CN108766753A - The preparation method of high energy product high-coercive force Sintered NdFeB magnet - Google Patents
The preparation method of high energy product high-coercive force Sintered NdFeB magnet Download PDFInfo
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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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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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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- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0266—Moulding; Pressing
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- 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
- H01F41/0273—Imparting anisotropy
Abstract
The invention discloses a kind of preparation methods of high energy product high-coercive force Sintered NdFeB magnet, including：By design ingredient composition, dispensing is smelting, rapid hardening slab, obtains rapid hardening slab；Neodymium iron boron slab broken, disproportionated reaction, airflow milling powder through hydrogen, obtain 0.5~10 μm of neodymium iron boron fine powder；Using thermal resistance vapor deposition method, Dy/Tb particles, Pr/Nd particle elementary particle stepped depositions or synchronize are deposited on neodymium iron boron fine powder；Gained has been coated to the compression moulding of neodymium iron boron fine powder magnetic field orientating, isostatic cool pressing, vacuum-sintering, the heat treatment of Dy/Tb particles, Pr/Nd particles, it is final to obtain high energy product high-coercive force neodymium iron boron magnetic body.The present invention is effectively increased the volume ratio of ferromagnetism phase, improves the distribution of crystal boundary Nd-rich phase, improve the utilization rate of heavy rare earth element, the magnetic energy product of magnet and coercivity is made to significantly improve by coating Pr/Nd and Dy/Tb thin layers in NdFeB magnetic powder surface recombination.
Description
Technical field
The present invention relates to a kind of rare earth permanent-magnetic material technologies of preparing, specifically, are related to a kind of high energy product high-coercive force burning
Tie the preparation method of neodymium iron boron magnetic body.
Background technology
Nd-Fe-B permanent magnet material is the rare earth application industry that China's rare-earth trade is paid close attention to the most, with the development of science and technology
Demand of the progress to high-performance Ne-Fe-B permanent-magnet material with technology is increasingly extensive.In order to improve remanent magnetism, the coercivity of neodymium iron boron
With applied at elevated temperature, commonly used approach is that a small amount of heavy rare earth element (such as Dy, Tb) or optimize technique refinement magnet is added
Crystal grain.
Currently, the method for reducing heavy rare earth usage amount includes mainly pairing gold process and grain boundary decision heavy rare earth element work
Skill.Pairing gold process is melting master alloying and the auxiliary alloy comprising heavy rare earth element respectively, is crushed powder processed, by master alloying fine powder and
Auxiliary alloyed powder mixes, is orientated compacting, is sintered according to the ratio, obtained Nd-Fe-B permanent magnet material, heavy rare earth element usage amount in the technique
It is still higher.Grain boundary decision heavy rare earth element technique is formed on neodymium iron boron surface by modes such as smearing, sprinkling, dipping and plated films
Heavy rare earth element is diffused to inside magnet through temperature grain diffusion and improves magnet coercive to reach by heavy rare earth element coating
Power achievees the purpose that use heavy rare earth on a small quantity；But the technique is only limitted to make relatively thin magnetic part that (thickness is usually no more than
5mm), in preparation (sintering) bulk magnet, coercivity promotes unobvious.
Currently, refinement magnet crystal grain method mainly by smelting process be added micro W, Mo, V, Ti, Ta, Zr,
The elements such as Nb, Co, Cr inhibit growing up for magnet crystal grain, but the uneven distributions such as segregation can occur in magnet for this dvielement, right
The inhibition that crystal grain is grown up is limited, and addition is excessively high, can produce serious influence to magnet performance.
The prior art uses physical vapour deposition (PVD), such as magnetron sputtering, electron beam evaporation, vacuum induction evaporation to coat neodymium iron
Boron powder and then (sintering) neodymium iron boron magnetic body is prepared, but is the utilization rate of material the shortcomings that magnetically controlled sputter method less than 50%；Electricity
Beamlet evaporation equipment is expensive, it is high to require vacuum and evaporating temperature；Although vacuum induction evaporates stock utilization close to 99%,
The disadvantage is that requiring high vacuum, temperature is low to cause evaporation rate relatively low.
Invention content
Technical problem solved by the invention is to provide a kind of preparation of high energy product high-coercive force Sintered NdFeB magnet
Method is effectively increased the volume ratio of ferromagnetism phase, changes by coating Pr/Nd and Dy/Tb thin layers in NdFeB magnetic powder surface recombination
Kind crystal boundary Nd-rich phase distribution, improves the utilization rate of heavy rare earth element, the magnetic energy product of magnet and coercivity is made to significantly improve.
Technical solution is as follows：
A kind of preparation method of high energy product high-coercive force Sintered NdFeB magnet, including：
By design ingredient composition, dispensing is smelting, rapid hardening slab, obtains rapid hardening slab；
Neodymium iron boron slab broken, disproportionated reaction, airflow milling powder through hydrogen, obtain 0.5~10 μm of neodymium iron boron fine powder；
Using thermal resistance vapor deposition method, by Dy/Tb particles, Pr/Nd particle elementary particle stepped depositions or synchronous deposition
On neodymium iron boron fine powder；
By gained coated Dy/Tb particles, the neodymium iron boron fine powder magnetic field orientating compression moulding of Pr/Nd particles, isostatic cool pressing,
Vacuum-sintering, heat treatment obtain neodymium iron boron magnetic body.
Further：Thermal resistance evaporation use heavy rare earth thermal resistance wire include the first deposition of elements and the second deposition of elements, first
Deposition of elements includes that either the second deposition of elements of Tb elements includes Pr Nd elements, the first deposition of elements and the second deposition to Dy
Element stepped depositions or synchronous deposition.
Further：Heavy rare earth thermal resistance wire includes the first deposition of elements thermal resistance wire and the second deposition of elements thermal resistance wire, and first is heavy
Product element thermal resistance wire is the simple metal or alloy for including element Dy either Tb；Second deposition of elements thermal resistance wire be element Pr or
Simple metal, alloy in Nd.
Further：It is respectively placed in thermal resistance vapor deposition apparatus by neodymium iron boron fine powder and by Dy/Tb, Pr/Nd thermal resistance wire, very
Reciprocal of duty cycle is 105Pa~102Pa；Under protective atmosphere, keep neodymium iron boron fine powder evenly dispersed；Heavy rare earth thermal resistance wire heating evaporation, will
Dy/Tb elements, Pr/Nd element depositions are on neodymium iron boron fine powder surface；It waits for that temperature is cooled to room temperature and takes out neodymium iron boron fine powder.
Further：The magnetic field intensity used when magnetic field orientating compression moulding is more than 1.5 teslas；It is used when isostatic cool pressing
Pressure is 100-200MPa；Sintering temperature keeps the temperature 2-5 hours, vacuum degree is higher than in sintering process between 980-1080 DEG C
5.0×10-2Pa；Heat treatment is divided to two sections of progress, 850-950 DEG C of level-one heat treatment temperature, 400-600 DEG C of two level heat treatment temperature.
Further：According to mass percent meter, dispensing includes：Pr-Nd：28-32%；Co：0-1.2%； Cu：0-
0.6%；Nb：0-0.6%；Ga：0-0.6%；B：The Fe of 0.9-1.2% and remaining content.
The technology of the present invention effect includes：
(1) present invention can make the crystal grain of Sintered NdFeB magnet be maintained at 5 microns hereinafter, in magnet ferromagnetism phase ratio
Raising helps to improve remanent magnetism, magnet coercivity significantly improves, and neodymium is also reduced while reducing heavy rare earth element usage amount
Iron boron magnet manufacturing cost.
(2) high fever that thermal resistance hydatogenesis is generated using metal internal resistance under high current effect directly melts source material,
To achieve the purpose that evaporation, advantage are can to carry out the evaporation of alloy material under partial vacuum, moment generates a large amount of metal vapours
Change particle, stock utilization reaches 100%, and equipment manufacturing cost is low, it can be achieved that low pressure, high current, high power operation, no heat transfer and
Thermal convection current process, heat loss are small.
(3) it uses thermal resistance hydatogenesis to coat neodymium iron boron fine powder, and then prepares (sintering) neodymium iron boron magnetic body, magnet can be made to rectify
Stupid power significantly improves, and refines magnet crystal grain, reduces heavy rare earth element usage amount and magnet manufacturing cost.
(4) in the preparation process of powder, covering material Dy/Tb can be improved magnetocrystalline anisotropy field, limit crystal grain or
Domain rotation improves coercivity；Another covering material Pr/Nd can increase (more) neodymium-rich phase at grain boundary, improve liquid-phase sintering work
Skill process improves low-temperature sintering trend, or reduces sintering temperature, to reduce the long main trend of crystal grain.
Specific implementation mode
Be described below and specific embodiments of the present invention be fully shown, with enable those skilled in the art to practice and
It reproduces.
The preparation method of high energy product high-coercive force Sintered NdFeB magnet, specifically includes following steps：
Step 1：By design ingredient composition, dispensing is smelting, rapid hardening slab, obtains rapid hardening slab；
According to by following masses percentage dispensing：Pr-Nd：28-32%；Co：0-1.2%；Cu：0-0.6%； Nb：0-
0.6%；Ga：0-0.6%；B：The Fe of 0.9-1.2% and remaining content.
Step 2：Neodymium iron boron slab broken, disproportionated reaction, airflow milling powder through hydrogen, it is thin to obtain 0.5~10 μm of neodymium iron boron
Powder；
Step 3：Using thermal resistance vapor deposition method, by Dy/Tb particles, Pr/Nd particles elementary particle substep or synchronize it is heavy
Product is on neodymium iron boron fine powder；
Heavy rare earth thermal resistance wire in thermal resistance evaporation includes the first deposition of elements and the second deposition of elements, the first deposition of elements packet
Dy/Tb elements are included, the second deposition of elements includes Pr/Nd elements, and the first deposition of elements and the second deposition of elements can deposit simultaneously,
It can also successively deposit.First deposition of elements is mixed using the arbitrary proportion of two kinds of elements of Dy or Tb；Second deposition of elements uses
The arbitrary proportion of two kinds of elements of Pr or Nd mixes.
It is respectively placed in thermal resistance vapor deposition apparatus by neodymium iron boron fine powder and by Dy/Tb, Pr/Nd thermal resistance wire, vacuum degree is
105Pa~102Pa；Under protective atmosphere, keep neodymium iron boron fine powder evenly dispersed；Heavy rare earth thermal resistance wire heating evaporation, by Dy/Tb members
Element, Pr/Nd element depositions are on neodymium iron boron fine powder surface；It waits for that temperature is cooled to room temperature and takes out neodymium iron boron fine powder.Heavy rare earth thermal resistance wire
Including the first deposition of elements thermal resistance wire and the second deposition of elements thermal resistance wire, the first deposition of elements thermal resistance wire be comprising element Dy or
The simple metal or alloy of Tb；Second deposition of elements thermal resistance wire is simple metal, alloy in element Pr or Nd.
In the preparation process of powder, covering material Pr/Nd increases (more) neodymium-rich phase at grain boundary, improves liquid sintering process,
Sintering temperature is reduced, plays the role of reducing the long main trend of crystal grain, has and significantly improve the coercitive effect of magnet；Another kind cladding
Material Dy/Tb improves magnetocrystalline anisotropy field, limits crystal grain or domain rotation, improves coercivity.
Step 4：Gained has been coated to the neodymium iron boron fine powder magnetic field orientating compression moulding, cold of Dy/Tb particles, Pr/Nd particles
Isostatic pressed, vacuum-sintering, heat treatment, it is final to obtain high energy product high-coercive force neodymium iron boron magnetic body.
The magnetic field intensity used when magnetic field orientating compression moulding is more than 1.5 teslas；The pressure used when isostatic cool pressing for
100-200MPa；Sintering temperature between 980-1080 DEG C, keep the temperature 2-5 hour, in sintering process vacuum degree be higher than 5.0 ×
10-2Pa.Heat treatment is divided to two sections of progress, and level-one heat treatment temperature is between 850-950 DEG C, and two level heat treatment temperature is between 400-600
℃。
Embodiment 1：
(1) according to by following masses percentage dispensing：Pr-Nd：29.8%；Co：0.8%；Cu：0.2%；Al：0.3%；
Nb：0.2%；Ga：0.2%；B：0.98% and remaining content Fe.
(2) in the raw material input vacuum rapid hardening slab stove prepared, be evacuated down under conditions of 1Pa be filled with Ar gas shieldeds into
Molten steel, is poured onto on the cooling copper roller of rotation by row heating fusing after refining, and it is about the casting of 0.2-0.4mm alloys to prepare thickness
Piece；Then through hydrogen is broken, disproportionated reaction, airflow milling powder prepare average particle size 2.9um magnetic powder；By Dy particles, Pr/Nd
Daughter element particle is synchronized using thermal resistance vapor deposition method and is deposited on neodymium iron boron fine powder, is controlled deposition process parameters, is passed through heat
Mass fraction in the method addition of resistance deposition to Dy and Pr/Nd in the magnetic powder for stating step preparation is respectively 0.2% He
0.2%；It is orientated simultaneously compression moulding in the magnetic field that magnetic field intensity is more than 1.5 teslas, the green compact after compression moulding are carried out true
Sky encapsulation, is then placed in isostatic pressing machine and is forced into 150-200MPa, keeps it further fine and close；Green compact after isostatic pressed are put into
It is sintered in vacuum sintering furnace, waits for that vacuum degree reaches 5 × 10-2Start to be promoted temperature when Pa to 400 DEG C, is kept for 2 hours, continued
800 DEG C are warming up to, keeps the temperature 2 hours, is finally warming up to 1050 DEG C, after keeping the temperature 4h, argon gas is filled with and is cooled to 50 DEG C or less；Then exist
High vacuum sintering furnace carries out split ag(e)ing heat treatment, 890 DEG C of first segment treatment temperature, and heat preservation is filled with 0.8 air after 2 hours
Press Ar air coolings to 50 DEG C or less；480 DEG C of second segment heat treatment temperature, heat preservation 3 hours it is air-cooled to 50 DEG C.
Embodiment 2：
(1) according to by following masses percentage dispensing：Pr-Nd：29.8%；Co：0.8%；Cu：0.2%；Al：0.3%；
Nb：0.2%；Ga：0.2%；B：0.98% and remaining content Fe.
(2) in the raw material input vacuum rapid hardening slab stove prepared, be evacuated down under conditions of 1Pa be filled with Ar gas shieldeds into
Molten steel, is poured onto on the cooling copper roller of rotation by row heating fusing after refining, and it is about the casting of 0.2-0.4mm alloys to prepare thickness
Piece；Then through hydrogen is broken, disproportionated reaction, airflow milling powder prepare average particle size 2.9um magnetic powder；By Dy particles, Pr/Nd
Daughter element particle is synchronized using thermal resistance vapor deposition method and is deposited on neodymium iron boron fine powder, and deposition process parameters are controlled, and control is heavy
Product technological parameter adds the mass fraction to Dy and Pr/Nd in the magnetic powder for stating step preparation by the method that thermal resistance deposits
Respectively 0.4% and 0.2%；Simultaneously compression moulding is orientated in the magnetic field that magnetic field intensity is more than 1.5 teslas, after compression moulding
Green compact carry out Vacuum Package, be then placed in isostatic pressing machine and be forced into 150-200MPa, keep its further fine and close；By isostatic pressed
Green compact afterwards are put into vacuum sintering furnace and are sintered, and wait for that vacuum degree reaches 5 × 10-2Start to be promoted temperature when Pa to 400 DEG C, protects
It holds 2 hours, is continuously heating to 800 DEG C, keep the temperature 2 hours, be finally warming up to 1050 DEG C, after keeping the temperature 4h, be filled with argon gas and be cooled to 50
DEG C or less；Then split ag(e)ing heat treatment, 890 DEG C of first segment treatment temperature are carried out in high vacuum sintering furnace, heat preservation is filled after 2 hours
Enter 0.8 atmospheric pressure Ar air cooling to 50 DEG C or less；480 DEG C of second segment heat treatment temperature, heat preservation 3 hours it is air-cooled to 50 DEG C.
Embodiment 3：
(1) according to by following masses percentage dispensing：Pr-Nd：29.8%；Co：0.8%；Cu：0.2%；Al：0.3%；
Nb：0.2%；Ga：0.2%；B：0.98% and remaining content Fe.
(2) it in the raw material input vacuum rapid hardening slab stove prepared, is evacuated down under conditions of 1Pa and is filled with the progress of Ar gas shieldeds
Molten steel, is poured onto on the cooling copper roller of rotation by heating fusing after refining, and it is about the casting of 0.2-0.4mm alloys to prepare thickness
Piece；Then through hydrogen is broken, disproportionated reaction, airflow milling powder prepare average particle size 2.9um magnetic powder；By Dy particles, Pr/Nd
Daughter element particle is synchronized using thermal resistance vapor deposition method and is deposited on neodymium iron boron fine powder, is controlled deposition process parameters, is passed through heat
Mass fraction in the method addition of resistance deposition to Dy and Pr/Nd in the magnetic powder for stating step preparation is respectively 0.2% He
0.4%；It is orientated simultaneously compression moulding in the magnetic field that magnetic field intensity is more than 1.5 teslas, the green compact after compression moulding are carried out true
Sky encapsulation, is then placed in isostatic pressing machine and is forced into 150-200MPa, keeps it further fine and close；Green compact after isostatic pressed are put into
It is sintered in vacuum sintering furnace, waits for that vacuum degree reaches 5 × 10-2Start to be promoted temperature when Pa to 400 DEG C, is kept for 2 hours, continued
800 DEG C are warming up to, keeps the temperature 2 hours, is finally warming up to 1050 DEG C, after keeping the temperature 4h, argon gas is filled with and is cooled to 50 DEG C or less；Then exist
High vacuum sintering furnace carries out split ag(e)ing heat treatment, 890 DEG C of first segment treatment temperature, and heat preservation is filled with 0.8 air after 2 hours
Press Ar air coolings to 50 DEG C or less；480 DEG C of second segment heat treatment temperature, heat preservation 3 hours it is air-cooled to 50 DEG C.
The property indices of Examples 1 to 3 are as shown in table 1.
Table 1
It should be understood that above description is only exemplary and explanatory, the present invention can not be limited, the present invention is simultaneously
It is not limited to the flow being described above, and various modifications and changes may be made without departing from the scope thereof.The present invention's
Range is only limited by the accompanying claims.
Claims (6)
1. a kind of preparation method of high energy product high-coercive force Sintered NdFeB magnet, including：
By design ingredient composition, dispensing is smelting, rapid hardening slab, obtains rapid hardening slab；
Neodymium iron boron slab broken, disproportionated reaction, airflow milling powder through hydrogen, obtain 0.5~10 μm of neodymium iron boron fine powder；
Using thermal resistance vapor deposition method, by Dy/Tb particles, Pr/Nd particle elementary particle stepped depositions or synchronizes and be deposited on neodymium
On iron boron fine powder；
Gained Dy/Tb particles, the neodymium iron boron fine powder magnetic field orientating compression moulding of Pr/Nd particles, isostatic cool pressing, vacuum have been coated into
Sintering, heat treatment, obtain neodymium iron boron magnetic body.
2. the preparation method of high energy product high-coercive force Sintered NdFeB magnet as described in claim 1, it is characterised in that：Thermal resistance
The heavy rare earth thermal resistance wire that evaporation uses includes the first deposition of elements and the second deposition of elements, and the first deposition of elements includes Dy or Tb
Element, the second deposition of elements include Pr Nd elements, the first deposition of elements and the second deposition of elements stepped depositions or synchronous heavy
Product.
3. the preparation method of high energy product high-coercive force Sintered NdFeB magnet as described in claim 1, it is characterised in that：Weight is dilute
Native thermal resistance wire includes the first deposition of elements thermal resistance wire and the second deposition of elements thermal resistance wire, and the first deposition of elements thermal resistance wire is to include member
The simple metal or alloy of plain Dy either Tb；Second deposition of elements thermal resistance wire is simple metal or conjunction of the element Pr either in Nd
Gold.
4. the preparation method of high energy product high-coercive force Sintered NdFeB magnet as described in claim 1, it is characterised in that：By neodymium
Iron boron fine powder and Dy/Tb, Pr/Nd thermal resistance wire are respectively placed in thermal resistance vapor deposition apparatus, vacuum degree 105Pa~102Pa；
Under protective atmosphere, keep neodymium iron boron fine powder evenly dispersed；Heavy rare earth thermal resistance wire heating evaporation, by Dy/Tb elements, Pr/Nd elements
It is deposited on neodymium iron boron fine powder surface；It waits for that temperature is cooled to room temperature and takes out neodymium iron boron fine powder.
5. the preparation method of high energy product high-coercive force Sintered NdFeB magnet as described in claim 1, it is characterised in that：Magnetic field
It is orientated the magnetic field intensity used when compression moulding and is more than 1.5 teslas；The pressure used when isostatic cool pressing is 100-200MPa；It burns
Junction temperature keeps the temperature 2-5 hours between 980-1080 DEG C, and vacuum degree is higher than 5.0 × 10 in sintering process-2Pa；Heat treatment is divided to two sections
It carries out, 850-950 DEG C of level-one heat treatment temperature, 400-600 DEG C of two level heat treatment temperature.
6. the preparation method of high energy product high-coercive force Sintered NdFeB magnet as described in claim 1, which is characterized in that according to
Mass percent meter, dispensing include：Pr-Nd：28-32%；Co：0-1.2%；Cu：0-0.6%；Nb：0-0.6%；Ga：0-
0.6%；B：The Fe of 0.9-1.2% and remaining content.
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| CN112435820A (en) * | 2020-11-18 | 2021-03-02 | 宁波金鸡强磁股份有限公司 | High-performance sintered neodymium-iron-boron magnet and preparation method thereof |
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