CN103745823A - Preparation method for R-Fe-B-series sintering magnet - Google Patents
Preparation method for R-Fe-B-series sintering magnet Download PDFInfo
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- CN103745823A CN103745823A CN201410034871.5A CN201410034871A CN103745823A CN 103745823 A CN103745823 A CN 103745823A CN 201410034871 A CN201410034871 A CN 201410034871A CN 103745823 A CN103745823 A CN 103745823A
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- 238000005245 sintering Methods 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 40
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 40
- 238000007751 thermal spraying Methods 0.000 claims abstract description 40
- 238000005507 spraying Methods 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 239000013078 crystal Substances 0.000 claims abstract description 11
- 230000001681 protective effect Effects 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 238000012545 processing Methods 0.000 claims description 29
- 229910052751 metal Inorganic materials 0.000 claims description 22
- 239000002184 metal Substances 0.000 claims description 22
- 230000032683 aging Effects 0.000 claims description 14
- 230000004913 activation Effects 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 11
- 238000005554 pickling Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 6
- 229910052779 Neodymium Inorganic materials 0.000 claims description 5
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 229910052735 hafnium Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 229910052715 tantalum 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
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 50
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 27
- 229910045601 alloy Inorganic materials 0.000 abstract description 16
- 239000000956 alloy Substances 0.000 abstract description 16
- 150000002910 rare earth metals Chemical class 0.000 abstract description 16
- 238000009792 diffusion process Methods 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000007796 conventional method Methods 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 24
- 230000008569 process Effects 0.000 description 22
- 239000007921 spray Substances 0.000 description 20
- 239000000843 powder Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 230000008018 melting Effects 0.000 description 9
- 238000002844 melting Methods 0.000 description 9
- 238000005406 washing Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 8
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- 230000003321 amplification Effects 0.000 description 7
- 238000005520 cutting process Methods 0.000 description 7
- 238000001704 evaporation Methods 0.000 description 7
- 230000008020 evaporation Effects 0.000 description 7
- 230000005389 magnetism Effects 0.000 description 7
- 238000003199 nucleic acid amplification method Methods 0.000 description 7
- 230000007115 recruitment Effects 0.000 description 5
- 238000010183 spectrum analysis Methods 0.000 description 5
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 4
- 229910001172 neodymium magnet Inorganic materials 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- 229910001117 Tb alloy Inorganic materials 0.000 description 3
- MOSURRVHVKOQHA-UHFFFAOYSA-N [Tb].[Dy] Chemical compound [Tb].[Dy] MOSURRVHVKOQHA-UHFFFAOYSA-N 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005324 grain boundary diffusion Methods 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 238000007906 compression Methods 0.000 description 1
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- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The invention relates to a preparation method for an R-Fe-B-series sintering magnet. The preparation method for the R-Fe-B-series sintering magnet comprises the following steps of firstly, preparing an R-Fe-B-series sintering magnet with the thickness of 1-10mm by using the conventional method; secondly, spraying DyTb alloy with the thickness of 10-200 micrometers and the Dy mass percent of 60%-90% on the surface of the sintering magnet in a sealing box at an Ar gas protective atmosphere by using a thermal spraying method; and finally, placing the sintering magnet with the DyTb alloy on the surface in a vacuum sintering furnace, and performing heat treatment on the sintering magnet in a vacuum or Ar gas protective atmosphere at the temperature of 750-1000 DEG C so that heavy rare earth elements such as Tb and Dy enter the sintering magnet along a crystal boundary by diffusion. The DyTb alloy is sprayed on the surface of the sintering magnet by using the thermal spraying method, the problem of waste on resources due to high volatility of the Dy is solved, a phenomenon that production only depends on the heavy rare earth Tb with quite low content is avoided, the treatment speed is high, the coating is uniform, the yield is high, and the coercivity of the magnet after heat treatment is performed on the magnet is greatly improved.
Description
Technical field
The present invention relates to a kind of preparation method of R-Fe-B based sintered magnet, belong to rare earth permanent-magnetic material field.
Background technology
R-Fe-B be rare-earth sintering magnet due to its higher intensity, good magnetic property, cheap cost, since self-discovery, obtained develop rapidly, be widely used in the conglomerate fields such as hard disc of computer, hybrid vehicle, medical treatment, wind power generation.
Coercive force is the important indicator of weighing rare-earth sintering magnet magnetic property, and traditional coercitive method of raising magnet is in fusion process, to add simple metal or the alloy of rare earth raw material Tb or Dy.Because Tb or Dy major part enter principal phase, and only have small part to be distributed in crystal boundary, to magnet, coercitive raising has contribution, causes the utilance of Tb or Dy low.Because global rare earth resources is relatively deficient in recent years, especially heavy rare earth element Tb or Dy price increase substantially, and reduce production costs, reduce the consumption of heavy rare earth element, guarantee that the magnetic property that magnet is high becomes important development direction of neodymium iron boron industry simultaneously.
Crystal boundary diffusion method method (grain boundary diffusion) refers to Tb, Dy or its compound is provided around sintered NdFeB magnet, at high temperature make the melting of magnet Grain-Boundary Phase, make Tb or the Dy a kind of method along the crystal boundary of magnet from diffusion into the surface to sintered magnet inside.The method has improved the utilance of heavy rare earth element greatly, has reduced the use amount of heavy rare earth element, and can increase substantially the coercive force of magnet.
Patent documentation JP-A2004-304543, JP-A2004-377379, JP-A2005-0842131 disclose and the oxide of Tb or Dy, fluoride and oxyfluoride are done to form slurry have been coated on sintered magnet surface, put into that sintering furnace carries out high temperature and Ageing Treatment makes Tb or Dy along crystal boundary, enter the method for sintered magnet inside after oven dry.Use the method complicated operation, the powder of a large amount of Tb of magnetic sheet surface adhesion after treatment or Dy, needs machining or cleans and remove, complex process and cause waste; The slurry that is coated on magnet surface is still powdery after oven dry, easily come off, and after processing, magnet coercive force can not increase substantially.
Patent documentation JP-A2006-058555 discloses evaporation heavy rare earth material and has diffused into simultaneously the method for sintered magnet inside, and the fluoride that patent documentation JP-A2006-344779 discloses evaporation Tb or Dy diffuses into the method for sintered magnet inside simultaneously.Adopt the method to process magnet, need strict evaporation source evaporation rate and the vapour concentration controlled, very high to the requirement of temperature, vacuum degree and operating system; Owing to being subject to processing between magnet and evaporation source, have certain intervals, reduced space availability ratio, processing cost is higher simultaneously.
Patent documentation JP-A2009-166488 discloses rare earth magnet has been contacted with the diffuse source of heavy rare earth metal or alloy, adopts the method for similar barrel plating at high temperature to complete the diffusion of heavy rare earth element to sintered magnet inside.Because heavy rare earth element is that Grain-Boundary Phase at high temperature melts to the prerequisite of sintered magnet diffusion inside, and fusing Grain-Boundary Phase in Pr, Nd very easily replace with heavy rare earth element, once so move not in time, sintered magnet and heavy rare earth metal or alloy are easily sticked together, and practicality is poor.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of R-Fe-B based sintered magnet, this method has overcome in prior art with the oxide of Tb or Dy or fluoride slurry cladding process coating adhesion is poor, the problem of complicated operation, overcome and adopted evaporation coating method to strict high, treatment effeciency is low, cost the is high problem of operating system call, avoided using the existing method cause the problem of sintered magnet and the adhesion of heavy rare earth material.The inventive method is simple to operate, and cost is low, and productive rate is high, has significantly improved the performance of magnet simultaneously.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of preparation method of R-Fe-B based sintered magnet, comprising:
1) adopt the method that well known to a person skilled in the art to prepare R
1-Fe-B-M sintered magnet, wherein, R
1be selected from one or more in Nd, Pr, Dy, Tb, its total amount is 27wt%～32wt%; M is selected from one or more in Ti, V, Cr, Mn, Co, Ni, Ga, Ca, Cu, Zn, Si, Al, Mg, Zr, Nb, Hf, Ta, W, Mo, and its total amount is 0～3wt%; B total amount is 0.8wt%～1.2wt%; All the other are Fe;
2) sintered magnet step 1) being obtained carries out oil removing, pickling, activation and washed with de-ionized water processing;
3) by step 2) in sintered magnet after cleaning put into stuffing box and make sintered magnet in circulation A r gas protective atmosphere, on sintered magnet surface, use heat spraying method apply a layer thickness be 10～200 μ m containing Dy ratio at 60%～90% DyTb alloy-layer;
4) sintered magnet after treatment step 3) is put into vacuum sintering furnace, 750～1000 ℃ of heat treatment 2～72h, in vacuum sintering furnace, vacuum degree control is 10
-2～10
-5the Ar gas protective atmosphere that adopts 5～20kPa in Pa or vacuum sintering furnace, makes metal Tb and Dy diffuse into sintered magnet inside by crystal boundary;
5) by sintered magnet after treatment step 4) at 450～600 ℃ of Ageing Treatment 1～10h, obtain R-Fe-B based sintered magnet.
On the basis of technique scheme, the present invention can also do following improvement.
Further, in step 3), the size that it is 100mm that the sintered magnet of accepting thermal spraying has along maximal side, is the size of 10mm to the maximum along anisotropic orientation.
Further, in step 3), on sintered magnet surface, using heat spraying method to apply a layer thickness is the DyTb alloy-layer of 20～100 μ m.
Further, in step 3), Ar gas input port and Ar gas control valve are set on the casing of stuffing box, casing arranges Ar air compressor outward, basicly stable to maintain box house pressure.
Further, in step 3), sintered magnet was closely arranged in stuffing box inside before thermal spraying, sintered magnet one side is carried out overturning after thermal spraying, another side was carried out to thermal spraying treatment.
Further, in step 4), in vacuum sintering furnace, temperature is 820～900 ℃, and heat treatment time is 5～72h, and in vacuum sintering furnace, vacuum degree is 10
-3～10
-4pa, or the interior Ar gas protective atmosphere that adopts 5～10kPa of vacuum sintering furnace.
Further, in step 5), aging temperature is 470～550 ℃, and the processing time is 2～5h.
The invention has the beneficial effects as follows:
The present invention applies one deck DyTb alloy-layer on sintered NdFeB magnet surface by the method for thermal spraying, then by heat treated mode, make Tb and the Dy of magnet surface spraying at high temperature by crystal boundary, diffuse into sintered magnet inside, can significantly improve the coercive force of sintered magnet, resultant effect has significant lifting than the coercive force that sprays separately Tb or Dy; Due to global content of rare earth scarcity, the content of heavy rare earth Tb is only 10% left and right of the content of Dy, and spray separately Dy metal, again can be more a lot of than the high volatility of Tb because of the volatility of Dy, more Dy will be attached on production equipment, the utilance of Dy metal reduces and can pollute production equipment and cause producing and can not carry out, and the DyTb alloy that adds a small amount of Tb formation in Dy metal had both solved the strong volatility problem of Dy, can not make again production only depend on the few heavy rare earth Tb of content, this is that the present invention is compared with the improvement of prior art maximum.Compared with carrying out crystal boundary DIFFUSION TREATMENT with the method such as other surface-coated, vacuum evaporation, by the method, heavy rare earth metal is sprayed directly into magnet surface, closely, the diffusion effect of Tb and Dy is good in contact; That this method has is simple to operate, efficiency is high, productive rate is large, the feature of energy savings, and magnet after treatment such as does not need to clean at the processing, and outward appearance is good, has high Practical significance.
On above-mentioned improved basis, the quality percentage composition that the present invention further selects Dy is at 60%～90% DyTb alloy.When the quality percentage composition of Dy is lower than 60% or higher than 90% time, the coercitive increase rate of magnet and separately spraying Tb or Dy quite.And when the DyTb alloy of the quality percentage composition of selecting Dy 60%～90%, both can be at the coercive force that effectively improves magnet, can reach again aforementioned " add DyTb alloy that a small amount of Tb forms and both solved the strong volatility problem of Dy in Dy metal, can not make again to produce only depend on the few heavy rare earth Tb of content " comprehensive like this gain effect simultaneously.This beneficial effect obtains the Data support in a large amount of production practices, and has good using value in the production of sintered NdFeB magnet, and can be cost-saving.And the principle that this phenomenon occurs, may be quality percentage composition based on Dy provided by the present invention more easily enters in magnet at the DyTb alloy of this proportioning of 60%～90%, and around crystal grain, has formed more perfect high coercivity layer.
Accompanying drawing explanation
Fig. 1 is the thermal spraying treatment device sketch relating in the present invention.
In accompanying drawing, the list of parts of each label representative is as follows:
1, thermic lance, 2, input, 3, dysprosium terbium alloy silk, 4, Ar air compressor, 5, ceramic wafer, 6, magnetic sheet, 7, Ar gas control valve, 8, stuffing box, 9, Ar gas input port.
Embodiment
Below principle of the present invention and feature are described, example, only for explaining the present invention, is not intended to limit scope of the present invention.
The sintered magnet that is subject to processing used in the present invention adopts known method to prepare.The device that sintered magnet is carried out to thermal spraying treatment can adopt thermal spraying treatment device as shown in Figure 1, comprises thermic lance 1, Ar air compressor 4, Ar gas control valve 7, stuffing box 8 and Ar gas input port 9.Wherein, the thermic lance 1 using in device is common arc pistol, in the interior vertical layout of stuffing box 8; The arranged just beneath magnetic sheet 6 of thermic lance 1, thermic lance 1 is 0.2m～1.0m with the distance of magnetic sheet 6; In addition, the outer layout of stuffing box 8 Ar air compressor 4 completes the circulation of Ar gas in casing; In stuffing box 8 casing top layout, there is Ar gas control valve 7, by controlling, from Ar gas input port 9, enter Ar gas in stuffing box 8 casings to maintain in casing pressure stable.
When thermic lance 1 is worked, at input 2 places inputs three-phase alternating currents, the fusing that heats up of dysprosium terbium alloy silk 3 moment under arcing, under the effect of compression Ar gas, high velocity jet is to the magnetic sheet 6 on ceramic wafer 5.The three-phase alternating current of inputting 380V, 50Hz during thermic lance work, power output can reach 20kW; Use is of a size of the dysprosium terbium alloy silk of φ 2～5mm, with crossing by the delivery rate of wire-feed motor control terbium or dysprosium silk; In stuffing box 8, be Ar gas protective atmosphere, by Ar control valve 7 and Ar air compressor 4, guarantee that casing pressure is basicly stable.
Magnetic sheet 5 is closely arranged at box house, improves quantity and the efficiency of processing magnetic sheet.Magnetic sheet 5 one sides have been carried out, after thermal spraying treatment, can overturning, then another side has been carried out to thermal spraying treatment.
In thermal spray process, need to select suitable delivery rate, thereby control the speed toward magnet surface thermal spraying DyTb alloy.Delivery rate is faster, and spraying rate is faster, and the processing time shortens, but the sprayed coating obtaining is coarse, homogeneity variation; Delivery rate is excessively slow, and spraying rate is slow, the fine and close homogeneous of coat obtaining, but productive rate reduces.
In the present embodiment; when use heat spraying method in sintered magnet surface-coated after DyTb alloy-layer; sintered magnet is put into vacuum sintering furnace; be set in 750～1000 ℃; more excellent is 800～950 ℃; in order to control the permeating speed and the volatilization that prevents Dy of Dy, under the Ar gas protective atmosphere condition of employing 5～20kPa, heat-treat.
If temperature is lower than 750 ℃ in vacuum sintering furnace, the Tb, Dy atom that is attached to sintered magnet surface to the diffusion velocity of grain boundary layer by slack-off, Tb, Dy atom can not enter sintered magnet inside effectively, thereby cause top layer Tb and Dy atomic concentration too high, center content is low does not even have entering of Tb and Dy atom; If temperature is higher than 1000 ℃, Tb or Dy atom can be diffused in crystal grain, make sintered magnet surface property variation simultaneously, cause the significantly reduction of remanent magnetism and maximum magnetic energy product.
If heat treatment time is lower than 2h, the Tb of thermal spraying on surface and Dy do not have sufficient time grain boundary diffusion to enter sintered magnet center, thereby cause sintered magnet top layer magnetic property apparently higher than center, magnet homogeneity variation makes sintered magnet entirety magnetic property promote not high simultaneously; If the processing time exceedes 72h, when being attached to after the Tb on sintered magnet surface and Dy run out of, (diffuse into magnet inside, or evaporation enters process chamber atmosphere), the rare earth element in sintered magnet can continue volatilization as rare earth elements such as Pr, Nd, thereby causes sintered magnet magnetic property variation.
Finally, after above-mentioned processing has been implemented to the stipulated time, stop heating, temperature in vacuum sintering furnace is reduced under 200 ℃; Restart afterwards heating, make temperature in vacuum sintering furnace be raised to 450～600 ℃, more excellent is 470～550 ℃; Processing time is 1～10h, and more excellent is 2～5h.Until above-mentioned heat treatment, implemented after the stipulated time, in vacuum sintering furnace, passed into Ar gas and be cooled to room temperature.
Embodiment 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%, the ratio of B-1%, vacuum melting furnace under inert gas environment completes cast, 1450 ℃ of pouring temperatures, chilling roller rotating speed is 60r/min, the about 0.3mm of flake thickness obtaining; Scale is through HD powder process, and airflow milling, makes the powder that particle mean size is 3.0 μ m; In the magnetic field of 15kOe, be orientated compressingly, make pressed compact; Pressed compact is put into the sintering furnace under Ar atmosphere, and 1070 ℃ of sintering 5h obtain green compact, and green compact are timeliness 5h at 500 ℃ of temperature, obtains sintering blank.By machine work, sintering blank is processed into the 50M magnet that is of a size of 40mm*20mm*4mm, is designated as M
0.
By 50M sintered magnet (40mm*20mm*4mm) dry processing after oil removing, pickling, activation and deionized water washing, sintered magnet is put into thermal spraying stuffing box with 20 * 10, at the thick DyTb alloy-layer that is 60% containing Dy ratio of sintered magnet surface spraying 20 μ m; After having sprayed one side, can use glove box to overturn to sintered magnet, at another side, spray the DyTb alloy-layer that 20 μ m are thick.Sintered magnet after thermal spraying treatment is placed in vacuum sintering furnace, at 900 ℃ of temperature, (pressure 10 under vacuum condition
-3～10
-4within the scope of Pa) process 24h, Ageing Treatment 5h at 500 ℃ afterwards, logical Ar is cooled to room temperature.Open vacuum-sintering furnace door, obtain sintered magnet M
1.Through Measurement and analysis, its performance is as shown in table 1.
By 50M sintered magnet (40mm*20mm*4mm) dry processing after oil removing, pickling, activation and deionized water washing, sintered magnet is put into thermal spraying stuffing box with 20 * 10, at the thick Tb metal level of sintered magnet surface spraying 20 μ m; After having sprayed one side, can use glove box to overturn to sintered magnet, at another side, spray the Tb metal level that 20 μ m are thick.Sintered magnet after thermal spraying treatment is placed in vacuum sintering furnace, at 900 ℃ of temperature, (pressure 10 under vacuum condition
-3～10
-4within the scope of Pa) process 24h, Ageing Treatment 5h at 500 ℃ afterwards, logical Ar is cooled to room temperature.Open vacuum-sintering furnace door, obtain sintered magnet M
2.Through Measurement and analysis, its performance is as shown in table 1.
Table 1M
1, M
2and M
0comparison of magnetic property
| Project | Density | Br | Hcj | (BH)max | Hk/iHc |
| Unit | （g/cm 3） | kGs | kOe | MGOe | - |
| M 0 | 7.56 | 14.31 | 15.02 | 49.66 | 0.97 |
| M 1 | 7.59 | 14.13 | 27.86 | 47.68 | 0.96 |
| M 2 | 7.58 | 14.12 | 26.16 | 47.58 | 0.95 |
Pass through M
1, M
0and M
2comparison of magnetic property, can find out, through heat treated M after thermal spraying on surface DyTb alloy-layer
1sintered magnet has been obtained good effect, and the coercive force of 50M rises to 27.86kOe from 15.02kOe, and coercive force is increased dramatically, and remanent magnetism, squareness and magnetic energy product reduce slightly; And the M of the same terms processing
2the coercive force of sintered magnet rises to 26.16kOe from 15.02kOe, and the amplitude that coercive force promotes is not as good as M
1magnet, this is new discovery of the present invention.Get the rear magnet surface of processing and core sample spot and do energy spectrum analysis (ICP-MS), result shows, M
1sintered magnet top layer Tb, Dy content increase respectively 0.8%, 0.5%, and center Tb, Dy content increase respectively 0.3%, 0.2%, show that Tb, Dy have permeated magnet completely; M
2sintered magnet top layer Tb content increases by 0.7%, and center Tb content difference 0.2%, shows that Tb has permeated magnet completely.More than analyze the recruitment of the Tb in the magnet that shows to spray DyTb alloy higher than the recruitment of Tb in a magnet of spray metal Tb, this is M of the present invention
1the larger reason of coercive force amplification of magnet.
Embodiment 2
Use is prepared 50M magnetic sheet with melting identical in embodiment 1, powder process, die mould, heat treatment and line cutting, spraying method.By 50M sintered magnet (40mm*20mm*4mm) dry processing after oil removing, pickling, activation and deionized water washing, sintered magnet is put into thermal spraying stuffing box with 20 * 10, at the thick DyTb alloy-layer that is 60% containing Dy ratio of sintered magnet surface spraying 20 μ m; After having sprayed one side, can use glove box to overturn to sintered magnet, at another side, spray the DyTb alloy-layer that 20 μ m are thick.Sintered magnet after thermal spraying treatment is placed in vacuum sintering furnace, at 900 ℃ of temperature, in the Ar atmosphere of 5kPa, processes 48h, Ageing Treatment 5h at 500 ℃ afterwards, logical Ar is cooled to room temperature.Open vacuum-sintering furnace door, obtain sintered magnet M
3.Its performance is as shown in table 2.
Table 2M
3, M
1and M
0comparison of magnetic property
| Project | Density | Br | Hcj | (BH)max | Hk/iHc |
| Unit | （g/cm 3） | kGs | kOe | MGOe | - |
| M 0 | 7.56 | 14.31 | 15.02 | 49.66 | 0.97 |
| M 1 | 7.59 | 14.13 | 27.86 | 47.68 | 0.95 |
| M 3 | 7.56 | 14.15 | 28.25 | 48.23 | 0.95 |
Pass through M
3and M
0comparison of magnetic property, can find out, through heat treated sintered magnet after thermal spraying on surface DyTb alloy-layer, obtained good effect, the coercive force of 50M rises to 28.25kOe from 15.02kOe, coercive force is increased dramatically, and remanent magnetism, squareness and magnetic energy product reduce slightly; And M
1compare, remanent magnetism, coercive force and magnetic energy product improve slightly, because Ar gas has limited the volatilization of rare earth element in high temperature lower magnet simultaneously, so although heat treatment time extends, sintered density is substantially constant.Get the rear magnet surface of processing and core sample spot and do energy spectrum analysis, result shows, M
3sintered magnet top layer Tb, Dy content increase respectively 0.7%, 0.4%, and center Tb, Dy content increase respectively 0.3%, 0.2%, show that Tb, Dy have permeated magnet completely; With M
1compare, surface and center Tb, Dy content difference reduce.
Embodiment 3
Use with implementing identical melting, powder process, die mould, heat treatment and wire cutting method in 1 and prepare 50M magnetic sheet.By 50M sintered magnet (40mm*20mm*4mm) dry processing after oil removing, pickling, activation and deionized water washing, sintered magnet is put into thermal spraying vacuum tank with 20 * 10, at the thick DyTb alloy-layer that is 80% containing Dy ratio of sintered magnet surface spraying 20 μ m; After having sprayed one side, sintered magnet is overturn, at another side, spray the same DyTb layer that 20 μ m are thick.Sintered magnet after thermal spraying treatment is placed in vacuum sintering furnace, at 880 ℃ of temperature, processes 24h, Ageing Treatment 5h at 500 ℃ afterwards, logical Ar gas is cooled to room temperature.Open vacuum-sintering furnace door, obtain magnet M
4.Through Measurement and analysis, its performance is as shown in table 3.
Use is prepared 50M magnetic sheet with melting identical in embodiment 1, powder process, die mould, heat treatment and wire cutting method.By 50M sintered magnet (40mm*20mm*4mm) dry processing after oil removing, pickling, activation and deionized water washing, sintered magnet is put into thermal spraying vacuum tank with 20 * 10, at the thick Dy metal level of sintered magnet surface spraying 20 μ m; After having sprayed one side, sintered magnet is overturn, at another side, spray the Dy metal level that 20 μ m are thick.Sintered magnet after thermal spraying treatment is placed in vacuum sintering furnace, at 880 ℃ of temperature, processes 24h, Ageing Treatment 5h at 500 ℃ afterwards, logical Ar gas is cooled to room temperature.Open vacuum-sintering furnace door, obtain magnet M
5.Through Measurement and analysis, its performance is as shown in table 3.
Table 3M
0, M
4and M
5comparison of magnetic property
| Project | Density | Br | Hcj | (BH)max | Hk/iHc |
| Unit | （g/cm 3） | kGs | kOe | MGOe | - |
| M 0 | 7.56 | 14.31 | 15.02 | 49.66 | 0.97 |
| M 4 | 7.55 | 14.18 | 24.88 | 47.35 | 0.97 |
| M 5 | 7.54 | 14.17 | 23.28 | 47.25 | 0.97 |
Pass through M
4, M
5and M
0comparison of magnetic property, can find out, through heat treated M after thermal spraying on surface DyTb
4sintered magnet has been obtained good effect, and the coercive force of 50M rises to 24.88kOe from 15.02kOe, and coercive force is increased dramatically, and remanent magnetism and magnetic energy product reduce slightly, and squareness is substantially unaffected.M
5the coercive force of sintered magnet rises to 23.28kOe from 15.02kOe, and the amplitude that coercive force promotes is not as good as M
4magnet, this is new discovery of the present invention.Get the rear magnet surface of processing and core sample spot and do energy spectrum analysis (ICP-MS), result shows, M
4sintered magnet top layer Tb, Dy content increase respectively 0.3%, 0.8%, and center Tb, Dy content increase respectively 0.1%, 0.3%, show that Tb, Dy have permeated magnet completely.M
5sintered magnet top layer Dy content increases by 0.9%, and center Dy content increases by 0.4%, shows that Dy has permeated magnet completely.More than analyze the M that shows to spray DyTb alloy
4the recruitment of Dy in magnet, although than the M of a spray metal Dy
5the amplification of the Dy of magnet is slightly low, but due to its infiltration that can introduce 0.1% metal Tb simultaneously, this is M of the present invention just
4the larger reason of coercive force amplification of magnet.
Embodiment 4
Use with implementing identical melting, powder process, die mould, heat treatment and wire cutting method in 1 and prepare 50M magnetic sheet.By 50M sintered magnet (40mm*20mm*4mm) dry processing after oil removing, pickling, activation and deionized water washing, sintered magnet is put into thermal spraying vacuum tank with 20 * 10, at the thick DyTb alloy-layer that is 80% containing Dy ratio of sintered magnet surface spraying 60 μ m; After having sprayed one side, sintered magnet is overturn, at another side, spray the DyTb layer that 60 μ m are thick.Sintered magnet after thermal spraying treatment is placed in vacuum sintering furnace, at 880 ℃ of temperature, processes 24h, Ageing Treatment 5h at 500 ℃ afterwards, logical Ar gas is cooled to room temperature.Open vacuum-sintering furnace door, obtain magnet M
6.Through Measurement and analysis, its performance is as shown in table 4.
Use with implementing identical melting, powder process, die mould, heat treatment and wire cutting method in 1 and prepare 50M magnetic sheet.By 50M sintered magnet (40mm*20mm*4mm) dry processing after oil removing, pickling, activation and deionized water washing, sintered magnet is put into thermal spraying vacuum tank with 20 * 10, at the thick Dy metal level of sintered magnet surface spraying 60 μ m; After having sprayed one side, sintered magnet is overturn, at another side, spray the Dy metal level that 60 μ m are thick.Sintered magnet after thermal spraying treatment is placed in vacuum sintering furnace, at 880 ℃ of temperature, processes 24h, Ageing Treatment 5h at 500 ℃ afterwards, logical Ar gas is cooled to room temperature.Open vacuum-sintering furnace door, obtain magnet M
7.Through Measurement and analysis, its performance is as shown in table 4.
Table 4M
0, M
6and M
7comparison of magnetic property
| Project | Density | Br | Hcj | (BH)max | Hk/iHc |
| Unit | （g/cm 3） | kGs | kOe | MGOe | - |
| M 0 | 7.56 | 14.31 | 15.02 | 49.66 | 0.97 |
| M 6 | 7.55 | 14.15 | 25.78 | 47.30 | 0.97 |
| M 7 | 7.54 | 14.13 | 24.18 | 47.23 | 0.97 |
Pass through M
6, M
7and M
0comparison of magnetic property, can find out, through heat treated M after thermal spraying on surface DyTb
6sintered magnet has been obtained good effect, and the coercive force of 50M rises to 25.78kOe from 15.02kOe, and coercive force is increased dramatically, and remanent magnetism and magnetic energy product reduce slightly, and squareness is substantially unaffected.M
7the coercive force of sintered magnet rises to 24.18kOe from 15.02kOe, and the amplitude that coercive force promotes is not as good as M
6magnet, this is new discovery of the present invention.Get the rear magnet surface of processing and core sample spot and do energy spectrum analysis (ICP-MS), result shows, M
6sintered magnet top layer Tb, Dy content increase respectively 0.4%, 0.9%, and center Tb, Dy content increase respectively 0.2%, 0.4%, show that Tb, Dy have permeated magnet completely.M
7sintered magnet top layer Dy content increases by 1.1%, and center Dy content increases by 0.6%, shows that Dy has permeated magnet completely.More than analyze the M that shows to spray DyTb alloy
6the recruitment of Dy in magnet, although than the M of a spray metal Dy
7the amplification of the Dy of magnet is slightly low, but due to its infiltration that can introduce 0.2% metal Tb simultaneously, this is M of the present invention just
6the larger reason of coercive force amplification of magnet.
Embodiment 5
Use with implementing identical melting, powder process, die mould, heat treatment and wire cutting method in 1 and prepare 50M magnetic sheet.By 50M sintered magnet (40mm*20mm*4mm) dry processing after oil removing, pickling, activation and deionized water washing, sintered magnet is put into thermal spraying vacuum tank with 20 * 10, at the thick DyTb alloy-layer that is 80% containing Dy ratio of sintered magnet surface spraying 100 μ m; After having sprayed one side, sintered magnet is overturn, at another side, spray the DyTb layer that 100 μ m are thick.Sintered magnet after thermal spraying treatment is placed in vacuum sintering furnace, at 880 ℃ of temperature, processes 24h, Ageing Treatment 5h at 500 ℃ afterwards, logical Ar gas is cooled to room temperature.Open vacuum-sintering furnace door, obtain magnet M
8.Through Measurement and analysis, its performance is as shown in table 5.
Use with implementing identical melting, powder process, die mould, heat treatment and wire cutting method in 1 and prepare 50M magnetic sheet.By 50M sintered magnet (40mm*20mm*4mm) dry processing after oil removing, pickling, activation and deionized water washing, sintered magnet is put into thermal spraying vacuum tank with 20 * 10, at the thick Dy metal level of sintered magnet surface spraying 100 μ m; After having sprayed one side, sintered magnet is overturn, at another side, spray the Dy metal level that 100 μ m are thick.Sintered magnet after thermal spraying treatment is placed in vacuum sintering furnace, at 880 ℃ of temperature, processes 24h, Ageing Treatment 5h at 500 ℃ afterwards, logical Ar gas is cooled to room temperature.Open vacuum-sintering furnace door, obtain magnet M
9.Through Measurement and analysis, its performance is as shown in table 5.
Table 5M
0, M
8and M
9comparison of magnetic property
| Project | Density | Br | Hcj | (BH)max | Hk/iHc |
| Unit | （g/cm 3） | kGs | kOe | MGOe | - |
| M 0 | 7.56 | 14.31 | 15.02 | 49.66 | 0.97 |
| M 8 | 7.55 | 14.14 | 25.98 | 47.28 | 0.97 |
| M 9 | 7.54 | 14.11 | 24.38 | 47.20 | 0.97 |
Pass through M
8, M
9and M
0comparison of magnetic property, can find out, through heat treated M after thermal spraying on surface DyTb
8sintered magnet has been obtained good effect, and the coercive force of 50M rises to 25.98kOe from 15.02kOe, and coercive force is increased dramatically, and remanent magnetism and magnetic energy product reduce slightly, and squareness is substantially unaffected.M
9the coercive force of sintered magnet rises to 24.38kOe from 15.02kOe, and the amplitude that coercive force promotes is not as good as M
8magnet, this is new discovery of the present invention.Get the rear magnet surface of processing and core sample spot and do energy spectrum analysis (ICP-MS), result shows, M
8sintered magnet top layer Tb, Dy content increase respectively 0.4%, 0.9%, and center Tb, Dy content increase respectively 0.2%, 0.5%, show that Tb, Dy have permeated magnet completely.M
9sintered magnet top layer Dy content increases by 1.1%, and center Dy content increases by 0.6%, shows that Dy has permeated magnet completely.More than analyze the M that shows to spray DyTb alloy
8the recruitment of Dy in magnet, although than the M of a spray metal Dy
9the amplification of the Dy of magnet is slightly low, but due to its infiltration that can introduce 0.2% metal Tb simultaneously, this is M of the present invention just
8the larger reason of coercive force amplification of magnet.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (6)
1. a preparation method for R-Fe-B based sintered magnet, comprises the following steps:
1) prepare R
1-Fe-B-M sintered magnet, wherein, R
1be selected from one or more in Nd, Pr, Dy, Tb, its total amount is 27wt%～32wt%; M is selected from one or more in Ti, V, Cr, Mn, Co, Ni, Ga, Ca, Cu, Zn, Si, Al, Mg, Zr, Nb, Hf, Ta, W, Mo, and its total amount is 0～3wt%; B total amount is 0.8wt%～1.2wt%; Surplus is Fe;
2) sintered magnet step 1) being obtained carries out oil removing, pickling, activation and washed with de-ionized water processing;
3) by step 2) in sintered magnet after cleaning put into airtight container and make sintered magnet in circulation A r gas protective atmosphere, on sintered magnet surface, using heat spraying method to apply a layer thickness is the DyTb alloy-layer that the quality percentage composition of the Dy of 10～200 μ m is 60%～90%;
4) sintered magnet after treatment step 3) is put into vacuum sintering furnace, 750～1000 ℃ of heat treatment 2～72h, in vacuum sintering furnace, vacuum degree control is 10
-2～10
-5the Ar gas protective atmosphere that adopts 5～20kPa in Pa or vacuum sintering furnace, makes metal Tb and Dy diffuse into sintered magnet inside by crystal boundary;
5) by sintered magnet after treatment step 4) at 450～600 ℃ of Ageing Treatment 1～10h, obtain R-Fe-B based sintered magnet.
2. preparation method according to claim 1, is characterized in that: in described step 3), on sintered magnet surface, using the thickness of the described DyTb alloy-layer of heat spraying method coating is 20～100 μ m.
3. preparation method according to claim 1, it is characterized in that: in described step 3), described airtight container is stuffing box, and Ar gas input port and Ar gas control valve are set on the casing of described stuffing box, casing arranges Ar air compressor outward, basicly stable for maintaining box house pressure.
4. preparation method according to claim 1, it is characterized in that: in described step 3), described sintered magnet was closely arranged in stuffing box inside before thermal spraying, sintered magnet one side is being carried out overturning after thermal spraying, then another side is carried out to thermal spraying treatment.
5. according to the arbitrary described preparation method of claim 1 to 4, it is characterized in that: in described step 4), in vacuum sintering furnace, temperature is 820～900 ℃, and heat treatment time is 5～72h, and in vacuum sintering furnace, vacuum degree is 10
-3～10
-4pa, or the interior Ar gas protective atmosphere that adopts 5～10kPa of vacuum sintering furnace.
6. according to the arbitrary described preparation method of claim 1 to 4, it is characterized in that: in described step 5), described aging temperature is 470～550 ℃, and the processing time is 2～5h.
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| JP7342280B2 (en) | 2020-02-26 | 2023-09-11 | フージャン チャンティン ゴールデン ドラゴン レア－アース カンパニー リミテッド | Neodymium iron boron magnet materials, raw material compositions, manufacturing methods, and applications |
| KR102631761B1 (en) * | 2020-02-26 | 2024-01-31 | 푸젠 골든 드래곤 레어-어스 컴퍼니 리미티드 | Neodymium iron boron magnetic material, raw material composition, manufacturing method and application |
| CN111292952A (en) * | 2020-03-03 | 2020-06-16 | 浙江英洛华磁业有限公司 | Method for improving coercive force of neodymium iron boron magnet |
| CN112908666A (en) * | 2020-03-27 | 2021-06-04 | 北京京磁电工科技有限公司 | Method for attaching heavy rare earth on surface of sintered neodymium iron boron |
| CN112908666B (en) * | 2020-03-27 | 2022-08-05 | 北京京磁电工科技有限公司 | Method for attaching heavy rare earth on surface of sintered neodymium iron boron |
| CN112614690A (en) * | 2020-12-31 | 2021-04-06 | 宁波松科磁材有限公司 | Preparation method of high-performance permanent magnet |
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