CN106952721A - A kind of method that high temperature compression improves rare earth permanent-magnetic material performance - Google Patents
A kind of method that high temperature compression improves rare earth permanent-magnetic material performance Download PDFInfo
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- CN106952721A CN106952721A CN201710152068.5A CN201710152068A CN106952721A CN 106952721 A CN106952721 A CN 106952721A CN 201710152068 A CN201710152068 A CN 201710152068A CN 106952721 A CN106952721 A CN 106952721A
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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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- 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
- H01F1/0576—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 pressed, e.g. hot working
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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
-
- 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
Abstract
The method that high temperature compression disclosed by the invention improves rare earth permanent-magnetic material performance, this method at least comprises the following steps：Adhere to heavy rare earth compound in the magnet surface obtained through oversintering, and by heating, applying compression at high temperature, obtain magnet.By improving magnet diffusion depth, the problem of inconsistency is spread to the limitation of magnet specification and heavy rare earth in traditional handicraft is overcome, diffusion effect is enhanced, magnet obtains preferably magnetic property, and equipment investment is simple, and cost is relatively low, suitable for large-scale promotion.
Description
Technical field
The present invention relates to a kind of method for improving rare-earth Nd-Fe-B magnetic material performance, magnet is particularly improved coercitive
Method, the method that especially a kind of high temperature compression improves rare earth permanent-magnetic material performance.
Background technology
Since last century the eighties neodymium iron boron magnetic body invention, due to its very-high performance characteristic electronics, new energy,
Aero-Space, medical treatment, message area etc. have extensive purposes.With the development of technology, the market demand of high trade mark magnet is got over
Come more extensive, each research unit and neodymium iron are just turned into for the new technology of representative with pressureless sintering, crystal grain refinement, heavy rare earth diffusion etc.
The Research Emphasis of boron enterprise.Because rare earth price is unstable in recent years, therefore it has been altogether to develop low heavy rare earth high-coercivity magnet
Know, and promoted energetically for each enterprise.
Improving the coercitive method of neodymium iron boron at present mainly has following two：Crystal grain refinement and grain boundary decision.Neodymium iron boron is brilliant
Grain refinement can reduce the reverse forming core of magnet, using low-temperature sintering, can suppress magnet crystal grain and grow up.Japanese researchers utilize helium
Airflow milling crystal grain thinning, 1 μm or so is controlled in by granularity of magnet powder, and have developed coercivity is 20kOe without dysprosium magnet.It is domestic
There is enterprise to be improved by crystal grain refinement without dysprosium magnet coercivity to 21kOe.In addition, TDK is using crystal grain thinning and optimization structure
The method being combined, prepares no heavy rare earth 48SH magnets.
Grain boundary decision mainly uses rare earth especially heavy rare earth simple substance and its oxide, fluoride, hydride etc. and magnet
Heavy rare earth enters crystal boundary and Grain Surface by liquid phase in magnet in contact, ag(e)ing process, due to the anti-magnetic of Sintered NdFeB magnet
Change forming core and betide grain surface, and the entrance of heavy rare earth can improve the anisotropy field in the region, so as to improve rectifying for magnet
Stupid power.Simultaneously as heavy rare earth is primarily present in crystal boundary and is introduced into principal phase, therefore the saturation magnetization of principal phase is not sent out substantially
Obvious reduction will not also occur for changing, magnet remanent magnetism.Another contactless diffusion process is evaporation timeliness, by heavy rare earth list
Matter is heated to uniform temperature so that the heavy rare earth vaporised atom, which comes out and diffused to inside magnet, enters crystal boundary, equally plays carrying
The high coercitive purpose of magnet.
It is known that heavy rare earth is entered inside magnet by surface in the grain boundary decision of magnet, therefore carried using grain boundary decision
High magnet coercivity is limited to magnet thickness, namely raising magnet coercivity effect is more obvious when magnet is relatively thin, and for
Thicker magnet, heavy rare earth atomic concentration is from surface to center distribution gradient, and position coercivity lifts effect very at bosom
Limited, so as to cause that the overall coercivity of magnet is not obvious, squareness is poor.In addition, existing process oozes dysprosium/terbium efficiency low, magnetic
Body surface face is uneven, and automaticity is low, is unfavorable for batch production.In the prior art, it is (such as nano level using heavy rare earth powder
Or the micron-sized powder compared with small particle) form that is mixed with magnet alloy powder realizes adding for heavy rare earth element in magnet
Plus and diffusion, this scheme is limited by that proportion is different, the not equal factor of granular size is difficult to realize in mixed process
Complete is well mixed, and in sintering process, the particle of powder morphology because fusing point it is different make low-melting easy flow
It is dynamic to gather, so that the scattered uniformity of magnet rare earth elements can greatly be influenceed.
The content of the invention
To solve the above problems, the invention discloses a kind of method that high temperature compression improves rare earth permanent-magnetic material performance,
Magnet diffusion depth and method suitable for volume production can be improved there is provided a kind of, traditional rare earth permanent magnetism body processing technology face is overcome
The problem for the magnet specification limitation faced, and the diffusion consistency problem of heavy rare earth element in magnet is solved, enhance expansion
Effect is dissipated, magnet obtains preferably magnetic property, and equipment investment is simple, and cost is relatively low, suitable for large-scale promotion.
The method that high temperature compression disclosed by the invention improves rare earth permanent-magnetic material performance, this method at least includes following step
Suddenly：Adhere to heavy rare earth compound in the magnet surface obtained through oversintering, and by heating, applying compression at high temperature, obtain
To magnet.
The present invention program in the way of stress permeates by the shaped magnet of densification, realizing at a suitable temperature
The crystal boundary of heavy rare earth element in magnet is added, it is achieved thereby that the controllability that is distributed to heavy rare earth element in magnet, real
Show being uniformly distributed for heavy rare earth element in magnet, lifted the magnetic property of magnet, particularly lift the coercivity of magnet, and also
Reduce the consumption of heavy rare earth element.
High temperature compression disclosed by the invention is improved in a kind of improvement of the method for rare earth permanent-magnetic material performance, this method：
Magnet surface adhere to heavy rare earth compound when and/or heating when and/or at high temperature apply compression when, under protective gas atmosphere
Carry out.It is preferred that protective gas atmosphere be nitrogen, helium, argon gas etc. one or more kinds of atmosphere.
High temperature compression disclosed by the invention is improved in a kind of improvement of the method for rare earth permanent-magnetic material performance, this method,
Magnet surface attachment heavy rare earth compound is that heavy rare earth compound roll-in is attached into magnet surface by hard alloy roller.We
Case, with the squeezing action of hard alloy, promotes heavy rare earth atom under high temperature pressure effect in magnetic by the form of high temperature roll-in
Conveyed in body grain boundary structure, while compression plays a role in promoting, and avoid heavy rare earth atom (special because of the diffusion of freely activity
In the case of being prolonged free diffusing) principal phase structure is entered, both improve heavy rare earth element in magnet and be distributed, lifting is uniform
Property, improve magnet mass and be conducive to improving production efficiency.
High temperature compression disclosed by the invention is improved in a kind of improvement of the method for rare earth permanent-magnetic material performance, this method,
When magnet surface adheres to heavy rare earth compound, hard alloy roller is is not added with thermalloy roller, and heavy rare-earth solution passes through hard alloy roller
Surface roll-in is attached to magnet surface.This programme is by using the overall compacting environment for being not added with thermalloy roller and suppressing magnet
Temperature control is carried out, so as to reduce the constructive difficulty of roller and the cost of production application so that overall temperature environment has good
Good controllability and stability, can greatly reduce temperature fluctuation, so that magnet product has good quality of lot
Stability.
High temperature compression disclosed by the invention is improved in a kind of improvement of the method for rare earth permanent-magnetic material performance, this method,
When magnet surface adheres to heavy rare earth compound, the magnet that surface attachment has heavy rare earth is heated to 750 DEG C~950 DEG C.This programme control
The temperature of system control magnet, makes especially structure for conveying occur in grain boundaries in the microstructure of magnet --- as crystal boundary liquefies
Phenomenon etc., so as to both be beneficial to the seeping for promoting heavy rare earth atom, is improved to the osmotic efficiency inside magnet, and with good
Good compression restorability, it is to avoid deformation occur, realize heavy rare earth atom uniformly penetrating in various sizes magnet, while keep away again
Exempt from temperature it is too high there is the liquefaction of transition and so that magnet deformation or so that heavy rare earth element is pressed into principal phase structure, and mistake
It is low, it certainly can then hinder to penetrate into activity, and be limited to the fragility of magnet and be prone to brittle damage.
High temperature compression disclosed by the invention is improved in a kind of improvement of the method for rare earth permanent-magnetic material performance, this method,
When magnet surface adheres to heavy rare earth compound, surface attachment have the compression of the magnet of heavy rare earth at high temperature for 50~
150kPa.This programme by suitable pressure size, both avoided the occurrence of stress it is excessive and cause occur stress damage (as it is damaged,
Crackle, internal crystalline phase dislocation etc.), meanwhile, extra stress power is provided for heavy rare earth element atom at appropriate temperatures, and
Increase osmotic efficiency, lift overall permeability, realize heavy rare earth atom uniformly penetrating in various sizes magnet.
High temperature compression disclosed by the invention is improved in a kind of improvement of the method for rare earth permanent-magnetic material performance, this method,
When magnet surface adheres to heavy rare earth compound, hard alloy roller is interior heating arrangement, and heavy rare-earth solution passes through hard alloy roller table
Face roll-in is attached to magnet surface.This programme is by using heating alloy roller to the temperature of magnet and alloy roller in different magnetic
The carry out Adaptive Control in the stage of body compacting, temperature controlled flexibility during lifting processing so that temperature has good in processing
Good control accuracy, can greatly lift the osmotic efficiency and osmotic evenness of heavy rare earth atom, so that various rule
The magnet product of lattice size is obtained with the product quality optimized.
High temperature compression disclosed by the invention is improved in a kind of improvement of the method for rare earth permanent-magnetic material performance, this method,
When magnet surface adheres to heavy rare earth compound, the skin temperature of the hard alloy roller of interior heating is heated to 750 DEG C~950 DEG C.This
The temperature of scheme control control magnet, makes especially structure for conveying occur in grain boundaries in the microstructure of magnet --- as crystal boundary goes out
Existing liquefaction phenomenon etc., so as to both be beneficial to the seeping for promoting heavy rare earth atom, is improved to the osmotic efficiency inside magnet, and
With good compression restorability, it is to avoid deformation occur, heavy rare earth atom uniformly penetrating in various sizes magnet is realized, together
When avoid again temperature it is too high there is the liquefaction of transition and so that magnet deformation or so that heavy rare earth element is pressed into principal phase knot
Structure, and too low, certainly can then hinder to penetrate into activity, and be limited to the fragility of magnet to be prone to brittle damage.
High temperature compression disclosed by the invention is improved in a kind of improvement of the method for rare earth permanent-magnetic material performance, this method,
When magnet surface adheres to heavy rare earth compound, the hard alloy roller of interior heating is 50~150kPa to the compression of magnet.We
Case had both avoided the occurrence of stress excessive and cause and stress damage occur (such as breakage, crackle, internal crystalline substance by suitable pressure size
Phase dislocation etc.), meanwhile, extra stress power is provided for heavy rare earth element atom at appropriate temperatures, and increase infiltration effect
Rate, lifts overall permeability, realizes heavy rare earth atom uniformly penetrating in various sizes magnet.
The implementation of the present invention program, magnet with after hard alloy roller identical temperature, then by hard alloy roller
Roll-in.In roll-in, by under compression and heat effect, conveying is mutually produced in magnet, and the compression applied by roller makes
The heavy rare earth atom for obtaining magnet surface is moved and is distributed in crystal boundary along pressure direction, the distance that heavy rare earth atom is moved in crystal boundary
Length and pressure size that disk roller applies and relevant by the time length of compression with magnet.This method can increase the expansion of magnet
Depth is dissipated, beneficial to preparing the higher magnet of thickness.Heavy rare earth atomic migration distance increase when, moderately increase compression size or
Person's extension applies time or compression and the afterburning time increase simultaneously of compression.
High temperature compression disclosed by the invention is improved in a kind of improvement of the method for rare earth permanent-magnetic material performance, this method,
Ageing Treatment is also carried out after applying compression at high temperature.It is preferred that, when timeliness includes the one-level that temperature is 850 DEG C~950 DEG C
Effect, temperature is 450 DEG C~550 DEG C of secondary time effect.Wherein one-level timeliness is vacuum infiltration process, while using higher timeliness
Temperature, its purpose coordinates residual stress to produce liquid phase so that extraneous heavy rare earth compound enters inside magnet with liquid phase, from
And further promote effective diffusion of heavy rare earth element, and realize heavy rare earth element and uniformly divide in the deep layer of magnet interiors of products
Cloth, while eliminating residual stress；Secondary time effect is diffusion process, realizes the further diffusion in magnet so that heavy rare earth is in magnetic
It is evenly distributed in body.
The method that high temperature compression disclosed by the invention improves rare earth permanent-magnetic material performance can also include other being ability
Processing step known to field technique personnel, such as carries out melting, broken hydrogen, airflow milling, shaping, sintering cause to rare-earth iron-boron material
Densification process technique, and being made with certain thickness magnet, and deoiling, pickling, the aftertreatment technology step such as cleaning.Then
Implement the high temperature compression technique of the application again.
In addition, rare earth permanent-magnetic material is also the rare-earth permanent magnet being well known to those skilled in the art, can be include and
It is not limited to the magnet containing rare earth, transition elements, trace element (copper, gallium, aluminium, zirconium, niobium etc.) and boron element：Here rare earth member
Element can be billows, cerium, praseodymium, neodymium, terbium, dysprosium, at least one of holmium etc.；Transition elements can be iron and/or cobalt etc.；Trace element can
At least one of think copper, gallium, aluminium, zirconium, niobium etc..
Heavy rare earth compound includes the hydride of fluoride, the oxide of dysprosium and/or terbium, dysprosium and/or the terbium of dysprosium and/or terbium
Deng andThe bianry alloy of (praseodymium and/or neodymium), (dysprosium and/or terbium), (aluminium and/or copper and/or iron and/or cobalt and/or gallium) etc. or Ternary alloy three-partalloy or quaternary alloy, each bracket of dashed part is unitary, and (dysprosium and/or terbium) is in bianry alloy or ternary
There must be in alloy or quaternary alloy.
The method that high temperature compression disclosed by the invention improves rare earth permanent-magnetic material performance can improve magnetic there is provided one kind
Body diffusion depth and the method suitable for volume production, are carried out using heavy rare earth atom under the conditions of suitable high temperature pressure along magnet crystal boundary
Depth of penetration, so as to overcome the problem for the magnet specification limitation that traditional rare earth permanent magnetism body processing technology faces, and is solved
The diffusion consistency problem of heavy rare earth element, enhances diffusion effect, reduces need of the magnet to heavy rare earth element in magnet
Ask, magnet is obtained preferably magnetic property and is reduced production cost, and equipment investment is simple, cost is relatively low, suitable for pushing away on a large scale
Extensively.
Brief description of the drawings
Fig. 1, high temperature compression disclosed by the invention improve a kind of showing for embodiment of the method for rare earth permanent-magnetic material performance
It is intended to；
Fig. 2, high temperature compression disclosed by the invention improve another embodiment of the method for rare earth permanent-magnetic material performance
Schematic diagram.
Reference numerals list：
1st, magnet；2nd, hard alloy roller；3rd, heater.
Embodiment
With reference to the accompanying drawings and detailed description, the present invention is furture elucidated, it should be understood that following embodiments are only
For illustrating the present invention rather than limitation the scope of the present invention.It should be noted that the word " preceding " used below in description,
" rear ", "left", "right", "up" and "down" refer to the direction in accompanying drawing, and word " interior " and " outer " refer respectively to direction or remote
From the direction of particular elements geometric center.
Embodiment 1
The present embodiment, the method that high temperature compression improves rare earth permanent-magnetic material performance at least comprises the following steps：Passing through
Obtained magnet surface attachment heavy rare earth compound is sintered, and by heating, applying compression at high temperature, obtains magnet.
Distinguished with above-described embodiment, the high temperature compression is improved in the method for rare earth permanent-magnetic material performance：Magnet table
In protective gas atmosphere, (protective gas atmosphere is nitrogen atmosphere or helium atmosphere or argon atmosphere when heavy rare earth compound is adhered in face
Or nitrogen argon gas gaseous mixture atmosphere or nitrogen helium mix atmosphere are enclosed or helium argon gas gaseous mixture atmosphere or nitrogen, helium
Gas, argon gas gaseous mixture atmosphere, atmosphere pressure is preferably 1atm, similarly hereinafter) under carry out.
Distinguished with above-described embodiment, the high temperature compression is improved in the method for rare earth permanent-magnetic material performance：During heating
Carried out under protective gas atmosphere.
Distinguished with above-described embodiment, the high temperature compression is improved in the method for rare earth permanent-magnetic material performance：In high temperature
Carried out during lower application compression under protective gas atmosphere.
Distinguished with above-described embodiment, the high temperature compression is improved in the method for rare earth permanent-magnetic material performance：Magnet table
Carried out when heavy rare earth compound is adhered in face with the when of heating under protective gas atmosphere.
Distinguished with above-described embodiment, the high temperature compression is improved in the method for rare earth permanent-magnetic material performance：Magnet table
Carried out during the attachment heavy rare earth compound of face and when applying compression at high temperature under protective gas atmosphere.
Distinguished with above-described embodiment, the high temperature compression is improved in the method for rare earth permanent-magnetic material performance：During heating
Carried out when applying compression at high temperature under protective gas atmosphere.
Distinguished with above-described embodiment, the high temperature compression is improved in the method for rare earth permanent-magnetic material performance：Magnet table
Face adhere to heavy rare earth compound when, heating when and at high temperature apply compression when, under protective gas atmosphere carry out.
Distinguished with above-described embodiment, the high temperature compression is improved in the method for rare earth permanent-magnetic material performance：Magnet table
Face attachment heavy rare earth compound is that heavy rare earth compound roll-in is attached into magnet surface by hard alloy roller.
Distinguished with above-described embodiment, the high temperature compression is improved in the method for rare earth permanent-magnetic material performance：Magnet table
Face adhere to heavy rare earth compound when, hard alloy roller for be not added with thermalloy roller (be not added with the alloy roller that thermalloy roller refers to not self-heating,
The explanation of other positions is identical), heavy rare-earth solution is attached to magnet surface by hard alloy roller surface roll-in.Preferably, weight
Earth solution is attached to after magnet surface processing by hard alloy roller surface roll-in, and the part heavy rare earth accounts for magnet gross mass and is
Include but not limited to following any：0.5%th, in the range of 0.6%, 0.7%, 0.8%, 0.9%, 1% and 0.5~1% its
Its any value.
Distinguished with above-described embodiment, the high temperature compression is improved in the method for rare earth permanent-magnetic material performance：Magnet table
Face adhere to heavy rare earth compound when, the magnet that surface attachment has heavy rare earth be heated to 750 DEG C (heating-up temperature can also be include and
It is not limited to following any：760℃、770℃、780℃、790℃、800℃、810℃、820℃、830℃、840℃、850℃、
860℃、870℃、880℃、890℃、900℃、910℃、920℃、930℃、940℃、950℃、762℃、777℃、784
℃、792℃、803℃、815℃、827℃、838℃、844℃、859℃、866℃、871℃、882℃、894℃、909℃、
Other arbitrary values in the range of 911 DEG C, 925 DEG C, 936 DEG C, 948 DEG C, 754 DEG C and 750 DEG C~950 DEG C).
Distinguished with above-described embodiment, the high temperature compression is improved in the method for rare earth permanent-magnetic material performance：Magnet table
When heavy rare earth compound is adhered in face, surface attachment has the compression of the magnet of heavy rare earth at high temperature, and for 50kPa, (compression may be used also
Think include but not limited to it is following any：60kPa、70kPa、80kPa、90kPa、100kPa、110kPa、120kPa、130kPa、
140kPa、150kPa、86kPa、87kPa、88kPa、89kPa、90kPa、91kPa、92kPa、93kPa、94kPa、95kPa、
62kPa、77kPa、78kPa、79kPa、103kPa、115kPa、127kPa、138kPa、144kPa、59kPa、106kPa、
71kPa, 82kPa, 134kPa, 149kPa, 111kPa, 125kPa, 136kPa, 148kPa, 54kPa and 50~150kPa scopes
Interior other arbitrary values).
Distinguished with above-described embodiment, the high temperature compression is improved in the method for rare earth permanent-magnetic material performance：Magnet table
When heavy rare earth compound is adhered in face, hard alloy roller is interior heating arrangement, and heavy rare-earth solution passes through hard alloy roller surface roll-in
It is attached to magnet surface.
Distinguished with above-described embodiment, the high temperature compression is improved in the method for rare earth permanent-magnetic material performance：Magnet table
When heavy rare earth compound is adhered in face, the skin temperature of the hard alloy roller of interior heating is heated to 750 DEG C, and (heating-up temperature can also be
Include but not limited to following any：760℃、770℃、780℃、790℃、800℃、810℃、820℃、830℃、840℃、
850℃、860℃、870℃、880℃、890℃、900℃、910℃、920℃、930℃、940℃、950℃、762℃、777
℃、784℃、792℃、803℃、815℃、827℃、838℃、844℃、859℃、866℃、871℃、882℃、894℃、
Other arbitrary values in the range of 909 DEG C, 911 DEG C, 925 DEG C, 936 DEG C, 948 DEG C, 754 DEG C and 750 DEG C~950 DEG C).
Distinguished with above-described embodiment, the high temperature compression is improved in the method for rare earth permanent-magnetic material performance：Magnet table
When heavy rare earth compound is adhered in face, the hard alloy roller of interior heating be that (compression can also be to wrap to 50kPa to the compression of magnet
Include and be not limited to following any：60kPa、70kPa、80kPa、90kPa、100kPa、110kPa、120kPa、130kPa、
140kPa、150kPa、86kPa、87kPa、88kPa、89kPa、90kPa、91kPa、92kPa、93kPa、94kPa、95kPa、
62kPa、77kPa、78kPa、79kPa、103kPa、115kPa、127kPa、138kPa、144kPa、59kPa、106kPa、
71kPa, 82kPa, 134kPa, 149kPa, 111kPa, 125kPa, 136kPa, 148kPa, 54kPa and 50~150kPa scopes
Interior other arbitrary values).
Distinguished with above-described embodiment, the high temperature compression is improved in the method for rare earth permanent-magnetic material performance：In high temperature
Ageing Treatment is also carried out after lower application compression.
Distinguished with above-described embodiment, the high temperature compression is improved in the method for rare earth permanent-magnetic material performance：Timeliness bag
Include temperature for 850 DEG C (one-level aging temp can also be include but not limited to it is following any：860℃、870℃、880℃、890
℃、900℃、910℃、920℃、930℃、940℃、950℃、862℃、877℃、884℃、892℃、87℃、885℃、927
℃、938℃、944℃、859℃、866℃、871℃、882℃、894℃、909℃、911℃、925℃、936℃、948℃、
Other arbitrary values in the range of 854 DEG C and 850 DEG C~950 DEG C) one-level timeliness, temperature be 550 DEG C (secondary time effect temperature is also
Can be include but not limited to it is following any：460℃、470℃、480℃、490℃、500℃、510℃、520℃、530℃、
540℃、450℃、462℃、477℃、484℃、492℃、503℃、515℃、527℃、538℃、544℃、459℃、466
DEG C, 471 DEG C, 482 DEG C, 494 DEG C, 509 DEG C, 511 DEG C, 525 DEG C, 536 DEG C, 548 DEG C, 454 DEG C and 450 DEG C~550 DEG C scopes
Interior other arbitrary values) secondary time effect.
Distinguished with above-described embodiment, heavy rare earth compound is to include but not limited to following at least one：Dysprosium and/or terbium
Fluoride, the oxide of dysprosium and/or terbium, the hydride of dysprosium and/or terbium etc. and (praseodymium and/or neodymium), (dysprosium and/or terbium),(aluminium And/or copper and/or iron and/or cobalt and/or gallium)Deng bianry alloy or ternary alloy three-partalloy or quaternary alloy, i.e., including dysprosium fluoride, fluorine
Change terbium, dysprosia, terbium oxide, hydrogenation dysprosium, hydrogenation terbium, the alloy of (praseodymium and/or neodymium) and (dysprosium and/or terbium), (praseodymium and/or neodymium) with
The alloy of (dysprosium and/or terbium) and (aluminium and/or copper and/or iron and/or cobalt and/or gallium), (dysprosium and/or terbium) and (aluminium and/or copper
And/or iron and/or cobalt and/or gallium) alloy.Dashed part is such as in this sectionAluminium and/or copper and/or iron and/or cobalt and/or galliumRefer to
At least one of aluminium, copper, iron, cobalt, gallium, to the characterizing portion of heavy rare earth compound in the present invention program, with similar statement shape
Formula does the similar explanation in this place.
As shown in figure 1, the magnet 1 that sintering is obtained, under suitable hot environment, heavy rare-earth solution is scribbled by surface
Hard alloy roller 2 (roller not self-heating), is suppressed by the suitable compression of certain time, so as to obtain high temperature compression
Improve rare earth permanent-magnetic material.
As shown in Fig. 2 the magnet 1 that sintering is obtained, magnet 1 is heated by heater 3 so as to have in roll-in with roll surface
Have identical temperature, under suitable hot environment, by surface scribble heavy rare-earth solution hard alloy roller 2 (roller be from
Heating), suppressed by the suitable compression of certain time, so that obtaining high temperature compression improves rare earth permanent-magnetic material.
Below by way of exemplified by choosing a kind of common Nd-Fe-B permanent magnet (such as N35, but in formula heavy rare earth element addition
Sample the present invention program, remaining raw material is using conventional method addition) illustrate the excellent part of the present invention program.
Specific embodiment one
The manufacture method of rare-earth permanent magnet in the present embodiment, by the way that the neodymium iron boron magnetic body of preparation is thinly sliced, passes through
Oil removing, pickling, drying and processing is dried heavy rare earth compound uniform adhesion in magnet surface by hard alloy roller through high temperature
It is dry to apply certain compression again by interior heating high temperature disk roller, taken out magnet Ageing Treatment, the acquisition He of test specimens 1 after cooling
Test specimens 2.
The preparation of above-mentioned neodymium iron boron magnetic body includes melting, and hydrogen is broken, airflow milling, shaping, the processing such as sintering.Magnet is without too high
Warm hardening processing, and cut into 50mm*60mm*10mm bulk square piece magnet (being contrasted using the magnet as original sample).
The thickness control of thin slice magnet is 10mm, by oil removing, pickling, the rustless stain of holding surface after drying.
Argon pressure is 1atm.Hard alloy roller is not heated, and the alcoholic solution of dysprosium fluoride is only sticked at into magnet surface, in
Between heater box temperature be 900 DEG C, interior heating disk roller temperature is 900 DEG C.It is 50kPa that two disk rollers, which apply stress, and mobile linear velocity is
1m/min。
The concentration of dysprosium fluoride alcoholic solution at normal temperatures and pressures is 40wt%, and accounting for magnet gross mass after this programme processing is
1%.
Taken out after above-mentioned magnet is cooled down, be placed in Ageing Treatment, one-level timeliness in the sintering furnace that vacuum is 1*10-3Pa
Temperature is 900 DEG C, and the time is 12h；Secondary time effect temperature is 500 DEG C, and the time is 4h.
Magnet magnetic property value before and after being spread in the specific embodiment one of table 1.
By upper table contrast as can be seen that this method can to obtain surfacing in dysprosium fluoride solution adhesion process uniform
Coating, can improve the diffusion depth of dysprosium atom during high temperature extrusion, be highly suitable for the heavy rare earth diffusion of thicker magnet,
On the premise of remanent magnetism, magnetic energy product, Hk/Hci etc. are not reduced substantially, coercivity is greatly improved, and uniformity is preferably,
Magnet squareness is higher.
Specific embodiment two：
The manufacture method of rare-earth permanent magnet in the present embodiment, by the way that the neodymium iron boron magnetic body of preparation is thinly sliced, passes through
Oil removing, pickling, drying and processing is dried heavy rare earth compound uniform adhesion in magnet surface by stainless steel disk roller through high temperature
Afterwards by stainless steel high temperature disk roller, apply certain compression, taken out magnet Ageing Treatment after cooling, obtain test specimens 1 and survey
Sample 2.
The preparation of above-mentioned neodymium iron boron magnetic body includes melting, and hydrogen is broken, airflow milling, shaping, the processing such as sintering.Magnet is without too high
Warm hardening processing, and cut into 50mm*60mm*10mm bulk square piece magnet (being contrasted using the magnet as original sample).
The thickness control of thin slice magnet is 10mm, by oil removing, pickling, the rustless stain of holding surface after drying.
Helium pressure is 1atm.Hard alloy roller is not heated, and the alcoholic solution for being fluorinated terbium is only sticked at into magnet surface, in
Between heater box temperature be 900 DEG C, interior heating disk roller temperature is 900 DEG C.It is 50kPa that two disk rollers, which apply stress, rotates linear speed
Spend for 1m/min.
It is 40wt% to be fluorinated the concentration of terbium alcoholic solution at normal temperatures and pressures, and accounting for magnet gross mass after this programme processing is
0.8%.
Taken out after above-mentioned magnet is cooled down, be placed in Ageing Treatment, one-level timeliness in the sintering furnace that vacuum is 1*10-3Pa
Temperature is 900 DEG C, and the time is 12h；Secondary time effect temperature is 500 DEG C, and the time is 4h.
Magnet magnetic property value before and after being spread in the specific embodiment two of table 2.
By upper table contrast, as can be seen that the present invention program is in fluorination terbium solution adhesion process, can to obtain surfacing equal
Even coating, can improve the diffusion depth of terbium atom during high temperature extrusion, and the heavy rare earth for being highly suitable for thicker magnet expands
Dissipate, on the premise of remanent magnetism, magnetic energy product, Hk/Hci etc. are not reduced substantially, coercivity is greatly improved, and uniformity
Preferably, magnet squareness is higher.
Specific embodiment three
The manufacture method of rare-earth permanent magnet in the present embodiment, by the way that the neodymium iron boron magnetic body of preparation is thinly sliced, passes through
Oil removing, pickling, drying and processing is dried heavy rare earth compound uniform adhesion in magnet surface by hard alloy roller through high temperature
It is dry to apply certain compression again by interior heating high temperature disk roller, taken out magnet Ageing Treatment, the acquisition He of test specimens 1 after cooling
Test specimens 2.
The preparation of above-mentioned neodymium iron boron magnetic body includes melting, and hydrogen is broken, airflow milling, shaping, the processing such as sintering.Magnet is without too high
Warm hardening processing, and cut into 50mm*60mm*10mm bulk square piece magnet (being contrasted using the magnet as original sample).
The thickness control of thin slice magnet is 10mm, by oil removing, pickling, the rustless stain of holding surface after drying.
Argon pressure is 1atm.Hard alloy roller is not heated, and the alcoholic solution of dysprosium fluoride is only sticked at into magnet surface, in
Between heater box temperature be 800 DEG C, interior heating disk roller temperature is 800 DEG C.It is 100kPa that two disk rollers, which apply stress, and mobile linear velocity is
1m/min。
The concentration of dysprosium fluoride alcoholic solution at normal temperatures and pressures is 40wt%, and accounting for magnet gross mass after this programme processing is
0.6%.
Taken out after above-mentioned magnet is cooled down, be placed in Ageing Treatment, one-level timeliness in the sintering furnace that vacuum is 1*10-3Pa
Temperature is 850 DEG C, and the time is 10h；Secondary time effect temperature is 550 DEG C, and the time is 2h.
Magnet magnetic property value before and after being spread in the specific embodiment three of table 3.
By upper table contrast as can be seen that this method can to obtain surfacing in dysprosium fluoride solution adhesion process uniform
Coating, can improve the diffusion depth of dysprosium atom during high temperature extrusion, be highly suitable for the heavy rare earth diffusion of thicker magnet,
On the premise of remanent magnetism, magnetic energy product, Hk/Hci etc. are not reduced substantially, coercivity is greatly improved, and uniformity is preferably,
Magnet squareness is higher.
Specific embodiment four：
The manufacture method of rare-earth permanent magnet in the present embodiment, by the way that the neodymium iron boron magnetic body of preparation is thinly sliced, passes through
Heavy rare earth compound uniform (solution morphology) is adhered to magnet surface by oil removing, pickling, drying and processing by stainless steel disk roller,
By stainless steel high temperature disk roller after being dried through high temperature, apply certain compression, take out magnet Ageing Treatment, surveyed after cooling
Sample 1 and test specimens 2.
The preparation of above-mentioned neodymium iron boron magnetic body includes melting, and hydrogen is broken, airflow milling, shaping, the processing such as sintering.Magnet is without too high
Warm hardening processing, and cut into 50mm*60mm*10mm bulk square piece magnet (being contrasted using the magnet as original sample).
The thickness control of thin slice magnet is 10mm, by oil removing, pickling, the rustless stain of holding surface after drying.
Helium pressure is 1atm.Hard alloy roller is not heated, and the alcoholic solution of heavy rare earth is only sticked at into magnet surface, in
Between heater box temperature be 900 DEG C, interior heating disk roller temperature is 900 DEG C.It is 50kPa that two disk rollers, which apply stress, rotates linear speed
Spend for 1m/min.
The concentration of dysprosia alcoholic solution at normal temperatures and pressures be 40wt%, terbium oxide alcoholic solution at normal temperatures and pressures
Concentration is 40wt%, and it is respectively 0.5% that both account for magnet gross mass after this programme processing.
Taken out after above-mentioned magnet is cooled down, be placed in Ageing Treatment, one-level timeliness in the sintering furnace that vacuum is 1*10-3Pa
Temperature is 900 DEG C, and the time is 12h；Secondary time effect temperature is 500 DEG C, and the time is 4h.
Magnet magnetic property value before and after being spread in the specific embodiment four of table 4.
By upper table contrast as can be seen that the present invention program can obtain table in dysprosia and terbium oxide solution adhesion process
The coating of face even uniform, dysprosium, the diffusion depth of terbium atom can be improved during high temperature extrusion, is highly suitable for thicker magnet
Heavy rare earth diffusion, on the premise of remanent magnetism, magnetic energy product, Hk/Hci etc. are not reduced substantially, coercivity has obtained very big carry
Rise, and uniformity is preferably, magnet squareness is higher.
Comparative example：
The manufacture method of rare-earth permanent magnet in the present embodiment, by the way that the neodymium iron boron magnetic body of preparation is thinly sliced, passes through
Dysprosium fluoride (test specimens 1)/fluorination terbium (test specimens 2) is well mixed and is coated on magnet by oil removing, pickling, drying and processing with alcohol
Surface, Ageing Treatment after being dried through high temperature.
In present case, the preparation of above-mentioned neodymium iron boron magnetic body includes melting, and hydrogen is broken, airflow milling, shaping, the processing such as sintering.Magnetic
Body is handled without high-temperature aging, and is cut into 50mm*60mm*10mm bulk square piece magnet and (be used as original sample using the magnet
Contrasted).
In the implementation case, the thickness control of thin slice magnet is 10mm, by oil removing, pickling, after drying holding surface without
Rust stain.
In present case, magnet is placed in Ageing Treatment in the sintering furnace that vacuum is 1*10-3Pa, and one-level aging temp is 900
DEG C, the time is 12h；Secondary time effect temperature is 500 DEG C, and the time is 4h.
Table 3
Contrasted by upper table and can be seen that the magnet without the inventive method processing, in remanent magnetism, magnetic energy product, Hk/Hci etc.
Reduction amplitude it is also big compared with the present invention program, coercivity lifting is low compared with the application.
Shown by the contrast exemplified by above-described embodiment one to four with comparative example, rather than to the present invention program protection domain
Limit, technical solution of the present invention is improved the diffusion depth of heavy rare earth atom under high temperature extrusion by heavy rare earth, is highly suitable for
The heavy rare earth diffusion of thicker magnet, so that on the premise of remanent magnetism, magnetic energy product, Hk/Hci etc. are not reduced substantially, coercivity is obtained
Very big lifting has been arrived, and uniformity is preferably, magnet squareness is higher.
This place embodiment is in place of the claimed non-limit of technical scope midrange and in embodiment technology
The new technical scheme formed in scheme to the equal replacement of single or multiple technical characteristics, equally all in application claims
In the range of protection；Simultaneously the present invention program it is all enumerate or unrequited embodiment in, in the same embodiment each
Parameter is merely representative of an example (i.e. a kind of feasible scheme) for its technical scheme, and between parameters and in the absence of strict
Cooperation and qualified relation, wherein each parameter can be replaced mutually when stating and asking without prejudice to axiom and the present invention, special declaration
Except.
Technological means disclosed in the present invention program is not limited only to the technological means disclosed in above-mentioned technological means, also includes
Constituted technical scheme is combined by above technical characteristic.The above is the embodiment of the present invention, should be referred to
Go out, for those skilled in the art, under the premise without departing from the principles of the invention, can also make some
Improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (10)
1. a kind of method that high temperature compression improves rare earth permanent-magnetic material performance, this method at least comprises the following steps：Passing through
Obtained magnet surface attachment heavy rare earth compound is sintered, and by heating, applying compression at high temperature, obtains magnet.
2. the method that high temperature compression according to claim 1 improves rare earth permanent-magnetic material performance, it is characterised in that described
In method：Magnet surface adhere to heavy rare earth compound when and/or heating when and/or at high temperature apply compression when, protection
Atmosphere encloses lower progress.
3. the method that high temperature compression according to claim 1 improves rare earth permanent-magnetic material performance, it is characterised in that described
In method, magnet surface attachment heavy rare earth compound is that heavy rare earth compound roll-in is attached into magnet table by hard alloy roller
Face.
4. the method that high temperature compression according to claim 3 improves rare earth permanent-magnetic material performance, it is characterised in that described
In method, during magnet surface attachment heavy rare earth compound, hard alloy roller is is not added with thermalloy roller, and heavy rare-earth solution passes through hard
The roll-in of alloy roller surface is attached to magnet surface.
5. the method that high temperature compression according to claim 4 improves rare earth permanent-magnetic material performance, it is characterised in that described
In method, during magnet surface attachment heavy rare earth compound, the magnet that surface attachment has heavy rare earth is heated to 750 DEG C~950 DEG C.
6. the method that high temperature compression according to claim 4 improves rare earth permanent-magnetic material performance, it is characterised in that described
In method, during magnet surface attachment heavy rare earth compound, it is 50 that surface attachment, which has the compression of the magnet of heavy rare earth at high temperature,
~150kPa.
7. the method that high temperature compression according to claim 3 improves rare earth permanent-magnetic material performance, it is characterised in that described
In method, during magnet surface attachment heavy rare earth compound, hard alloy roller is interior heating arrangement, and heavy rare-earth solution is closed by hard
Golden roller surface roll-in is attached to magnet surface.
8. the method that high temperature compression according to claim 7 improves rare earth permanent-magnetic material performance, it is characterised in that described
In method, during magnet surface attachment heavy rare earth compound, the skin temperature of the hard alloy roller of interior heating be heated to 750 DEG C~
950℃。
9. the method that high temperature compression according to claim 7 improves rare earth permanent-magnetic material performance, it is characterised in that described
In method, during magnet surface attachment heavy rare earth compound, the hard alloy roller of interior heating to the compression of magnet for 50~
150kPa。
10. the method for improving rare earth permanent-magnetic material performance according to any described high temperature compression of claim 1-9, its feature exists
In, in methods described, at high temperature apply compression after also carry out Ageing Treatment.
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| CN109411226A (en) * | 2018-10-23 | 2019-03-01 | 宁波同创强磁材料有限公司 | A kind of preparation process improving neodymium iron boron magnetic body high temperature resistance and ultralow weightlessness |
| CN110473684A (en) * | 2019-08-19 | 2019-11-19 | 中国计量大学 | A kind of preparation method of high-coercive force Sintered NdFeB magnet |
| CN111554502A (en) * | 2020-04-29 | 2020-08-18 | 南京理工大学 | Method for preparing high-coercivity sintered neodymium-iron-boron through pressurization diffusion heat treatment |
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| CN110473684A (en) * | 2019-08-19 | 2019-11-19 | 中国计量大学 | A kind of preparation method of high-coercive force Sintered NdFeB magnet |
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| CN111554502A (en) * | 2020-04-29 | 2020-08-18 | 南京理工大学 | Method for preparing high-coercivity sintered neodymium-iron-boron through pressurization diffusion heat treatment |
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