CN106952721B - 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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- CN106952721B CN106952721B CN201710152068.5A CN201710152068A CN106952721B CN 106952721 B CN106952721 B CN 106952721B CN 201710152068 A CN201710152068 A CN 201710152068A CN 106952721 B CN106952721 B CN 106952721B
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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
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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
Abstract
The method that high temperature compression disclosed by the invention improves rare earth permanent-magnetic material performance, this method include at least following steps: adhering to heavy rare earth compound in the magnet surface obtained through oversintering, and by heating, applying compression at high temperature, obtain magnet.The problem of by improving magnet diffusion depth, overcoming in traditional handicraft to the limitation of magnet specification and heavy rare earth diffusion inconsistency, diffusion effect is enhanced, magnet obtains preferable magnetic property, and equipment investment is simple, and cost is relatively low, is 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, especially raising magnet is coercitive
Method, the method that especially a kind of high temperature compression improves rare earth permanent-magnetic material performance.
Background technique
Since last century the eighties neodymium iron boron magnetic body invention, due to its very-high performance characteristic electronics, new energy,
Aerospace, 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 it is more extensive, with pressureless sintering, crystal grain refinement, heavy rare earth diffusion etc. just becoming each research unit and neodymium iron for the new technology of representative
The Research Emphasis of boron enterprise.Since rare earth price is unstable in recent years, developing low heavy rare earth high-coercivity magnet has been altogether
Know, and is pushed energetically for each enterprise.
Improving the coercitive method of neodymium iron boron at present, there are mainly two types of: crystal grain refinement and grain boundary decision.Neodymium iron boron is brilliant
Grain refinement can reduce the reversed forming core field of magnet, using low-temperature sintering, can inhibit magnet crystal grain and grow up.Japanese researchers utilize helium
Airflow milling refines crystal grain, and granularity of magnet powder is controlled in 1 μm or so, and having developed coercivity is 20kOe without dysprosium magnet.It is domestic
There is enterprise that will improve without dysprosium magnet coercivity to 21kOe by crystal grain refinement.In addition, TDK is using refinement crystal grain and optimization structure
The method combined prepares no heavy rare earth 48SH magnet.
Grain boundary decision mainly uses rare earth especially heavy rare earth simple substance and its oxide, fluoride, hydride etc. and magnet
It contacts, heavy rare earth enters crystal boundary and Grain Surface by liquid phase in magnet in ag(e)ing process, due to the anti-magnetic of Sintered NdFeB magnet
Change forming core and betides grain surface, and the anisotropy field in the region can be improved in the entrance of heavy rare earth, to improve rectifying for magnet
Stupid power.Simultaneously as heavy rare earth is primarily present in crystal boundary and does not enter main phase, therefore the saturation magnetization of main phase is not sent out substantially
Changing, magnet remanence will not be substantially reduced.Another contactless diffusion process is vapor deposition timeliness, by heavy rare earth list
Matter is heated to certain temperature, so that the heavy rare earth vaporised atom, which comes out and diffuses to, enters crystal boundary inside magnet, equally plays and mentions
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 mentioned 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 promotes effect very at bosom
It is limited, it is not obvious so as to cause magnet entirety coercivity, squareness is poor.In addition, prior art seeps dysprosium/terbium low efficiency, magnetic
Body surface face is uneven, and the degree of automation is low, is unfavorable for producing in batches.In the prior art, using heavy rare earth powder (such as nanoscale
Or the micron-sized powder compared with small particle) form that mixes with magnet alloy powder realizes adding for heavy rare earth element in magnet
Adduction diffusion, this scheme are limited by the factors such as specific gravity difference, granular size difference and are difficult to realize realize in mixed process
Complete to be uniformly mixed, and during the sintering process, the particle of powder morphology makes low-melting easy flow because of the difference of fusing point
It is dynamic to gather, so that the uniformity that rare earth element disperses in magnet can greatly be influenced.
Summary 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,
Provide it is a kind of can be improved magnet diffusion depth and the method suitable for volume production, overcome traditional rare earth permanent magnetism body processing technology face
The problem for the magnet specification limitation faced, and solve the diffusion consistency problem of heavy rare earth element in magnet, enhance expansion
Effect is dissipated, magnet obtains preferable magnetic property, and equipment investment is simple, and cost is relatively low, is suitable for large-scale promotion.
The method that high temperature compression disclosed by the invention improves rare earth permanent-magnetic material performance, this method include at least following step
It is rapid: to 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 a manner of stress infiltration by being realized on the shaped magnet of densification at a suitable temperature
The crystal boundary of heavy rare earth element in magnet is added, thus realize the controllability being distributed in magnet to heavy rare earth element, it is real
Show being uniformly distributed for heavy rare earth element in magnet, promoted the magnetic property of magnet, especially promotes the coercivity of magnet, and also
Reduce the dosage of heavy rare earth element.
High temperature compression disclosed by the invention improves a kind of improvement of the method for rare earth permanent-magnetic material performance, in 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
It carries out.Preferred protective gas atmosphere is one or more kinds of atmosphere in nitrogen, helium, argon gas etc..
High temperature compression disclosed by the invention improves a kind of improvement of the method for rare earth permanent-magnetic material performance, in this method,
Magnet surface attachment heavy rare earth compound is that heavy rare earth compound roll-in is attached to 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 way of high temperature roll-in
It is conveyed in body grain boundary structure, while compression plays a role in promoting, and avoids heavy rare earth atom (special because of the diffusion moveing freely
In the case of being prolonged free diffusing) main phase structure is entered, both improve heavy rare earth element in magnet and be distributed, has been promoted uniform
Property, it improves magnet mass and is conducive to improve production efficiency.
High temperature compression disclosed by the invention improves a kind of improvement of the method for rare earth permanent-magnetic material performance, in this method,
When magnet surface adheres to heavy rare earth compound, hard alloy roller is that thermalloy roller is not added, and heavy rare-earth solution passes through hard alloy roller
Surface roll-in is attached to magnet surface.This programme is by using the compacting environment that thermalloy roller and the entirety to magnet compacting is not added
Temperature control is carried out, so that the constructive difficulty of roller and the cost of production application are reduced, so that whole temperature environment is with 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 improves a kind of improvement of the method for rare earth permanent-magnetic material performance, in this method,
When magnet surface adheres to heavy rare earth compound, the magnet that surface is attached with 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. improves the osmotic efficiency to the inside of magnet, and have good to both be conducive to promote the seeping of heavy rare earth atom
Good compression restorability avoids the occurrence of deformation, realizes heavy rare earth atom uniformly penetrating in various sizes magnet, while keeping away again
Exempt from that temperature is excessively high the liquefaction of transition is occurred and magnet is deformed or heavy rare earth element is made to be pressed into main phase structure, and mistake
Low, unquestionable then can hinder to penetrate into activity, and the brittleness for being limited to magnet is prone to brittle damage.
High temperature compression disclosed by the invention improves a kind of improvement of the method for rare earth permanent-magnetic material performance, in this method,
Magnet surface adhere to heavy rare earth compound when, surface be attached with the compression of the magnet of heavy rare earth at high temperature be 50~
150kPa.This programme by suitable pressure size, both avoid the occurrence of stress it is excessive and cause to occur stress damage (as it is damaged,
Crackle, internal crystal phase dislocation etc.), meanwhile, additional stress power is provided for heavy rare earth element atom at appropriate temperatures, and
Increase osmotic efficiency, promote whole permeability, realizes heavy rare earth atom uniformly penetrating in various sizes magnet.
High temperature compression disclosed by the invention improves a kind of improvement of the method for rare earth permanent-magnetic material performance, in this method,
When magnet surface adheres to heavy rare earth compound, hard alloy roller is interior heating structure, 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 and to the temperature of magnet and alloy roller in different magnetic
The carry out Adaptive Control in the stage of body compacting promotes temperature controlled flexibility when processing, so that temperature is with good in processing
Good control accuracy, can greatly promote the osmotic efficiency and osmotic evenness of heavy rare earth atom, so that various rule
The magnet product of lattice size, which obtains, has the product quality optimized.
High temperature compression disclosed by the invention improves a kind of improvement of the method for rare earth permanent-magnetic material performance, in 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. improves the osmotic efficiency to the inside of magnet to both be conducive to promote the seeping of heavy rare earth atom, and
With good compression restorability, deformation is avoided the occurrence of, realizes heavy rare earth atom uniformly penetrating in various sizes magnet, together
When avoid again temperature it is excessively high there is the liquefaction of transition and make magnet deform or make heavy rare earth element be pressed into main phase knot
Structure, and too low, it is unquestionable then can hinder to penetrate into activity, and also the brittleness for being limited to magnet is prone to brittle damage.
High temperature compression disclosed by the invention improves a kind of improvement of the method for rare earth permanent-magnetic material performance, in 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
It is excessive and cause to occur stress damage (such as breakage, crackle, internal crystalline substance both to avoid the occurrence of stress by suitable pressure size for case
Phase dislocation etc.), meanwhile, additional stress power is provided for heavy rare earth element atom at appropriate temperatures, and increase infiltration effect
Rate promotes whole permeability, realizes heavy rare earth atom uniformly penetrating in various sizes magnet.
The implementation of the present invention program, magnet is after having temperature identical with hard alloy roller, then by hard alloy roller
Roll-in.In roll-in, by under compression and heat effect, conveying is mutually generated in magnet, is made by the compression that roller applies
The heavy rare earth atom for obtaining magnet surface is moved and is distributed in crystal boundary along pressure direction, the heavy rare earth atom distance mobile in crystal boundary
Pressure size that length and roller apply and related by the length of time of compression with magnet.This method can increase the expansion of magnet
Depth is dissipated, conducive to the higher magnet of thickness is prepared.Heavy rare earth atomic migration distance increase when, moderately increase compression size or
Person extends the time for applying compression or compression and afterburning time increases simultaneously.
High temperature compression disclosed by the invention improves a kind of improvement of the method for rare earth permanent-magnetic material performance, in this method,
Ageing treatment is also carried out after applying compression at high temperature.Preferably, when timeliness includes the level-one that temperature is 850 DEG C~950 DEG C
Effect, the secondary time effect that temperature is 450 DEG C~550 DEG C.Wherein level-one timeliness is vacuum infiltration process, while using higher timeliness
Temperature cooperates residual stress its purpose is that generating 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, the further diffusion in magnet is realized, so that heavy rare earth is in magnetic
It is evenly distributed in body.
It is ability that the method that high temperature compression disclosed by the invention improves rare earth permanent-magnetic material performance, which can also include other,
Processing step known to field technique personnel, such as rare-earth iron-boron material progress melting, hydrogen are broken, airflow milling, molding, sintering cause
Densification process technique, and be made with certain thickness magnet, and deoil, pickling, the aftertreatment technologies 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, microelement (copper, gallium, aluminium, zirconium, niobium etc.) and boron element: rare earth member here
Element can be billows, cerium, praseodymium, neodymium, terbium, dysprosium, at least one of holmium etc.；Transition elements can be iron and/or cobalt etc.；Microelement can
Think copper, gallium, aluminium, zirconium, at least one of niobium etc..
Heavy rare earth compound includes the hydride of the fluoride of dysprosium and/or terbium, the oxide of dysprosium and/or terbium, 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, providing one kind can be improved magnetic
Body diffusion depth and method suitable for volume production are carried out under the conditions of suitable high temperature pressure along magnet crystal boundary using heavy rare earth atom
Depth of penetration to overcome the problem for the magnet specification limitation that traditional rare earth permanent magnetism body processing technology faces, and solves
The diffusion consistency problem of heavy rare earth element, enhances diffusion effect, reduces magnet to the need of heavy rare earth element in magnet
It asks, magnet is made to obtain preferable magnetic property and reduces production cost, and equipment investment is simple, cost is relatively low, suitable for pushing away on a large scale
Extensively.
Detailed description of the invention
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 signs list:
1, magnet；2, hard alloy roller；3, heating device.
Specific embodiment
With reference to the accompanying drawings and detailed description, the present invention is furture elucidated, it should be understood that following specific embodiments are only
For illustrating the present invention rather than limiting the scope of the invention.It should be noted that word " preceding " used in the following description,
" rear ", "left", "right", "up" and "down" refer to that the direction in attached drawing, word "inner" and "outside" refer respectively to direction or remote
Direction from geometric center of specific component.
Embodiment 1
The present embodiment, the method that high temperature compression improves rare earth permanent-magnetic material performance include at least following steps: passing through
It is sintered obtained magnet surface attachment heavy rare earth compound, and by heating, applying compression at high temperature, obtains magnet.
It is distinguished with above-described embodiment, which improves 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
Either 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.
It is distinguished with above-described embodiment, which improves in the method for rare earth permanent-magnetic material performance: when heating
It is carried out under protective gas atmosphere.
It is distinguished with above-described embodiment, which improves in the method for rare earth permanent-magnetic material performance: in high temperature
It is carried out under protective gas atmosphere when lower application compression.
It is distinguished with above-described embodiment, which improves in the method for rare earth permanent-magnetic material performance: magnet table
It is carried out under protective gas atmosphere when heavy rare earth compound is adhered in face and when heating.
It is distinguished with above-described embodiment, which improves in the method for rare earth permanent-magnetic material performance: magnet table
It is carried out under protective gas atmosphere when the attachment heavy rare earth compound of face and when applying compression at high temperature.
It is distinguished with above-described embodiment, which improves in the method for rare earth permanent-magnetic material performance: when heating
It is carried out under protective gas atmosphere when applying compression at high temperature.
It is distinguished with above-described embodiment, which improves 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, carried out under protective gas atmosphere.
It is distinguished with above-described embodiment, which improves 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 to magnet surface by hard alloy roller.
It is distinguished with above-described embodiment, which improves in the method for rare earth permanent-magnetic material performance: magnet table
Face adhere to heavy rare earth compound when, hard alloy roller be not added thermalloy roller (alloy roller that thermalloy roller refers to not self-heating is not added,
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
After earth solution is attached to magnet surface processing by hard alloy roller surface roll-in, which accounts for magnet gross mass and is
It include but not limited to following any: 0.5%, its in 0.6%, 0.7%, 0.8%, 0.9%, 1% and 0.5~1% range
Its any value.
It is distinguished with above-described embodiment, which improves in the method for rare earth permanent-magnetic material performance: magnet table
Face adhere to heavy rare earth compound when, the magnet that surface is attached with heavy rare earth be heated to 750 DEG C (heating temperature can also be include and
Be not limited to following any: 760 DEG C, 770 DEG C, 780 DEG C, 790 DEG C, 800 DEG C, 810 DEG C, 820 DEG C, 830 DEG C, 840 DEG C, 850 DEG C,
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 within the scope of 911 DEG C, 925 DEG C, 936 DEG C, 948 DEG C, 754 DEG C and 750 DEG C~950 DEG C).
It is distinguished with above-described embodiment, which improves in the method for rare earth permanent-magnetic material performance: magnet table
When heavy rare earth compound is adhered in face, it is that 50kPa (may be used also by compression that surface, which is attached with the compression of the magnet of heavy rare earth at high temperature,
Think to include but 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 range
Interior other arbitrary values).
It is distinguished with above-described embodiment, which improves 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 structure, and heavy rare-earth solution passes through the roll-in of hard alloy roller surface
It is attached to magnet surface.
It is distinguished with above-described embodiment, which improves 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 temperature can also be
Include but not limited to following any: 760 DEG C, 770 DEG C, 780 DEG C, 790 DEG C, 800 DEG C, 810 DEG C, 820 DEG C, 830 DEG C, 840 DEG C,
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 within the scope 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).
It is distinguished with above-described embodiment, which improves 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 is that (compression can also be packet 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 range
Interior other arbitrary values).
It is distinguished with above-described embodiment, which improves in the method for rare earth permanent-magnetic material performance: in high temperature
Ageing treatment is also carried out after lower application compression.
It is distinguished with above-described embodiment, which improves in the method for rare earth permanent-magnetic material performance: timeliness packet
Include temperature be 850 DEG C (level-one aging temp can also be include but not limited to following any: 860 DEG C, 870 DEG C, 880 DEG C, 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 within the scope of 854 DEG C and 850 DEG C~950 DEG C) level-one timeliness, temperature be 550 DEG C (secondary aging temperature is also
It includes but not limited to following any for being: 460 DEG C, 470 DEG C, 480 DEG C, 490 DEG C, 500 DEG C, 510 DEG C, 520 DEG C, 530 DEG C,
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 ranges
Interior other arbitrary values) secondary time effect.
Distinguished with above-described embodiment, heavy rare earth compound be include but not limited to following at least one: dysprosium and/or terbium
Fluoride, the oxide of dysprosium and/or terbium, the hydride etc. of dysprosium and/or terbium 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, that is, include 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 have similar statement shape to the characterizing portion of heavy rare earth compound in the present invention program
Formula does explanation similar at this.
As shown in Figure 1, the magnet 1 that sintering obtains is coated with heavy rare-earth solution by surface under suitable hot environment
Hard alloy roller 2 (roller not self-heating) is suppressed by the suitable compression of certain time, to obtain high temperature compression
Improve rare earth permanent-magnetic material.
As shown in Fig. 2, the magnet 1 that sintering obtains, magnet 1 is heated by heating device 3 so as to have in roll-in with roll surface
Have identical temperature, under suitable hot environment, by surface be coated with heavy rare-earth solution hard alloy roller 2 (roller be from
Heating), it is suppressed by the suitable compression of certain time, so that obtaining high temperature compression improves rare earth permanent-magnetic material.
Below by way of for choosing a kind of common Nd-Fe-B permanent magnet (such as N35, but in being formulated heavy rare earth element addition
The present invention program is sampled, remaining raw material is using conventional method addition) illustrate the excellent place of the present invention program.
Specific embodiment one
The manufacturing method of rare-earth permanent magnet in the present embodiment is passed through by thinly slicing the neodymium iron boron magnetic body of preparation
Oil removing, pickling, drying and processing are 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 roller, it is taken out after cooling by magnet ageing treatment, acquisition 1 He of test specimens
Test specimens 2.
The preparation of above-mentioned neodymium iron boron magnetic body includes melting, and hydrogen is broken, airflow milling, molding, the processing such as sintering.Magnet is without excessively high
Warm hardening processing, and it is cut into the bulk square piece magnet (comparing using the magnet as original sample) of 50mm*60mm*10mm.
The thickness control of thin slice magnet is 10mm, and by oil removing, pickling keeps the rustless stain in 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 roller temperature be 900 DEG C.It is 50kPa that two 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%, accounts for magnet gross mass after this programme processing and is
1%.
It will be taken out after the cooling of above-mentioned magnet, be placed in ageing treatment in the sintering furnace that vacuum degree is 1*10-3Pa, level-one timeliness
Temperature is 900 DEG C, time 12h；Secondary aging temperature is 500 DEG C, time 4h.
Diffusion front and back magnet magnetic property value in 1 specific embodiment one of table.
By the comparison of upper table as can be seen that this method available surfacing in dysprosium fluoride solution adhesion process is uniform
The diffusion depth of dysprosium atom can be improved in coating during high temperature extrusion, is highly suitable for the heavy rare earth diffusion of thicker magnet,
Under the premise of remanent magnetism, magnetic energy product, Hk/Hci etc. are not reduced substantially, coercivity is greatly improved, and consistency is preferable,
Magnet squareness is higher.
Specific embodiment two:
The manufacturing method of rare-earth permanent magnet in the present embodiment is passed through by thinly slicing the neodymium iron boron magnetic body of preparation
Oil removing, pickling, drying and processing are dried heavy rare earth compound uniform adhesion in magnet surface by stainless steel roller through high temperature
Afterwards by stainless steel high temperature roller, applies certain compression, taken out after cooling by magnet ageing treatment, 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, molding, the processing such as sintering.Magnet is without excessively high
Warm hardening processing, and it is cut into the bulk square piece magnet (comparing using the magnet as original sample) of 50mm*60mm*10mm.
The thickness control of thin slice magnet is 10mm, and by oil removing, pickling keeps the rustless stain in 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 roller temperature be 900 DEG C.It is 50kPa that two rollers, which apply stress, rotates linear speed
Degree is 1m/min.
Being fluorinated the concentration of terbium alcoholic solution at normal temperatures and pressures is 40wt%, accounts for magnet gross mass after this programme processing and is
0.8%.
It will be taken out after the cooling of above-mentioned magnet, be placed in ageing treatment in the sintering furnace that vacuum degree is 1*10-3Pa, level-one timeliness
Temperature is 900 DEG C, time 12h；Secondary aging temperature is 500 DEG C, time 4h.
Diffusion front and back magnet magnetic property value in 2 specific embodiment two of table.
By the comparison of upper table as can be seen that the present invention program available surfacing in fluorination terbium solution adhesion process is equal
The diffusion depth of terbium atom can be improved in even coating during high temperature extrusion, and the heavy rare earth for being highly suitable for thicker magnet expands
It dissipates, under the premise of remanent magnetism, magnetic energy product, Hk/Hci etc. are not reduced substantially, coercivity is greatly improved, and consistency
Preferably, magnet squareness is higher.
Specific embodiment three
The manufacturing method of rare-earth permanent magnet in the present embodiment is passed through by thinly slicing the neodymium iron boron magnetic body of preparation
Oil removing, pickling, drying and processing are 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 roller, it is taken out after cooling by magnet ageing treatment, acquisition 1 He of test specimens
Test specimens 2.
The preparation of above-mentioned neodymium iron boron magnetic body includes melting, and hydrogen is broken, airflow milling, molding, the processing such as sintering.Magnet is without excessively high
Warm hardening processing, and it is cut into the bulk square piece magnet (comparing using the magnet as original sample) of 50mm*60mm*10mm.
The thickness control of thin slice magnet is 10mm, and by oil removing, pickling keeps the rustless stain in 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 roller temperature be 800 DEG C.It is 100kPa that two 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%, accounts for magnet gross mass after this programme processing and is
0.6%.
It will be taken out after the cooling of above-mentioned magnet, be placed in ageing treatment in the sintering furnace that vacuum degree is 1*10-3Pa, level-one timeliness
Temperature is 850 DEG C, time 10h；Secondary aging temperature is 550 DEG C, time 2h.
Diffusion front and back magnet magnetic property value in 3 specific embodiment three of table.
By the comparison of upper table as can be seen that this method available surfacing in dysprosium fluoride solution adhesion process is uniform
The diffusion depth of dysprosium atom can be improved in coating during high temperature extrusion, is highly suitable for the heavy rare earth diffusion of thicker magnet,
Under the premise of remanent magnetism, magnetic energy product, Hk/Hci etc. are not reduced substantially, coercivity is greatly improved, and consistency is preferable,
Magnet squareness is higher.
Specific embodiment four:
The manufacturing method of rare-earth permanent magnet in the present embodiment is passed through by thinly slicing the neodymium iron boron magnetic body of preparation
Heavy rare earth compound uniformly (solution morphology) is adhered to magnet surface by stainless steel roller by oil removing, pickling, drying and processing,
By stainless steel high temperature roller after high temperature is dried, applies certain compression, take out after cooling by magnet ageing treatment, surveyed
Sample 1 and test specimens 2.
The preparation of above-mentioned neodymium iron boron magnetic body includes melting, and hydrogen is broken, airflow milling, molding, the processing such as sintering.Magnet is without excessively high
Warm hardening processing, and it is cut into the bulk square piece magnet (comparing using the magnet as original sample) of 50mm*60mm*10mm.
The thickness control of thin slice magnet is 10mm, and by oil removing, pickling keeps the rustless stain in 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 roller temperature be 900 DEG C.It is 50kPa that two rollers, which apply stress, rotates linear speed
Degree is 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 the two, which accounts for magnet gross mass after this programme processing,.
It will be taken out after the cooling of above-mentioned magnet, be placed in ageing treatment in the sintering furnace that vacuum degree is 1*10-3Pa, level-one timeliness
Temperature is 900 DEG C, time 12h；Secondary aging temperature is 500 DEG C, time 4h.
Diffusion front and back magnet magnetic property value in 4 specific embodiment four of table.
By the comparison of upper table as can be seen that the present invention program can get table in dysprosia and terbium oxide solution adhesion process
The diffusion depth of dysprosium, terbium atom can be improved in the coating of face even uniform during high temperature extrusion, is highly suitable for thicker magnet
Heavy rare earth diffusion, under the premise of remanent magnetism, magnetic energy product, Hk/Hci etc. are not reduced substantially, coercivity has obtained very big mention
It rises, and consistency is preferable, magnet squareness is higher.
Comparative example:
The manufacturing method of rare-earth permanent magnet in the present embodiment is passed through by thinly slicing the neodymium iron boron magnetic body of preparation
Dysprosium fluoride (test specimens 1)/fluorination terbium (test specimens 2) is uniformly mixed with alcohol and is coated on magnet by oil removing, pickling, drying and processing
Surface, the ageing treatment after high temperature is dried.
In present case, the preparation of above-mentioned neodymium iron boron magnetic body includes melting, and hydrogen is broken, airflow milling, molding, the processing such as sintering.Magnetic
Body is handled without high-temperature aging, and is cut into the bulk square piece magnet of 50mm*60mm*10mm (using the magnet as original sample
It compares).
In the implementation case, the thickness control of thin slice magnet is 10mm, by oil removing, pickling, kept after drying surface without
Rust stain.
In present case, magnet is placed in ageing treatment in the sintering furnace that vacuum degree is 1*10-3Pa, and level-one aging temp is 900
DEG C, time 12h；Secondary aging temperature is 500 DEG C, time 4h.
Table 3
The magnet as can be seen that handling without the method for the present invention is compared by upper table, in remanent magnetism, magnetic energy product, Hk/Hci etc.
Reduction amplitude it is also big compared with the present invention program, coercivity promoted it is low compared with the application.
Show rather than with the comparison of comparative example to the present invention program protection scope for one to four through the foregoing embodiment
It limits, technical solution of the present invention improves the diffusion depth of heavy rare earth atom by heavy rare earth under high temperature extrusion, is highly suitable for
The heavy rare earth of thicker magnet is spread, so that coercivity obtains under the premise of remanent magnetism, magnetic energy product, Hk/Hci etc. are not reduced substantially
Very big promotion is arrived, and consistency is preferable, magnet squareness is higher.
This place embodiment is not exhaustive claimed midpoint of technical range and in embodiment technology
In scheme to single or multiple technical characteristics it is same replacement be formed by new technical solution, equally all the present invention claims
In the range of protection；Simultaneously the present invention program it is all enumerate or unlisted embodiment in, in the same embodiment each
Parameter is merely representative of an example (i.e. a kind of feasible scheme) for its technical solution, and between parameters and is not present stringent
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.
The technical means disclosed in the embodiments of the present invention is not limited to the technical means disclosed in the above technical means, and further includes
Technical solution consisting of any combination of the above technical features.The foregoing is a specific embodiment of the present invention, should refer to
Out, for those skilled in the art, without departing from the principle of the present invention, can also make several
Improvements and modifications, these modifications and embellishments are also considered to be within the scope of the present invention.
Claims (5)
1. a kind of method that high temperature compression improves rare earth permanent-magnetic material performance, this method includes at least following steps: passing through
It is sintered obtained magnet surface attachment heavy rare earth compound, and passes through heating, apply compression at high temperature, obtains magnet,
Middle magnet surface attachment heavy rare earth compound is that heavy rare earth compound roll-in is attached to magnet surface, magnetic by hard alloy roller
When heavy rare earth compound is adhered in body surface face, hard alloy roller is that thermalloy roller is not added, and heavy rare-earth solution passes through hard alloy roller table
Face roll-in is attached to magnet surface.
2. the method that high temperature compression according to claim 1 improves rare earth permanent-magnetic material performance, which is characterized 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, protecting
Atmosphere encloses lower progress.
3. the method that high temperature compression according to claim 1 improves rare earth permanent-magnetic material performance, which is characterized in that described
In method, when magnet surface adheres to heavy rare earth compound, the magnet that surface is attached with heavy rare earth is heated to 750 DEG C~950 DEG C.
4. the method that high temperature compression according to claim 1 improves rare earth permanent-magnetic material performance, which is characterized in that described
In method, when magnet surface adheres to heavy rare earth compound, it is 50 that surface, which is attached with the compression of the magnet of heavy rare earth at high temperature,
~150kPa.
5. the method that high temperature compression according to claim 1 to 4 improves rare earth permanent-magnetic material performance, feature exist
In, in the method, at high temperature apply compression after also carry out ageing treatment.
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| CN108372179A (en) * | 2017-12-28 | 2018-08-07 | 龙南县中利再生资源开发有限公司 | A kind of regeneration method of rare earth permanent-magnetic material |
| 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 |
| CN110473684B (en) * | 2019-08-19 | 2020-09-01 | 中国计量大学 | Preparation method of high-coercivity sintered neodymium-iron-boron magnet |
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