CN108511179A - A kind of method that hot isostatic pressing low-temperature sintering prepares high magnetic sintered NdFeB - Google Patents
A kind of method that hot isostatic pressing low-temperature sintering prepares high magnetic sintered NdFeB Download PDFInfo
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 58
- 238000009766 low-temperature sintering Methods 0.000 title claims abstract description 22
- 238000001513 hot isostatic pressing Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 23
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011521 glass Substances 0.000 claims abstract description 20
- 238000009792 diffusion process Methods 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 13
- 238000000576 coating method Methods 0.000 claims abstract description 12
- -1 rare earth compound Chemical class 0.000 claims abstract description 12
- 238000007789 sealing Methods 0.000 claims abstract description 9
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005496 tempering Methods 0.000 claims abstract description 6
- 229910016468 DyF3 Inorganic materials 0.000 claims abstract description 5
- 239000006247 magnetic powder Substances 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000010583 slow cooling Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims 3
- 150000002085 enols Chemical class 0.000 claims 1
- 238000007710 freezing Methods 0.000 claims 1
- 230000008014 freezing Effects 0.000 claims 1
- 150000002910 rare earth metals Chemical class 0.000 abstract description 7
- 238000000280 densification Methods 0.000 abstract description 6
- 239000000696 magnetic material Substances 0.000 abstract description 4
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000007670 refining Methods 0.000 abstract 1
- 230000005389 magnetism Effects 0.000 description 5
- 239000011247 coating layer Substances 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000005347 demagnetization Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005324 grain boundary diffusion Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- 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
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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
- H01F41/0266—Moulding; Pressing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/241—Chemical after-treatment on the surface
- B22F2003/242—Coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
A kind of method that hot isostatic pressing low-temperature sintering prepares high magnetic sintered NdFeB, belongs to rareearth magnetic material technical field.Sintered NdFeB magnetic powder is carried out half densification sintering by the present invention, and consistency is 85%~95%；The suspension containing heavy rare earth compound that viscosity is 100~500mpa.s is coated in around half densification sintering neodymium iron boron again, vacuum glass tube sealing is carried out again, using 700~900 DEG C of low-temperature sinterings of hot isostatic pressing, 400~500 DEG C of tempering, the high magnetic Sintered NdFeB magnet of high density is prepared.Dy2S3、Dy2O3、Tb2O3、DyF3Or DyH3There are preferable adhesive force between equal coatings and half dense sintering neodymium iron boron magnetic body, during hot isostatic pressing low-temperature sintering, heavy rare earth element is diffused along crystal boundary and hole, under gas pressure in all directions, diffusion rate faster, is effectively improved diffusion depth and diffusion uniformity；Meanwhile effectively increasing the sintered density of magnet, refining grain size.
Description
Technical field
The invention belongs to rareearth magnetic material technical fields, provide a kind of high magnetic burning of hot isostatic pressing low-temperature sintering preparation
The method for tying neodymium iron boron.
Background technology
Sintered Nd-Fe-B permanent magnetic material is third generation permanent magnet, is invented in nineteen eighty-three Japanese scholars.Since it is with pole
High coercivity and magnetic energy product and be referred to as " magnetic king ".It is widely used in aerospace, auto industry, electronic apparatus, Medical treatment device
Tool, energy-saving electric machine, new energy, field of wind power generation are with fastest developing speed, permanent magnetism materials that market prospects are best in the world today
Material.NdFeB material has high energy product, high-coercive force, high-energy density, high performance-price ratio and good mechanical property etc. prominent
Advantage acts as important role in high-technology field.Worsening shortages with Global Oil resource and a large amount of combustions
Heavy environmental pollution caused by petrol car exhaust emissions so that the exploitation and use of energy-saving and environment-friendly new-energy automobile have attracted much attention
And quickly grow, this brings new developing direction without the development suspected of high performance sintered Nd-Fe-B permanent-magnet materials.
Currently, the remanent magnetism B of Sintered Nd-Fe-B MagnetrWith maximum magnetic energy product (BH)maxActual value have been approached it
Theoretical value.However, the coercivity H of magnetcj(μ0Hc~1.2T) it is relatively low, the 10~20% of theoretical value are only reached, it is serious to limit
The further development of Sintered Nd-Fe-B Magnet；Meanwhile the Curie temperature T of Sintered Nd-Fe-B MagnetcIt is relatively low, temperature
It is poor to spend stability, under high temperature environment, apparent demagnetization phenomenon occurs for Sintered Nd-Fe-B Magnet, and operating temperature is usual
Less than 100 DEG C, the application in fields such as high-temperature electric machines is limited by very large.Therefore, how to improve the coercivity of magnet at
The major issue of rareearth magnetic material industry.
In order to obtain the neodymium iron boron magnetic body of high-coercive force, forefathers had done many researchs.Currently, common method is in magnetic
Heavy rare earth element Dy and Tb are added in body, and common heavy rare earth additive is Dy2O3、Tb2O3、DyF3、DyH3Deng.But due to
Heavy rare earth resource is limited, how to reduce the usage amount of heavy rare earth element and is particularly important.It can be maximum using grain boundary decision technology
The heavy rare earth such as heavy rare earth Dy, Tb are saved to limit, magnet coercivity can be increased substantially and do not lose remanent magnetism, but due to magnetic
The limitation of body surface face coating thickness and diffusion depth, it is desirable that magnet size is narrow.Therefore, the expansion of grain boundary decision magnet how is improved
It is the emphasis studied at present to dissipate thickness and diffusion uniformity.
Using the lower rate that can accelerate element grain boundary decision of the gas pressure effect of hot isostatic pressing technique in all directions
And diffusion depth, the limited obstacle of current grain boundary decision thickness and uniformity is broken through, to improve the thickness of sample of grain boundary decision.
In addition, carrying out grain boundary decision using half fine and close Sintered NdFeB magnet, under the action of gas pressure, half fine and close magnet is more
Using alloying element grain boundary diffusion, to optimize crystal boundary, the coercivity of magnet is improved.
Invention content
The purpose of the present invention is to provide a kind of method that hot isostatic pressing low-temperature sintering prepares high magnetic sintered NdFeB,
Coercivity, sintered density, remanent magnetism, maximum magnetic energy product and thickness of sample etc. have all reached satisfactory effect.
In order to obtain above-mentioned Sintered NdFeB magnet, the present invention is as follows：
(1) NdFeB magnetic powder is subjected to orientation die mould under the magnetic field of 1.2~2.0T；The green compact that die mould is completed is put into very
Half dense sintering of vacuum is carried out in empty sintering furnace, sintering temperature is 850~950 DEG C, and soaking time is 1~3h, obtains half densification
Sintered NdFeB sample；
(2) suspension containing heavy rare earth compound is prepared, viscosity is 100~500mpa.s, by suspension in glove box
Coated in half fine and close sintered neodymium iron boron material surface, it is then placed in vacuum drying chamber and is dried in vacuo, at 35~45 DEG C
Dry 30~60min, obtains half dense sintering neodymium iron boron of the coating containing heavy rare earth compound；
(3) the half dense sintering neodymium iron boron containing coating in step (2) is put in a glass tube, then vacuum is carried out to glass tube
Tube sealing, vacuum degree is up to 10-2~10-3Pa obtains the sample of vacuum glass tube sealing；
(4) sample of vacuum glass tube sealing in step (4) is placed in hot isostatic press carry out hot isostatic pressing low-temperature sintering,
Tempering, sintering temperature are 700~900 DEG C, keep the temperature 0.5~1.5h, then through 400~500 DEG C of 1~3h of tempering, diffusion is made in slow cooling
Uniform Sintered NdFeB magnet.Wherein, using high-purity argon gas as applying pressurised gas, pressure is 10~100MPa.
Further, the consistency of half fine and close sintered NdFeB sample described in step (1) is 85%~95%.
Further, the solvent of the suspension of heavy rare earth compound described in step (2) is ethyl alcohol, ethylene glycol, acetone, third
One or more mixed liquors in glycol or polyvinyl alcohol.
Further, the heavy rare earth compound described in step (2) is Dy2S3、Dy2O3、Tb2O3、DyF3Or DyH3In
It is one or more kinds of.
Further, the thickness of heavy rare earth compound coating described in step (2) is 0.5~2mm.
Further, the softening temperature of glass tube described in step (3) is 450~650 DEG C.
Further, low-temperature sintering temperature described in step (4) is 700~900 DEG C.
Advantages of the present invention：
1, using on solvent of the sintered NdFeB magnetic property without influence, Dy is obtained2S3、Dy2O3、Tb2O3、DyF3Or DyH3Deng
There are preferable adhesive force between coating and neodymium iron boron magnetic body, can reduce destruction of the subsequent operation to coating.
2, during half fine and close Sintered NdFeB magnet hot isostatic pressing low-temperature sintering, grain boundary decision is directly carried out, is had
Conducive to the diffusion rate of heavy rare earth element is accelerated, the diffusion depth and diffusion uniformity of heavy rare earth element are improved, thickness of sample can
Up to 1.5cm.
3, use softening temperature for 450~650 DEG C of glass evacuated tube sealing, in sintering process, glass is in molten state packet
The step of overlaying on the surface of half compactness magnet, form one layer of glass bag, saving the individually jackets such as processing heat, simple for process, behaviour
Facilitate.
4, using half fine and close neodymium iron boron magnetic body of hot isostatic pressing technique low-temperature sintering, one side sintered density can reach
7.5g/cm3More than, crystallite dimension has effectively on the other hand been refined, has been conducive to the coercivity and sintered density that improve magnet.
5, high magnetic neodymium iron boron magnetic body has that diffusion depth is big, Grain-Boundary Phase is evenly distributed, sharpness of border, coercivity height etc. are excellent
Point.
Specific implementation mode
Embodiment 1：
The neodymium iron boron magnetic body surface that 1.5cm thickness consistency is 90% coats Dy2O3Suspension, coating layer thickness 1.0mm；
Step 1：NdFeB magnetic powder is subjected to oriented moulding under the magnetic field of 1.2T, green compact are carried out in vacuum sintering furnace
Half densification sintering, sintering temperature are 950 DEG C, keep the temperature 1.5h, consistency 90%；
Step 2：By Dy2O3Powder is scattered in absolute ethyl alcohol, obtains suspension, viscosity 200mpa.s after mixing；
In glove box by suspension be coated uniformly on consistency be 90% Sintered NdFeB magnet surface, coating layer thickness 1.0mm,
It is dried in vacuo in vacuum drying chamber, drying temperature is 40 DEG C, dry 45min；
Step 3：Containing Dy2O3Half dense sintering neodymium iron boron of coating is put in a glass tube, then carries out vacuum seal to glass tube
Pipe, vacuum degree is up to 10-2Pa or more；
Step 4：The sample of vacuum glass tube sealing is placed in graphite crucible, then carries out hot isostatic pressing low-temperature sintering and tempering
Processing, application pressure are 100MPa, and sintering temperature is 810 DEG C, keeps the temperature 1h, using 500 DEG C of annealing 3h, slow cooling to room temperature；
Step 5：The neodymium iron boron magnetic body prepared is subjected to VSM magnetic property measurements, the results detailed in Table 1.Comparative example 1：
The green compact suppressed in embodiment 1 are subjected to densification sintering in vacuum sintering furnace, sintering temperature is 1050 DEG C,
Again 3h, 485 DEG C of second annealing 5h, slow cooling are tempered through 930 DEG C of level-ones.The magnetic property for the neodymium iron boron magnetic body being finally prepared refers to
Table 1.As it can be seen that the Dy of this method grain boundary decision2O3Diffusion effect is fine, and sintered density reaches 7.5g/cm3More than, and coercivity is notable
It improves, remanent magnetism and magnetic energy product vary less.
1. grain boundary decision Dy of table2O3The magnetic property of sintered NdFeB sample is influenced
Embodiment 2：
The neodymium iron boron magnetic body surface that 1.5cm thickness consistency is 87% coats Tb2O3Suspension, coating layer thickness 0.8mm；
Step 1：NdFeB magnetic powder is subjected to oriented moulding under the magnetic field of 1.8T, green compact are carried out in vacuum sintering furnace
Half densification sintering, sintering temperature are 900 DEG C, keep the temperature 1h, consistency 87%；
Step 2：By Tb2O3Powder is scattered in acetone, obtains suspension, viscosity 300mpa.s after mixing；In hand
Suspension is coated uniformly on the Sintered NdFeB magnet surface that consistency is 87%, coating layer thickness 0.8mm, true in casing
It is dried in vacuo in empty drying box, drying temperature is 35 DEG C, dry 35min；
Step 3：Containing Tb2O3Half dense sintering neodymium iron boron of coating is put in a glass tube, then carries out vacuum seal to glass tube
Pipe, vacuum degree is up to 10-2Pa or more；
Step 4：The sample of vacuum glass tube sealing is placed in graphite crucible, then carries out hot isostatic pressing low-temperature sintering and tempering
Processing, application pressure are 50MPa, and sintering temperature is 900 DEG C, keeps the temperature 0.5h, using 480 DEG C of annealing 3h, slow cooling to room temperature；
Step 5：The neodymium iron boron magnetic body prepared is subjected to VSM magnetic property measurements, the results detailed in Table 2.
2. grain boundary decision Tb of table2O3The magnetic property of sintered NdFeB sample is influenced
Claims (7)
1. a kind of method that hot isostatic pressing low-temperature sintering prepares high magnetic sintered NdFeB, which is characterized in that include the following steps：
(1) NdFeB magnetic powder is subjected to orientation die mould under the magnetic field of 1.2~2.0T；The green compact that die mould is completed is put into vacuum to burn
Half dense sintering of vacuum is carried out in freezing of a furnace, sintering temperature is 850~950 DEG C, and soaking time is 1~3h, obtains half fine and close burning
Tie neodymium iron boron sample；
(2) suspension containing heavy rare earth compound is prepared, and viscosity is 100~500mpa.s, suspension is coated in glove box
On half fine and close sintered neodymium iron boron material surface, it is then placed in vacuum drying chamber and is dried in vacuo, it is dry at 35~45 DEG C
30~60min obtains half dense sintering neodymium iron boron of the coating containing heavy rare earth compound；
(3) the half dense sintering neodymium iron boron containing coating in step (2) is put in a glass tube, then vacuum seal is carried out to glass tube
Pipe, vacuum degree is up to 10-2~10-3Pa obtains the sample of vacuum glass tube sealing；
(4) sample of vacuum glass tube sealing in step (3) is placed on progress hot isostatic pressing low-temperature sintering in hot isostatic press, then passed through
The uniform Sintered NdFeB magnet of diffusion is made in 400~500 DEG C of 1~3h of tempering, slow cooling；Wherein, it is pressure gas with high-purity argon gas
Body, pressure are 10~100MPa.
2. the method that a kind of hot isostatic pressing low-temperature sintering according to claim 1 prepares high magnetic sintered NdFeB, special
Sign is：The consistency of half fine and close sintered NdFeB sample described in step (1) is 85%~95%.
3. the method that a kind of hot isostatic pressing low-temperature sintering according to claim 1 prepares high magnetic sintered NdFeB, special
Sign is：The solvent of the suspension of heavy rare earth compound described in step (2) is ethyl alcohol, ethylene glycol, acetone, propylene glycol or poly- second
One or more mixed liquors in enol.
4. the method that a kind of hot isostatic pressing low-temperature sintering according to claim 1 prepares high magnetic sintered NdFeB, special
Sign is：Heavy rare earth compound described in step (2) is Dy2S3、Dy2O3、Tb2O3、DyF3Or DyH3In it is a kind of or more
Kind.
5. the method that a kind of hot isostatic pressing low-temperature sintering according to claim 1 prepares high magnetic sintered NdFeB, special
Sign is：The thickness of heavy rare earth compound coating described in step (2) is 0.5~2mm.
6. the method that a kind of hot isostatic pressing low-temperature sintering according to claim 1 prepares high magnetic sintered NdFeB, special
Sign is：The softening temperature that glass tube described in step (3) requires is 450~650 DEG C.
7. the method that a kind of hot isostatic pressing low-temperature sintering according to claim 1 prepares high magnetic sintered NdFeB, special
Sign is：Low-temperature sintering temperature described in step (4) is 700~900 DEG C, keeps the temperature 0.5~1.5h.
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| CN112382498A (en) * | 2020-11-23 | 2021-02-19 | 杨杭福 | Preparation method of high-coercivity and high-energy product diffusion samarium-iron-nitrogen magnet |
| US20210166870A1 (en) * | 2019-11-28 | 2021-06-03 | Yantai Shougang Magnetic Materials Inc | Method for increasing the coercivity of a sintered type ndfeb permanent magnet |
| CN113394015A (en) * | 2021-05-17 | 2021-09-14 | 江苏科技大学 | Preparation method of large-depth grain boundary diffusion neodymium iron boron magnet |
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| US12027307B2 (en) * | 2019-11-28 | 2024-07-02 | Yantai Shougang Magnetic Materials Inc | Method for increasing the coercivity of a sintered type NdFeB permanent magnet |
| CN112382498A (en) * | 2020-11-23 | 2021-02-19 | 杨杭福 | Preparation method of high-coercivity and high-energy product diffusion samarium-iron-nitrogen magnet |
| CN113394015A (en) * | 2021-05-17 | 2021-09-14 | 江苏科技大学 | Preparation method of large-depth grain boundary diffusion neodymium iron boron magnet |
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