CN108335898A - A kind of sintered NdFeB sheet magnet steel temperature stability of improving oozes dysprosium technique - Google Patents
A kind of sintered NdFeB sheet magnet steel temperature stability of improving oozes dysprosium technique Download PDFInfo
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- CN108335898A CN108335898A CN201810110441.5A CN201810110441A CN108335898A CN 108335898 A CN108335898 A CN 108335898A CN 201810110441 A CN201810110441 A CN 201810110441A CN 108335898 A CN108335898 A CN 108335898A
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- magnet steel
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
Abstract
Dysprosium technique, including following operating procedure are oozed the invention discloses a kind of raising sintered NdFeB sheet magnet steel temperature stability:Neodymium iron boron blank after sintering timeliness is processed into black-film by step 1, is sintered in the neodymium iron boron blank after timeliness, rare earth total content is not less than 31wt%;Sintered NdFeB black-film in step 1 is removed surface and oil contaminant by step 2, and step 3 selects technical grade Dy-Fe alloy or pure dysprosium metal, its surface is polished totally using steel wire rotary brush;The sintered NdFeB black-film layered putting obtained in step 2 between dysprosium or Dy-Fe alloy, is then placed into vacuum heat treatment furnace at two pieces and carries out high temperature and Low Temperature Heat Treatment by step 4;At the end of heat treatment twice in step 5, step 4, it is filled with argon gas cooling respectively;Step 6 takes out black-film, detects magnetic property and heat subtracts magnetic property.The present invention provides ooze dysprosium technique, grain boundary decision processing cost can be reduced, increase heavy rare earth element diffusion depth, improve magnet steel temperature stability.
Description
Technical field
The present invention relates to rare-earth permanent-magnet material technical field, more particularly to a kind of raising sintered NdFeB sheet magnet steel temperature
Stability oozes dysprosium technique.
Background technology
Since last century the eighties come out, sintered NdFeB is widely used in information with its excellent magnetic property and deposits
The fields such as storage, traffic, medical treatment, new energy.A series of resource and environment problems for consuming and occurring in particular with fossil fuels,
The green traffics tool such as hybrid vehicle, pure electric automobile has been a great deal of attention.Among these, sintered NdFeB magnetic
Steel has played the effect that can not be substituted in terms of energy conversion.However, the motor work of hybrid vehicle or pure electric automobile
Make nearly 200 DEG C of environment, coercivity should be greater than 8kOe under working condition, and respective chamber/chambers temperature coercivity should at least reach 30kOe.This for
General room temperature coercivity only has for the pure ternary sintered NdFeB of 12kOe, how to improve the temperature stability under hot environment,
It is a no small challenge.
To solve this problem, usual way is that the heavy rare earth elements such as Dy/Tb are added to improve Nd2Fe14B main phases
Magnetocrystalline anisotropy field HA increases magnet steel stability in a high temperauture environment to improve intrinsic coercivity Hcj.But due to adding
The heavy rare earth elements such as the Dy/Tb added form anti-ferromagnetism with Fe elements and couple, and cause magnet steel remanent magnetism to decline serious.It ground in recent years
Study carefully the pairing technology for gold of development, i.e., the heavy rare earth elements such as Dy/Tb are added in fusion process about subsequent process, it can be dilute to avoid weight
Soil is directly entered main phase, to reduce the influence to remanent magnetism.But under the high temperature sintering stage, 1000-1100 DEG C of sintering temperature still
It has part heavy rare earth element and enters main phase, to reduce magnet steel remanent magnetism.
Recently, multiple research teams report is attached to magnet steel by the alloyed powder of the heavy rare earth elements such as Dy/Tb or compound
Surface, the grain boundary decision technology being then heat-treated.Compared with the technology of tradition addition heavy rare earth, grain boundary decision technology can be with
Heavy rare earth is set to be enriched in crystal boundary without entering main phase, in the case where reducing heavy rare earth usage amount by heat treatment temperature appropriate
Achieve the purpose that Grain-Boundary Phase modification and the hardening of crystal boundary epitaxial layer, improve intrinsic coercivity Hcj, and then the temperature for improving magnet steel is stablized
Property.
Currently used crystal boundary, which expands processing method, to be had:Magnetron sputtering method, cladding process, vapour deposition method, electrophoresis etc..More than although
Several method achieves the promotion of intrinsic coercivity on thin slice magnet steel, but there are still some yet unresolved issues:(1) utilize
The method cost of equipment that the heavy rare earth elements such as Dy/Tb are attached to magnet steel surface by magnetron sputtering is excessively high, and is susceptible to molten hole
The defects of;(2) the fluoride of the heavy rare earth elements such as Dy/Tb is typically chosen in cladding process as diffusion source, in diffusion process, fluorine
Element can also enter inside magnet steel, directly affect the mechanical property of magnet steel;(3) the heavy rare earth such as Dy/Tb are generally used in vapour deposition method
The alloys of the formation such as element and transition metal Cu, Co, Al is diffused, the ingot casting melting of the alloy cpd as diffusion source
And processing need to expend no small manpower and materials;(4) reported many researchs obtain on the thin slice magnet steel of 3mm left and right thicknesses
Good effect, but for thickness 5mm or more sheet magnet steel, have more existing diffusion depth not enough, the heavy rare earth member such as Dy/Tb
Phenomena such as element is unevenly distributed, demagnetization curve rectangularity is poor, and this directly affects the temperature stability of magnet steel.
Invention content
In view of the deficiencies of the prior art and defect, the present invention provides a kind of raising sintered NdFeB sheet magnet steel temperature is steady
Dysprosium technique qualitatively is oozed, it is steady that grain boundary decision processing cost, increase heavy rare earth element diffusion depth, raising magnet steel temperature can be reduced
It is qualitative.
To achieve the above object, the present invention provides following technical scheme.
A kind of sintered NdFeB sheet magnet steel temperature stability of improving oozes dysprosium technique, including following operating procedure:
Step 1, the black-film that the neodymium iron boron blank after sintering timeliness is processed into required specification;Pending sintered NdFeB magnet steel
Rare earth total content is not less than 31wt%;The increase of rare earth total content will provide continuously rich neodymium phase for subsequent grain boundary decision
Crystal boundary is attached to the heavy rare earth elements such as the Dy/Tb on magnet steel surface and enters magnet steel surface in high-temperature heat treatment process, due to continuous
The constantly presence of richness neodymium Grain-Boundary Phase, can greatly increase the diffusion range and depth of heavy rare earth element, overcome general crystal boundary
Diffusion technique is only applicable to the shortcomings that 3mm left and right thickness magnet steel;
Sintered NdFeB black-film in step 1 is put into degreasing tank and removes surface and oil contaminant by step 2, then clear with deionized water
It washes, is subsequently placed into progress pickling 30-90s in the dilute hydrochloric acid of a concentration of 1.0-3.0mol/L, then cleaned through deionized water, Zhi Houchao
Sonicated 60-120s is cleaned up after being finally passivated 5-20s in chromic acid solution with deionized water, and high wind rapid draing waits for
With;
Step 3 selects technical grade Dy-Fe alloy or pure dysprosium metal, and Dy-Fe alloy or pure dysprosium surface are polished using steel wire rotary brush and done
Only;
Step 4 between dysprosium or Dy-Fe alloy, then puts the sintered NdFeB black-film layered putting obtained in step 2 at two pieces
It is placed in vacuum heat treatment furnace and carries out high temperature and Low Temperature Heat Treatment;
At the end of heat treatment twice in step 5, step 4, it is filled with argon gas of the purity not less than 99.99% respectively and cools down;
Step 6 after the completion of waiting for Low Temperature Heat Treatment, takes out black-film, detects magnetic property and heat subtracts magnetic property.
Further, in step 1, neodymium iron boron blank is ground using end face or line cutting technology is processed into the black of required specification
Piece, the length of differently- oriented directivity is 5-10mm in black-film specification.
Further, in step 2, the black-film after cleaning up need to pass through chromic acid solution Passivation Treatment, to prevent from operating
Rustization occurs in journey, is more suitable for factory's mass operation.
Further, in step 3, the diffusion source for DIFFUSION TREATMENT is production pure dysprosium metal or Dy-Fe alloy, this
Step overcomes the disadvantage that diffusion source processing cost is excessively high in certain vapor deposition diffusion techniques, is conducive to realize batch production batch rapidly
Production.
Further, in step 4, high-temperature heat treatment temperature is 600-1000 DEG C, and the time is 5-30 hour, when heat treatment
Vacuum degree is in 1x10-5Between Pa -10Pa.
Further, in step 4, the temperature of Low Temperature Heat Treatment is 400-600 DEG C, and the time is 1-5 hour.
Beneficial effects of the present invention are:The present invention's oozes dysprosium technique compared with the prior art, and it is more to overcome its diffusion technique
The shortcomings that dysprosium being oozed suitable for 3mm or so thin slice magnet steel surface.By improving the rare earth total content in matrix magnet steel, rare earth total content
Increase continuously rich neodymium phase crystal boundary will be provided for subsequent grain boundary decision, it is dilute to be attached to the weight such as the Dy/Tb on magnet steel surface
Earth elements enter magnet steel surface in high-temperature heat treatment process, can be great due to the presence of successive rich neodymium Grain-Boundary Phase
The diffusion range and depth for increasing heavy rare earth element, overcome general grain boundary decision technology and are only applicable to 3mm left and right thickness magnet steel
The shortcomings that, 5mm or more sheets magnet steel is realized in heavy rare earth element diffusion depth, distribution consistency degree and demagnetization curve rectangularity
On breakthrough.Meanwhile the present invention is especially focused on the realizability in batch production batch production, using what is generally selected in industry
Dysprosium or Dy-Fe alloy are avoided to melting/processing request of diffusion source harshness in prior art technology, greatly as diffusion source
The mass production cost that grain boundary decision handles this technique is reduced, there is very strong practical and operability, be suitble to looking forward to
Industry is promoted the use of.
Description of the drawings
Fig. 1 is the magnetic property curve graph of magnet steel before being handled in the embodiment of the present invention 1
Fig. 2 is the magnetic property curve graph of magnet steel after being handled in the embodiment of the present invention 1
Specific implementation mode
It is further illustrated to of the invention in conjunction with attached drawing.
Referring to Fig. 1 to Fig. 2, embodiment 1
The formula components are taken to be(PrNdDyTb)32.5TM0.5FebalB1Sintered NdFeB blank carry out end face mill, wire cutting etc. adds
Work processing obtains the finished product black-film that specification is 32x16x6.5mm;
Sintered NdFeB black-film is put into degreasing tank and removes surface and oil contaminant, is then cleaned with deionized water, concentration is subsequently placed into
It to carry out pickling 60s in the dilute hydrochloric acid of 2.5mol/L, then cleans through deionized water, later ultrasonication 100s, finally in chromium
It is cleaned up with deionized water after being passivated 8s in acid solution, high wind rapid draing is for use;
By production Dy80Fe20Using linear cutter at the thin slice that thickness is 3mm, sheet surface is carried out alloy with steel wire rotary brush
Polishing, removes the oxide skin on surface;
The black-film processed and diffusion source are placed in molybdenum box, is put into later in vacuum heat treatment furnace and carries out 900 degree of high temperature
15 hours be heat-treated, at the end of be filled with purity not less than 99.99% argon gas cool down;
480 degree of black-film low temperature after high-temperature process is heat-treated for 3 hours, it is cold not less than 99.99% argon gas to be filled with purity later
But.
Treated Nd-Fe-B magnet steel is subjected to magnetism testing and heat subtracts magnetic tester, it is as of the invention after the assay was approved
The sintered NdFeB magnet steel that the temperature stability arrived improves
Table 1 is the front and back sintered NdFeB magnet steel magnetism testing result of diffusion
Table 2 is that the front and back sintered NdFeB magnet steel magnetic heat of diffusion subtracts magnetic survey test result
Embodiment 2
The formula components are taken to be(PrNdDyTb)34.5TM0.5FebalB1Sintered NdFeB blank carry out end face mill, wire cutting etc. adds
Work processing obtains the finished product black-film that specification is 32x16x8mm;
Sintered NdFeB black-film is put into degreasing tank and removes surface and oil contaminant, is then cleaned with deionized water, concentration is subsequently placed into
It to carry out pickling 80s in the dilute hydrochloric acid of 2.0mol/L, then cleans through deionized water, later ultrasonication 120s, finally in chromium
It is cleaned up with deionized water after being passivated 15s in acid solution, high wind rapid draing is for use;
By production Dy70Fe30Alloy using linear cutter at thickness be 10mm bulk, bulk surface steel wire rotary brush into
Row polishing, removes the oxide skin on surface;
The black-film processed and diffusion source are placed in molybdenum box, is put into later in vacuum heat treatment furnace and carries out 950 degree of high temperature
20 hours be heat-treated, at the end of be filled with purity not less than 99.99% argon gas cool down;
550 degree of black-film low temperature after high-temperature process is heat-treated for 3 hours, it is cold not less than 99.99% argon gas to be filled with purity later
But.
Treated Nd-Fe-B magnet steel is subjected to magnetism testing and heat subtracts magnetic tester, it is as of the invention after the assay was approved
The sintered NdFeB magnet steel that the temperature stability arrived improves.
Table 3 is the front and back sintered NdFeB magnet steel magnetism testing result of diffusion
Table 4 is that the front and back sintered NdFeB magnet steel magnetic heat of diffusion subtracts magnetic survey test result
From table 1, table 2, table 3, table 4 data comparison in it can be found that method using the present invention carry out treated sintering neodymium
Iron boron magnet steel sheet, under the premise of intrinsic coercivity H j is obviously improved, squareness deteriorates there is no apparent, meanwhile, remanent magnetism
Reduction amplitude it is also very limited.This explanation, it is set forth in the present invention ooze dysprosium technique by improve matrix magnet steel in rare earth it is total
The increase of content, rare earth total content will provide continuously rich neodymium phase crystal boundary for subsequent grain boundary decision, be attached to magnet steel table
The heavy rare earth elements such as the Dy/Tb in face enter magnet steel surface in high-temperature heat treatment process, due to successive rich neodymium Grain-Boundary Phase
In the presence of can greatly increase the diffusion range and depth of heavy rare earth element, overcome general grain boundary decision technology and be only applicable to
The shortcomings that 3mm left and right thickness magnet steel, realize 5mm or more sheets magnet steel heavy rare earth element diffusion depth, distribution consistency degree with
And the breakthrough on demagnetization curve rectangularity.Meanwhile the present invention is especially focused on the realizability in batch production batch production, uses
The dysprosium or Dy-Fe alloy generally selected in industry avoid the melting to diffusion source harshness in prior art technology as diffusion source
And processing request, greatly reduce the mass production cost that grain boundary decision handles this technique, have it is very strong practical and
Operability is suitble to promote the use of in enterprise.
The above, the only preferable embodiment of this invention implementation result, this invention should not be limited by the examples, all
It is the professional technician for being familiar with neodymium iron boron industry, some can be all subject to according to the technical principle of this invention and improves and repaiies
Decorations, it is noted that the improvement and modification that every principle according to this invention is made belong in the covering scope of this patent.
Claims (5)
1. a kind of raising sintered NdFeB sheet magnet steel temperature stability oozes dysprosium technique, it is characterised in that:Including operating as follows
Step:
Step 1, the black-film that the neodymium iron boron blank after sintering timeliness is processed into required specification, the neodymium iron boron blank being sintered after timeliness
In, rare earth total content is not less than 31wt%;
Sintered NdFeB black-film in step 1 is put into degreasing tank and removes surface and oil contaminant by step 2, then clear with deionized water
It washes, is subsequently placed into progress pickling 30-90s in the dilute hydrochloric acid of a concentration of 1.0-3.0mol/L, then cleaned through deionized water, Zhi Houchao
Sonicated 60-120s is cleaned up after being finally passivated 5-20s in chromic acid solution with deionized water, and high wind rapid draing waits for
With;
Step 3 selects technical grade Dy-Fe alloy or pure dysprosium metal, and Dy-Fe alloy or pure dysprosium surface are polished using steel wire rotary brush and done
Only;
Step 4 between dysprosium or Dy-Fe alloy, then puts the sintered NdFeB black-film layered putting obtained in step 2 at two pieces
It is placed in vacuum heat treatment furnace and carries out high temperature and Low Temperature Heat Treatment;
At the end of heat treatment twice in step 5, step 4, it is filled with argon gas of the purity not less than 99.99% respectively and cools down;
Step 6 after the completion of waiting for Low Temperature Heat Treatment, takes out black-film, detects magnetic property and heat subtracts magnetic property.
2. a kind of raising sintered NdFeB sheet magnet steel temperature stability according to claim 1 oozes dysprosium technique, spy
Sign is:In step 1, neodymium iron boron blank is processed into the black-film of required specification, black-film specification using end face mill or line cutting technology
The length of middle differently- oriented directivity is 5-10mm.
3. a kind of raising sintered NdFeB sheet magnet steel temperature stability according to claim 1 oozes dysprosium technique, spy
Sign is:In step 2, the black-film after cleaning up need to pass through chromic acid solution Passivation Treatment, to prevent from becoming rusty in operating process
Change.
4. a kind of raising sintered NdFeB sheet magnet steel temperature stability according to claim 1 oozes dysprosium technique, spy
Sign is:In step 4, high-temperature heat treatment temperature is 600-1000 DEG C, and the time is 5-30 hour, and vacuum degree exists when heat treatment
1x10-5Between Pa -10Pa.
5. a kind of raising sintered NdFeB sheet magnet steel temperature stability according to claim 1 oozes dysprosium technique, spy
Sign is:In step 4, the temperature of Low Temperature Heat Treatment is 400-600 DEG C, and the time is 1-5 hour.
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Cited By (4)
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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 |
CN112712954A (en) * | 2020-12-23 | 2021-04-27 | 安徽大地熊新材料股份有限公司 | Preparation method of sintered neodymium-iron-boron magnet |
CN112820529A (en) * | 2020-12-31 | 2021-05-18 | 宁波松科磁材有限公司 | Preparation method of high-performance sintered neodymium iron boron |
CN113270241A (en) * | 2020-09-16 | 2021-08-17 | 江西理工大学 | Neodymium-iron-boron magnet and preparation method thereof |
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