CN107240469A - One kind improves the coercitive preparation method of ndfeb magnet - Google Patents

One kind improves the coercitive preparation method of ndfeb magnet Download PDF

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Publication number
CN107240469A
CN107240469A CN201710545742.6A CN201710545742A CN107240469A CN 107240469 A CN107240469 A CN 107240469A CN 201710545742 A CN201710545742 A CN 201710545742A CN 107240469 A CN107240469 A CN 107240469A
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powder
rare earth
preparation
heavy rare
ndfeb magnet
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姜华
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Jingci Material Technology Co Ltd
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Jingci Material Technology Co Ltd
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B22F2003/026—Mold wall lubrication or article surface lubrication

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

The coercitive preparation method of ndfeb magnet is improved the invention discloses one kind, step includes：1) NbFeB sintered raw material are broken into coarse powder；2) coarse powder made from step 1 is carried out into air-flow to grind, powder is made；3) heavy rare earth metal powder is mixed with organic solvent, is configured to sticking solution；4) it will uniformly be applied on the inwall of mould, then pour into powder prepared by step 2 in the mould with the viscosity solution postponed；5) pressed compact；6) green compact are put into sintering furnace under the protection of nitrogen and by the sintering stove evacuation, pressure is 0.4~0.6Pa；7) sinter.Go out to be formed rich neodymium phase in crystal boundary the invention enables heavy rare earth metal, greatly improve coercivity, simultaneously as the rich neodymium containing heavy rare earth metal mutually only exists in crystal boundary and the outer layer of principal phase, so not reducing remanent magnetism substantially.This special preparation method can obtain the magnet of excellent performance.

Description

One kind improves the coercitive preparation method of ndfeb magnet
Technical field
The invention belongs to permanent magnet preparing technical field, more particularly to a kind of coercitive preparation side of raising ndfeb magnet Method.
Background technology
Permanent magnet is hard magnetic body, and the magnet of its magnetic can be kept for a long time, loss of excitation is difficult, is not easy to be magnetized.Thus, nothing By being in industrial production or in daily life one of the most frequently used muscle material of hard magnetic body.Neodymium iron boron magnetic body is also referred to as neodymium Magnet (Neodymium magnet), its chemical formula is Nd2Fe14B, is a kind of artificial permanent magnet, is low by iron and price Honest and clean, aboundresources, can stable supplying neodymium and boron element combine, can inexpensively manufacture, while the magnetic energy product of neodymium iron boron Can reach ferritic more than 10 times, thus, neodymium iron boron magnetic body is because its cost performance is excellent, under volume, density is high, excellent performance And it is widely used in the fields such as wind-powered electricity generation, motor, VCM, unmanned plane, and with the development of hybrid-electric car, have very in future Big development opportunity.At present, high-performance Ne-Fe-B permanent magnet is mainly prepared by sintering process, and wherein Zhou Shouzeng etc. exists《Sinter neodymium iron Boron rare earth permanent-magnetic material and technology》In disclose the fabrication processing of sintered Nd-Fe-B permanent magnet, mainly melting, powder processed, Five steps of compressing, isostatic pressed and sintering, specifically include that dispensing, melting, hydrogen is broken, powder processed, powder be orientated it is compressing, The steps such as isostatic pressed, vacuum-sintering.
With the development of the association areas such as air-conditioning, electric automobile, to the demand more and more higher of neodymium iron boron, and will in performance Higher requirement is asked, in the case where ensureing high remanent magnetism, very high coercivity requirement is needed again, for trades mark such as 52UH The production of magnet, is difficult to produce with traditional handicraft, and for some products, even if conventional method can be prepared Come, but cost is again very high.The present invention is based on a preparation method for solving the design of this problem.Now in order to prepare height Residual magnetism high-coercive force permanent magnet, traditional process is extremely difficult to.
The content of the invention
The problem of for being previously mentioned, the coercitive preparation method of ndfeb magnet, step are improved the invention provides one kind Including：
1) NbFeB sintered raw material are broken into coarse powder；
2) coarse powder made from step 1 is carried out into air-flow to grind, powder is made, the powder size is 2.0~4.0 μm；
3) heavy rare earth metal powder is mixed with organic solvent, is configured to sticking solution, the heavy rare earth metal powder Last percentage by weight is more than 50%；
4) it will uniformly be applied on the inwall of mould, then pour into powder prepared by step 2 with the viscosity solution postponed In the mould；
5) mould that will be equipped with powder is placed on the defined position of press, adds more than 13000Oe magnetic field, while being pressed System, the surface of the green compact of compacting is with one layer of solution containing heavy rare earth element；
6) green compact being put into sintering furnace under the protection of nitrogen and by the sintering stove evacuation, pressure is 0.4~ 0.6Pa；
7) sintering furnace is warming up to after 200~300 DEG C, is incubated 1~3h；
8) sintering furnace is warming up to after 500~650 DEG C, is incubated 1~3h；
9) sintering furnace is warming up to after 700~850 DEG C, is incubated 3~4h；
10) sintering furnace is warming up to pre-burning platform, 900~1000 DEG C of the pre-burning platform temperature is, insulation 3~ 5h；
11) sintering furnace is warming up to sintering platform, the sintering platform temperature is 1050~1100 DEG C, insulation 10~ 12h；
12) sintering furnace is cooled down to 80~100 DEG C, and Sintered NdFeB magnet is made.
Preferred scheme is：Heavy rare earth metal is ground into powder by the quick-fried processing of hydrogen.
Preferred scheme is：In step 12, argon gas air cooling is filled with.
Preferred scheme is：The density of green compact in step 5 is 3.5~5.5g/cm3。
Preferred scheme is：Sintering furnace temperature uniformity ± 5 DEG C.
Preferred scheme is：The heavy rare earth metal is heavy rare earth simple metal or the compound containing heavy rare earth metal.
Preferred scheme is：The heavy rare earth metal is Dy or Tb.
Preferred scheme is：The heavy rare earth metal is the compound containing Dy or Tb.
Preferred scheme is：In temperature-rise period, heating rate is 2~8 DEG C/min.
Preferred scheme is：The method that the air-flow is ground is：
1) pretreatment of raw material：In the hermetically sealed can that superfine powder is collected into stabilizing gas protection, addition 0.4 ‰~0.5 ‰ Antioxidant is mixed 1~2 hour；In the hermetically sealed can that difficult abrasive material is collected into stabilizing gas protection, then protected in stabilizing gas Airflow milling in grind to form particle mean size be 5~8 μm of powder, according to components by weight percent be 1 by superfine powder and difficult abrasive powders:1 ~1:4 ratio is well mixed, and obtains mixed-powder；
2) sieve：By step 1) in mixed-powder put into sieve mesh number be 150~200 mesh ultrasonic wave sieving machine in carry out Sieving is handled, after processing terminates, and stands 5~8 hours；
3) it is compressing：The powder that sieving is handled well is put into the moulding press mould protected with stabilizing gas, Magnetic field intensity obtains pressed compact to be orientated and compressing under 1.4~2.0T alignment magnetic field.
Go out to be formed rich neodymium phase in crystal boundary the invention enables heavy rare earth metal, greatly improve coercivity, simultaneously as containing weight The rich neodymium of rare earth metal mutually only exists in crystal boundary and the outer layer of principal phase, so not reducing remanent magnetism substantially.The present invention can be with acquired The excellent magnet of energy.
Embodiment
The present invention is described in further detail below, to make those skilled in the art being capable of evidence with reference to specification word To implement.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or many The presence or addition of individual other elements or its combination.
Embodiment 1
A kind of raising coercitive preparation method of ndfeb magnet is present embodiments provided, step includes：
1) NbFeB sintered raw material are broken into coarse powder；
2) coarse powder made from step 1 is carried out into air-flow to grind, powder is made, the powder size is 2.0 μm；
3) crushing of the heavy rare earth metal Dy after the quick-fried processing of hydrogen is mixed with organic solvent, be configured to sticking molten Liquid, the heavy rare earth metal powder weight is more than 50%；
4) it will uniformly be applied on the inwall of mould, then pour into powder prepared by step 2 with the viscosity solution postponed In the mould；
5) mould that will be equipped with powder is placed on the defined position of press, adds more than 13000Oe magnetic field, while being pressed System, the density of green compact is 3.5g/cm3, the surface of the green compact of compacting is with one layer of solution containing heavy rare earth element；
6) green compact are put into sintering furnace under the protection of nitrogen and by the sintering stove evacuation, pressure is 0.4Pa, Sintering furnace temperature uniformity ± 5 DEG C, in temperature-rise period, heating rate is 2 DEG C/min；
7) sintering furnace is warming up to after 200 DEG C, is incubated 1h；
8) sintering furnace is warming up to after 500 DEG C, is incubated 1h；
9) sintering furnace is warming up to after 700 DEG C, is incubated 3h；
10) sintering furnace is warming up to pre-burning platform, 900 DEG C of the pre-burning platform temperature is to be incubated 3h；
11) sintering furnace is warming up to sintering platform, the sintering platform temperature is 1050 DEG C, is incubated 10h；
12) sintering furnace described in argon gas air cooling is filled with to 80 DEG C, and Sintered NdFeB magnet is made.The side that the air-flow is ground Method is：
1) pretreatment of raw material：By superfine powder be collected into stabilizing gas protection hermetically sealed can in, addition 0.4 ‰ ‰ it is anti-oxidation Agent is mixed 1 hour；In the hermetically sealed can that difficult abrasive material is collected into stabilizing gas protection, then in the airflow milling that stabilizing gas is protected It is 5 μm of powder to grind to form particle mean size, according to components by weight percent is 1 by superfine powder and difficult abrasive powders:1~1:4 ratio is mixed Close uniform, obtain mixed-powder；
2) sieve：By step 1) in mixed-powder put into sieve mesh number be 150 mesh ultrasonic wave sieving machine in sieved Processing, after processing terminates, stands 5 hours；
3) it is compressing：The powder that sieving is handled well is put into the moulding press mould protected with stabilizing gas, Magnetic field intensity obtains pressed compact to be orientated and compressing under 1.4T alignment magnetic field.
Magnetism testing is carried out to neodymium iron boron magnetic body prepared by above-mentioned steps, as a result referring to table 1, table 1 is implemented for the present invention Neodymium iron boron magnetic body magnetic property and composition correction data prepared by example 1.
Neodymium iron boron magnetic body magnetic property and composition correction data prepared by the embodiment of the present invention 1 of table 1
As can be seen from Table 1, coercivity shows the magnetic property of neodymium iron boron magnetic body manufactured in the present embodiment compared with the prior art Write and improve, remanent magnetism is slightly reduced.
Embodiment 2
A kind of raising coercitive preparation method of ndfeb magnet is present embodiments provided, step includes：
1) NbFeB sintered raw material are broken into coarse powder；
2) coarse powder made from step 1 is carried out into air-flow to grind, powder is made, the powder size is 4.0 μm；
3) crushing of the heavy rare earth metal DyTb after the quick-fried processing of hydrogen is mixed with organic solvent, be configured to sticking molten Liquid, the heavy rare earth metal powder weight is more than 50%；
4) it will uniformly be applied on the inwall of mould, then pour into powder prepared by step 2 with the viscosity solution postponed In the mould；
5) mould that will be equipped with powder is placed on the defined position of press, adds more than 13000Oe magnetic field, while being pressed System, the density of green compact is 5.5g/cm3, the surface of the green compact of compacting is with one layer of solution containing heavy rare earth element；
6) green compact are put into sintering furnace under the protection of nitrogen and by the sintering stove evacuation, pressure is 0.6Pa, Sintering furnace temperature uniformity ± 5 DEG C, in temperature-rise period, heating rate is 8 DEG C/min；
7) sintering furnace is warming up to after 300 DEG C, is incubated 3h；
8) sintering furnace is warming up to after 650 DEG C, is incubated 3h；
9) sintering furnace is warming up to after 850 DEG C, is incubated 4h；
10) sintering furnace is warming up to pre-burning platform, 1000 DEG C of the pre-burning platform temperature is to be incubated 5h；
11) sintering furnace is warming up to sintering platform, the sintering platform temperature is 1100 DEG C, is incubated 12h；
12) sintering furnace described in argon gas air cooling is filled with to 100 DEG C, and Sintered NdFeB magnet is made.
The method that the air-flow is ground is：
1) pretreatment of raw material：In the hermetically sealed can that superfine powder is collected into stabilizing gas protection, the antioxidant of addition 0.5 ‰ Mixing 2 hours；In the hermetically sealed can that difficult abrasive material is collected into stabilizing gas protection, then ground in the airflow milling that stabilizing gas is protected It is 8 μm of powder to wear into particle mean size, according to components by weight percent is 1 by superfine powder and difficult abrasive powders:4 ratio is well mixed, Obtain mixed-powder；
2) sieve：By step 1) in mixed-powder put into sieve mesh number be 200 mesh ultrasonic wave sieving machine in sieved Processing, after processing terminates, stands 8 hours；
3) it is compressing：The powder that sieving is handled well is put into the moulding press mould protected with stabilizing gas, Magnetic field intensity obtains pressed compact to be orientated and compressing under 2.0T alignment magnetic field.
Magnetism testing is carried out to neodymium iron boron magnetic body prepared by above-mentioned steps, as a result referring to table 2, table 2 is implemented for the present invention Neodymium iron boron magnetic body magnetic property and composition correction data prepared by example 2.
Neodymium iron boron magnetic body magnetic property and composition correction data prepared by the embodiment of the present invention 2 of table 2
As can be seen from Table 2, coercivity shows the magnetic property of neodymium iron boron magnetic body manufactured in the present embodiment compared with the prior art Write and improve, remanent magnetism is slightly reduced.
Embodiment 3
A kind of raising coercitive preparation method of ndfeb magnet is present embodiments provided, step includes：
1) NbFeB sintered raw material are broken into coarse powder；
2) coarse powder made from step 1 is carried out into air-flow to grind, powder is made, the powder size is 2.0 μm；
3) crushing of the compound containing Dy after the quick-fried processing of hydrogen is mixed with organic solvent, be configured to sticking molten Liquid, the heavy rare earth metal powder weight is more than 50%；
4) it will uniformly be applied on the inwall of mould, then pour into powder prepared by step 2 with the viscosity solution postponed In the mould；
5) mould that will be equipped with powder is placed on the defined position of press, adds more than 13000Oe magnetic field, while being pressed System, the density of green compact is 3.5g/cm3, the surface of the green compact of compacting is with one layer of solution containing heavy rare earth element；
6) green compact are put into sintering furnace under the protection of nitrogen and by the sintering stove evacuation, pressure is 0.4Pa, Sintering furnace temperature uniformity ± 5 DEG C, in temperature-rise period, heating rate is 2 DEG C/min；
7) sintering furnace is warming up to after 200 DEG C, is incubated 1h；
8) sintering furnace is warming up to after 500 DEG C, is incubated 1h；
9) sintering furnace is warming up to after 700 DEG C, is incubated 3h；
10) sintering furnace is warming up to pre-burning platform, 900 DEG C of the pre-burning platform temperature is to be incubated 3h；
11) sintering furnace is warming up to sintering platform, the sintering platform temperature is 1050 DEG C, is incubated 10h；
12) sintering furnace described in argon gas air cooling is filled with to 80 DEG C, and Sintered NdFeB magnet is made.
The method that the air-flow is ground is：
1) pretreatment of raw material：In the hermetically sealed can that superfine powder is collected into stabilizing gas protection, the antioxidant of addition 0.4 ‰ Mixing 1 hour；In the hermetically sealed can that difficult abrasive material is collected into stabilizing gas protection, then ground in the airflow milling that stabilizing gas is protected It is 5 μm of powder to wear into particle mean size, according to components by weight percent is 1 by superfine powder and difficult abrasive powders:1 ratio is well mixed, Obtain mixed-powder；
2) sieve：By step 1) in mixed-powder put into sieve mesh number be 150 mesh ultrasonic wave sieving machine in sieved Processing, after processing terminates, stands 5 hours；
3) it is compressing：The powder that sieving is handled well is put into the moulding press mould protected with stabilizing gas, Magnetic field intensity obtains pressed compact to be orientated and compressing under 1.4T alignment magnetic field.
Magnetism testing is carried out to neodymium iron boron magnetic body prepared by above-mentioned steps, as a result referring to table 3, table 3 is implemented for the present invention Neodymium iron boron magnetic body magnetic property correction data prepared by example 3.
Neodymium iron boron magnetic body magnetic property and composition correction data prepared by the embodiment of the present invention 3 of table 3
As can be seen from Table 3, the magnetic property of neodymium iron boron magnetic body prepared by this special preparation method is rectified compared with the prior art Stupid power is significantly improved, and remanent magnetism is slightly reduced.
Embodiment 4
A kind of raising coercitive preparation method of ndfeb magnet is present embodiments provided, step includes：
1) NbFeB sintered raw material are broken into coarse powder；
2) coarse powder made from step 1 is carried out into air-flow to grind, powder is made, the powder size is 4.0 μm；
3) crushing of the compound containing Tb after the quick-fried processing of hydrogen is mixed with organic solvent, be configured to sticking molten Liquid, the heavy rare earth metal powder weight is more than 50%；
4) it will uniformly be applied on the inwall of mould, then pour into powder prepared by step 2 with the viscosity solution postponed In the mould；
5) mould that will be equipped with powder is placed on the defined position of press, adds more than 13000Oe magnetic field, while being pressed System, the density of green compact is 5.5g/cm3, the surface of the green compact of compacting is with one layer of solution containing heavy rare earth element；
6) green compact are put into sintering furnace under the protection of nitrogen and by the sintering stove evacuation, pressure is 0.6Pa, Sintering furnace temperature uniformity ± 5 DEG C, in temperature-rise period, heating rate is 8 DEG C/min；
7) sintering furnace is warming up to after 300 DEG C, is incubated 3h；
8) sintering furnace is warming up to after 650 DEG C, is incubated 3h；
9) sintering furnace is warming up to after 850 DEG C, is incubated 4h；
10) sintering furnace is warming up to pre-burning platform, 1000 DEG C of the pre-burning platform temperature is to be incubated 5h；
11) sintering furnace is warming up to sintering platform, 1100 DEG C of the sintering platform temperature is incubated 12h；
12) sintering furnace described in argon gas air cooling is filled with to 100 DEG C, and Sintered NdFeB magnet is made.
The method that the air-flow is ground is：
1) pretreatment of raw material：In the hermetically sealed can that superfine powder is collected into stabilizing gas protection, the antioxidant of addition 0.5 ‰ Mixing 2 hours；In the hermetically sealed can that difficult abrasive material is collected into stabilizing gas protection, then ground in the airflow milling that stabilizing gas is protected It is 8 μm of powder to wear into particle mean size, according to components by weight percent is 1 by superfine powder and difficult abrasive powders:4 ratio is well mixed, Obtain mixed-powder；
2) sieve：By step 1) in mixed-powder put into sieve mesh number be 200 mesh ultrasonic wave sieving machine in sieved Processing, after processing terminates, stands 8 hours；
3) it is compressing：The powder that sieving is handled well is put into the moulding press mould protected with stabilizing gas, Magnetic field intensity obtains pressed compact to be orientated and compressing under 2.0T alignment magnetic field.
Magnetism testing is carried out to neodymium iron boron magnetic body prepared by above-mentioned steps, as a result referring to table 4, table 4 is implemented for the present invention Neodymium iron boron magnetic body magnetic property correction data prepared by example 4.
Neodymium iron boron magnetic body magnetic property and composition correction data prepared by the embodiment of the present invention 4 of table 4
As can be seen from Table 4, the magnetic property of neodymium iron boron magnetic body prepared by this special preparation method is rectified compared with the prior art Stupid power is significantly improved, and remanent magnetism is slightly reduced.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited In specific details.

Claims (10)

1. one kind improves the coercitive preparation method of ndfeb magnet, it is characterised in that step includes：
1) NbFeB sintered raw material are broken into coarse powder；
2) coarse powder made from step 1 is carried out into air-flow to grind, powder is made, the powder size is 2.0~4.0 μm；
3) heavy rare earth metal powder is mixed with organic solvent, is configured to sticking solution, the heavy rare earth metal powder weight Measure percentage and be more than 50%；
4) it will uniformly be applied on the inwall of mould, then pour into powder prepared by step 2 described with the viscosity solution postponed In mould；
5) mould that will be equipped with powder is placed on the defined position of press, adds more than 13000Oe magnetic field, while suppressed, The surface of the green compact of compacting is with one layer of solution containing heavy rare earth element；
6) green compact being put into sintering furnace under the protection of nitrogen and by the sintering stove evacuation, pressure is 0.4~ 0.6Pa；
7) sintering furnace is warming up to after 200~300 DEG C, is incubated 1~3h；
8) sintering furnace is warming up to after 500~650 DEG C, is incubated 1~3h；
9) sintering furnace is warming up to after 700~850 DEG C, is incubated 3~4h；
10) sintering furnace is warming up to pre-burning platform, 900~1000 DEG C of the pre-burning platform temperature is to be incubated 3~5h；
11) sintering furnace is warming up to sintering platform, the sintering platform temperature is 1050~1100 DEG C, is incubated 10~12h；
12) sintering furnace is cooled down to 80~100 DEG C, and Sintered NdFeB magnet is made.
2. the raising coercitive preparation method of ndfeb magnet according to claim 1, it is characterised in that heavy rare earth metal Powder is ground into by the quick-fried processing of hydrogen.
3. the raising coercitive preparation method of ndfeb magnet according to claim 1, it is characterised in that in step 12, It is filled with argon gas air cooling.
4. the raising coercitive preparation method of ndfeb magnet according to claim 1, it is characterised in that in step 5 The density of green compact is 3.5~5.5g/cm3。
5. the raising coercitive preparation method of ndfeb magnet according to claim 1, it is characterised in that the sintering furnace Temperature uniformity ± 5 DEG C.
6. the raising coercitive preparation method of ndfeb magnet according to claim 1, it is characterised in that the heavy rare earth Metal is heavy rare earth simple metal or the compound containing heavy rare earth metal.
7. the raising coercitive preparation method of ndfeb magnet according to claim 6, it is characterised in that the heavy rare earth Metal is Dy or Tb.
8. the raising coercitive preparation method of ndfeb magnet according to claim 6, it is characterised in that the heavy rare earth Metal is the compound containing Dy or Tb.
9. the raising coercitive preparation method of ndfeb magnet according to claim 1, it is characterised in that in temperature-rise period In, heating rate is 2~8 DEG C/min.
10. the raising coercitive preparation method of ndfeb magnet according to claim 1, it is characterised in that the air-flow The method ground is：
1) pretreatment of raw material：In the hermetically sealed can that superfine powder is collected into stabilizing gas protection, the oxygen of addition 0.4 ‰~0.5 ‰ Agent is mixed 1~2 hour；In the hermetically sealed can that difficult abrasive material is collected into stabilizing gas protection, the gas then protected in stabilizing gas It is 5~8 μm of powder that particle mean size is ground to form in stream mill, according to components by weight percent is 1 by superfine powder and difficult abrasive powders:1~1:4 Ratio be well mixed, obtain mixed-powder；
2) sieve：By step 1) in mixed-powder put into sieve mesh number be 150~200 mesh ultrasonic wave sieving machine in sieved Processing, after processing terminates, stands 5~8 hours；
3) it is compressing：The powder that sieving is handled well is put into the moulding press mould protected with stabilizing gas, in magnetic field Intensity obtains pressed compact to be orientated and compressing under 1.4~2.0T alignment magnetic field.
CN201710545742.6A 2017-07-06 2017-07-06 One kind improves the coercitive preparation method of ndfeb magnet Pending CN107240469A (en)

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CN109192493A (en) * 2018-09-20 2019-01-11 北京科技大学 A kind of preparation method of high performance sintered neodymium-iron-boron permanent-magnet material

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CN103903823A (en) * 2012-12-26 2014-07-02 宁波金鸡强磁股份有限公司 Rare earth permanent magnetic material and preparation method thereof
CN105448444A (en) * 2014-12-03 2016-03-30 北京中科三环高技术股份有限公司 Method for preparing rare-earth permanent magnetic material with improved performance and rare-earth permanent magnetic material
CN105551789A (en) * 2016-02-04 2016-05-04 宁波韵升股份有限公司 Manufacturing method of rare earth permanent magnet
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CN101996721A (en) * 2009-08-11 2011-03-30 中国科学院宁波材料技术与工程研究所 Method for improving coercive force of sintered neodymium ferrum boron (NdFeB)
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