98 | 7.44 | 0.2% | - |
The B1 it can be seen from data in table 3：Using fluorination terbium and organic solvent-acetone mixed slurry, coercivity from
14.31kOe rises to 20.28kOe, and by XRF detection, the amounts containing F of B1 magnet surfaces wants high more, because being expanded with fluoride
Dissipate for being spread compared with simple metal, not only heavy rare earth element terbium can be diffused into magnet crystal boundary, and fluorine element can also spread together with terbium
To inside magnet, so as to have impact on the diffusion effect of heavy rare earth terbium, and then the coercitive lifting of magnet is had an impact, therefore B1
The coercivity lifting of magnet is about 6kOe；B2：Using the mixing of simple metal Dy and 1,3,5- benzotrichlorides, organic solvent-acetone
Slurry, coercivity rise to 20.94kOe from 14.31kOe, and coercivity amplification is larger, and remanent magnetism in terms of B0 to B2 be from
13.8kGs to 13.66kGs, have no obvious reduction.B3：Using metal Dy powder and o-fluorotobuene, polyethylene, organic solvent
Mixed slurry, coercivity rises to 21.75kOe from 14.31kOe, and coercivity amplification is maximum, about 7.5kOe, and in terms of remanent magnetism
B0 to B3 is from 13.8kGs to 13.64kGs, has no obvious reduction.
By above-mentioned B1, B2, B3 magnet, do corrosion resistance and test 4 days PCT, test result is as shown in table 4：
4 B1, B2, B3 magnet of table, 4 days PCT compare
| 4 days PCT (mg/cm2) | |
| B1 | 1.2 |
| B2 | 2.1 |
| B3 | 0.6 |
From the test result in table 4, the corrosion resistance of B3 products is best, because B3 products are using fluorine-containing anti-
Oxidant prevents the oxidation of metal Dy powder as antioxidant, and the antioxidant of B2 products is using chloride oxygen
Easily with the neodymium in magnet electrochemical reaction occurs for agent, chlorion, causes magnet to corrode efflorescence, fluorine-containing antioxidant chemically stable
Property it is high, electrochemical reaction does not occur with neodymium, does not cause magnet to corrode.
Embodiment 3：
1) by neodymium, dysprosium, terbium, cobalt, copper, aluminium, boron by weight：Nd-30.5%, Tb-0.5%, Co-1.1%, Cu-
0.16%, Al-0.4%, B-1.02% ratio, surplus are Fe and inevitable impurity, in an inert atmosphere true
Cast, 1460 DEG C of pouring temperature are completed in empty smelting furnace, chilling roller rotating speed is 70r/min, leads to cooling water in chilling roller, obtains
Flake thickness about 0.3mm；Then scale passes through HD powder, airflow milling, the magnetic that particle mean size is 3.0 μm is made；In normal temperature and
Magnetic field intensity is to carry out orientation compacting in the environment of 2T is orientated field, and pressed compact is made；530 DEG C of Ageing Treatments, aging time are carried out again
For 4.0h, obtain sintering blank.By machine by sinter blank be processed into size be 40mm*20mm*4mm magnet, through except
After oil, pickling, activation and deionized water washing after drying process, C0 is designated as.
2) by 3.2 μm of dysprosium fluoride, be fluorinated the mixed-powder (wherein the part by weight of dysprosium fluoride be 40%) of terbium with it is organic
Solvent benzaldehyde is according to weight than 4:Uniform mixed slurry is made in 1 ratio.Infusion process is covered in the sintered magnet after processing
C0 surface, the thickness of slurry is 20 μm, then 60 DEG C of drying in argon gas atmosphere, is sintered 6 hours at 960 DEG C, after 460 DEG C
Lower Ageing Treatment carries out grain boundary decision processing in 6 hours, is designated as C1.
3) by mixed-powder (the wherein weight of metal Dy powder of 3.2 μm of metal Dy powder and metal Tb powder constituents
Ratio be 40%), p-fluorotoluene, polyethylene, organic solvent benzaldehyde, according to weight than 16:1:1:2 ratio is made uniform
Mixed slurry.Infusion process is covered in the surface of the sintered magnet C0 after processing, and the thickness of slurry is 20 μm, then in argon gas atmosphere
60 DEG C of drying, are sintered 6 hours at 960 DEG C, are carried out grain boundary decision processing within 6 hours after Ageing Treatment at 460 DEG C, are designated as C2.
C1, C2 magnet are taken respectively, 50 μm, the epidermis of 100 μ m thicks are ground off to magnet surface machinery, using XRF (X ray
Spectrofluorimetry) test magnet surface Oil repellent, ground off 50 μm of C1 magnets, the Oil repellent of magnet surface is
2.11%, 100 μm of C1 magnets are ground off, the Oil repellent of magnet surface is 0.9%.Because in C1 be fluorinated terbium in fluorine with
Dy/Tb is diffused into the inside of magnet simultaneously, and after product surface has ground off 100 μm, magnet surface still can detect fluorine with XRF
Content；And the C2 of fluorine-containing antioxidant and binding agent is added, fluorine element derives from antioxidant, can be basic in sintering process
On be evaporated completely complete, after carrying out magnet epidermis processing, F contents are not almost measured with XRF.
The magnetic property and C1, C2 magnet of C0, C1, C2 magnet grind off the test result of the test Oil repellents of the XRF behind top layer
As shown in table 5：
Table 5 C1, C2 and C0 comparison of magnetic property
| Project | Br | Hcj | (BH)max | Hk/iHc | △Hcj | F contents | F contents |
| Unit | kGs | kOe | MGOe | - | kOe | 50 μm of mill | 100 μm of mill |
| C0 | 13.59 | 15.52 | 44.62 | 0.99 | - | - | - |
| C1 | 13.48 | 25.62 | 43.92 | 0.95 | 10.10 | 2.11% | 0.9% |
| C2 | 13.52 | 26.56 | 43.99 | 0.94 | 11.04 | - | - |
Used it can be seen from the data in table 5 containing metal dust, antioxidant, binding agent, organic solvent mixing slurry
The products C 2 of material is than directly using fluoride, compared with products C 1 made of organic solvent mixed slurry, coercivity increasing degree is more
Height, and remanent magnetism does not reduce significantly, properties of product are more preferable.
Above-mentioned C1, C2 magnet is done into corrosion resistance and tests 4 days PCT, test result is as shown in table 6.
6 C1, C2 magnet of table, 4 days PCT compare
| 4 days PCT (mg/cm2) | |
| C1 | 1.3 |
| C2 | 0.6 |
From the test result in table 6, the corrosion resistance of C2 products is best.
Embodiment 4：
1) by neodymium, praseodymium, dysprosium, terbium, electrolytic iron, cobalt, copper, gallium, aluminium, zirconium, boron percentage composition by weight：Nd-24.3%, Pr-
5%, Dy-0.5%, Fe-68.29%, Co-0.5%, Cu-0.13%, Ga-0.1%, Al-0.1%, Zr-0.12%, B-1%
Ratio, vacuum melting furnace in an inert atmosphere completes cast, and 1450 DEG C of pouring temperature, chilling roller rotating speed is 60r/
Min, obtained flake thickness about 0.3mm；Scale passes through HD powder, airflow milling, the powder that particle mean size is 2.8 μm is made；
It is orientated compressing in 15kOe magnetic field, pressed compact is made；Pressed compact is put into the sintering furnace under Ar atmosphere, 1070 DEG C of sintering 5h
Green compact are obtained, green compact timeliness 5h at a temperature of 500 DEG C, obtain sintering blank.Sintering blank is processed into by size by machining
For 40mm*20mm*4mm 50M magnets, after the washing of oil removing, pickling, activation and deionized water after drying process, D is designated as0。
2) by 2.8 μm hydrogenation dysprosium, hydrogenate terbium mixed-powder (wherein hydrogenate dysprosium part by weight be 40%) with it is organic
Solvent benzyl carbinol is according to weight than 1:Uniform mixed slurry is made in 1 ratio.Infusion process is covered in the sintered magnet after processing
D0 surface, the thickness of slurry is 80 μm, then 70 DEG C of drying in argon gas atmosphere, is sintered 6 hours at 920 DEG C, after 510 DEG C
Lower Ageing Treatment carries out grain boundary decision processing in 5 hours, is designated as D1.
3) by 2.8 μm of hydrogenation dysprosium, benzotrifluoride, polyethylene, organic solvent benzyl carbinol, according to weight than 5:1:1:3
Uniform mixed slurry is made in ratio.Infusion process is covered in the surface of the sintered magnet D0 after processing, and the thickness of slurry is 80 μm,
Then 70 DEG C of drying in argon gas atmosphere, are sintered 6 hours at 920 DEG C, and crystal boundary expansion is carried out within 5 hours after Ageing Treatment at 510 DEG C
Processing is dissipated, is designated as D2.
4) by 2.8 μm of hydrogenation terbium, benzotrifluoride, polyethylene, organic solvent benzyl carbinol, according to weight than 5:1:1:3
Uniform mixed slurry is made in ratio.Infusion process is covered in the surface of the sintered magnet D0 after processing, and the thickness of slurry is 80 μm,
Then 70 DEG C of drying in argon gas atmosphere, are sintered 6 hours at 920 DEG C, and crystal boundary expansion is carried out within 5 hours after Ageing Treatment at 510 DEG C
Processing is dissipated, is designated as D3.
5) by 2.8 μm of hydrogenation dysprosium, mixed-powder (part by weight for wherein hydrogenating dysprosium is 40%), the fluoroform of hydrogenation terbium
Benzene, polyethylene, organic solvent benzyl carbinol, according to weight than 5:1:1:Uniform mixed slurry is made in 3 ratio.Infusion process covers
The surface of sintered magnet D0 after processing, the thickness of slurry is 80 μm, then 70 DEG C of drying in argon gas atmosphere, at 920 DEG C
Sintering 6 hours, carry out grain boundary decision processing within 5 hours after Ageing Treatment at 510 DEG C, be designated as D4.
The magnetism testing result of D0, D1, D2, D3, D4 magnet is as shown in table 7：
Table 7 D1, D2, D3, D4 and D0 comparison of magnetic property
| Project | Br | Hcj | (BH)max | Hk/iHc |
| Unit | kGs | kOe | MGOe | - |
| D0 | 14.31 | 15.02 | 49.66 | 0.97 |
| D1 | 14.25 | 24.53 | 48.72 | 0.95 |
| D2 | 14.26 | 22.05 | 49.15 | 0.96 |
| D3 | 14.26 | 26.89 | 49.18 | 0.95 |
| D4 | 14.27 | 25.61 | 49.21 | 0.95 |
Used it can be seen from the data in table 5 containing metal dust, antioxidant, binding agent, organic solvent mixing slurry
Product D2, D3, D4 of material are than directly using hydride, compared with product D1 made of the mixed slurry of organic solvent, coercivity increases
Long amplitude is higher, and remanent magnetism does not reduce significantly, and properties of product are more preferable.
Above-mentioned D1, D2, D3, D4 magnet is done into corrosion resistance respectively and tests 4 days PCT, test result is as shown in table 8.
8 D1, D2, D3, D4 magnet of table, 4 days PCT compare
| 4 days PCT (mg/cm2) | |
| D1 | 1.1 |
| D2 | 0.3 |
| D3 | 0.25 |
| D4 | 0.2 |
From the test result in table 8, the corrosion resistance of D2, D3, D4 product far due to D1 products, D4 products
Anti-corrosion capability is best.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.
Claims (10)
1. a kind of preparation method of the neodymium iron boron magnetic body with high-coercive force, it is characterised in that comprise the following steps：
1) sintered magnet R1-Fe-B-M is prepared, and is pre-processed；
2) heavy rare earth powder and antioxidant, binding agent, organic solvent are mixed to prepare uniform sizing material, the heavy rare earth powder is
Any one or a few compounding in Dy, hydrogenation dysprosium, Tb, hydrogenation terbium, the mass fraction of heavy rare earth powder is in the slurry
40-80%, the mass fraction of antioxidant is 5-20%, and the mass fraction of binding agent is 2-10%, and surplus is organic solvent, institute
It is fluorine-containing antioxidant to state antioxidant；
3) slurry obtained by step 2) is covered in the sintered magnet surface of step 1), the thickness for controlling slurry is 20-100 μm,
Then processing is dried；
4) magnet obtained by step 3) is sintered, Ageing Treatment, produced.
2. preparation method according to claim 1, it is characterised in that the antioxidant be between two benzotrifluorides, adjacent fluorine
Any one in toluene or p-fluorotoluene.
3. preparation method according to claim 1, it is characterised in that binding agent described in step 2) is butyral, poly- second
Any one in alkene or polyphenylene sulfide.
4. preparation method according to claim 1, it is characterised in that make slurry be covered in sintered magnet surface in step 3)
Method be spraying process, cladding process, one kind in infusion process.
5. preparation method according to claim 1, it is characterised in that metal Dy described in step 2) or metal Tb purity
More than 98%.
6. according to the preparation method any one of claim 1-5, it is characterised in that the temperature of sintering is in step 4)
800-960 DEG C, sintering time 6-16h.
7. preparation method according to claim 6, it is characterised in that the temperature of Ageing Treatment described in step 4) is 460-
580 DEG C, the time of Ageing Treatment is 2-6h.
8. according to the preparation method any one of claim 1-5, it is characterised in that organic solvent is described in step 2)
One kind in alcohols, aldehydes, ketone compounds.
9. according to the preparation method any one of claim 1-5, it is characterised in that the temperature of drying process in step 3)
For 60-100 DEG C.
10. according to the preparation method any one of claim 1-5, it is characterised in that the sintered magnet R1-Fe-B-M
One or several kinds of the middle R1 in Nd, Pr, Dy, Tb, Ho, Gd, its total amount are 26-33wt%；M be selected from Ti, Mn, Co, Ga,
One or more in Ca, Cu, Si, Al, Mg, Zr, Nb, its total amount are 0-5wt%；B total amounts are 0.8-1.2wt%；Surplus is
Fe。
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