CN110444387A - A kind of preparation method of performance Nd Fe B sintered magnet - Google Patents
A kind of preparation method of performance Nd Fe B sintered magnet Download PDFInfo
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- CN110444387A CN110444387A CN201910765838.2A CN201910765838A CN110444387A CN 110444387 A CN110444387 A CN 110444387A CN 201910765838 A CN201910765838 A CN 201910765838A CN 110444387 A CN110444387 A CN 110444387A
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- neodymium iron
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- iron boron
- airflow milling
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229910001172 neodymium magnet Inorganic materials 0.000 claims abstract description 100
- 239000000843 powder Substances 0.000 claims abstract description 100
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims abstract description 88
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 64
- 238000003801 milling Methods 0.000 claims abstract description 59
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000001257 hydrogen Substances 0.000 claims abstract description 43
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 43
- 239000002994 raw material Substances 0.000 claims abstract description 40
- 238000010438 heat treatment Methods 0.000 claims abstract description 36
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 30
- 239000000956 alloy Substances 0.000 claims abstract description 30
- 238000002844 melting Methods 0.000 claims abstract description 30
- 230000008018 melting Effects 0.000 claims abstract description 30
- 229910000521 B alloy Inorganic materials 0.000 claims abstract description 20
- 238000000748 compression moulding Methods 0.000 claims abstract description 16
- 238000009826 distribution Methods 0.000 claims abstract description 16
- 238000000926 separation method Methods 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 15
- FMGSKLZLMKYGDP-USOAJAOKSA-N dehydroepiandrosterone Chemical class C1[C@@H](O)CC[C@]2(C)[C@H]3CC[C@](C)(C(CC4)=O)[C@@H]4[C@@H]3CC=C21 FMGSKLZLMKYGDP-USOAJAOKSA-N 0.000 claims abstract description 12
- 238000003723 Smelting Methods 0.000 claims abstract description 11
- 239000000470 constituent Substances 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims description 28
- 229910052796 boron Inorganic materials 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 21
- 239000012159 carrier gas Substances 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 18
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 15
- 238000000465 moulding Methods 0.000 claims description 15
- PXAWCNYZAWMWIC-UHFFFAOYSA-N [Fe].[Nd] Chemical compound [Fe].[Nd] PXAWCNYZAWMWIC-UHFFFAOYSA-N 0.000 claims description 7
- 239000000463 material Substances 0.000 abstract description 16
- 238000006356 dehydrogenation reaction Methods 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 22
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 12
- 229910052802 copper Inorganic materials 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 10
- 239000002184 metal Substances 0.000 description 10
- 229910052689 Holmium Inorganic materials 0.000 description 8
- 229910052779 Neodymium Inorganic materials 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 8
- 235000012054 meals Nutrition 0.000 description 8
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 8
- 102220076495 rs200649587 Human genes 0.000 description 8
- 102220043159 rs587780996 Human genes 0.000 description 8
- 229910001021 Ferroalloy Inorganic materials 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- 229910017052 cobalt Inorganic materials 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 229910052692 Dysprosium Inorganic materials 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/023—Hydrogen absorption
-
- 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
- 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
-
- 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
- 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
- B22F2009/044—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet milling
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a kind of preparation method of performance Nd Fe B sintered magnet, include the following steps: that (1) prepares raw material according to the constituent for the Sintered NdFeB magnet finally to be obtained；(2) raw material is fitted into smelting equipment and carries out alloy melting, obtain Nd Fe B alloys thin slice；(3) suction hydrogen crushing treatment is carried out to Nd Fe B alloys thin slice, is crushed later half dehydrogenation, obtain neodymium iron boron coarse powder；(4) airflow milling is carried out to neodymium iron boron coarse powder at low temperature, then carries out secondary cyclone separation, obtains the neodymium iron boron fine powder of even particle size distribution；(5) neodymium iron boron fine powder is pressed and molded under low temperature；(6) target product finally is obtained through oversintering, heat treatment.The present invention carries out half Dehydroepiandrosterone derivative during hydrogen breaking, to material, improves the brittleness and inoxidizability of coarse powder；And at low temperature carry out airflow milling, compression molding and etc., the magnetic property of the Sintered NdFeB magnet finally prepared significantly improves.
Description
Technical field
The invention belongs to rare-earth permanent-magnet material technical fields, and in particular to a kind of preparation of performance Nd Fe B sintered magnet
Method.
Background technique
Sintered NdFeB magnet is strongest a kind of magnetic material magnetic so far, is widely used in aerospace, vapour
Turner industry, electronic apparatus, medical instrument, energy-saving electric machine, new energy, field of wind power generation, be in the world today it is with fastest developing speed,
The best permanent-magnet material of market prospects.Sintered NdFeB magnet has high energy product, high-coercive force, high-energy density, high sexual valence
Than with the outstanding advantages such as good mechanical property, important role is acted as in high-technology field.
Develop by 30 years of researches, has basically formed alloy melting → hydrogen breaking → airflow milling → molding → burning
Knot → heat treatment Sintered NdFeB magnet production process route, realize N~TH a trade mark magnet of totally 7 major class more than 100 batch
Amount production and application, meet the requirement of numerous application fields.However, on the one hand, the magnet performance of prior art preparation
There are also biggish gaps for Distance Theory performance, and on the other hand, the performance of existing Sintered NdFeB magnet is not met by very much
The application demand of emerging application field.Therefore, it is also desirable to be innovated on the basis of prior art route, to further increase
The magnetic property of Sintered NdFeB magnet meets the application demand of more areas.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of preparations of performance Nd Fe B sintered magnet
Method.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of performance Nd Fe B sintered magnet, includes the following steps:
(1) raw material raw material preparation: is prepared according to the constituent for the Sintered NdFeB magnet finally to be obtained；
(2) alloy melting: raw material being fitted into smelting equipment and carries out alloy melting, obtains Nd Fe B alloys thin slice；
(3) hydrogen breaking: carrying out suction hydrogen crushing treatment to Nd Fe B alloys thin slice, carry out half Dehydroepiandrosterone derivative after inhaling hydrogen breaking,
Obtain neodymium iron boron coarse powder；The hydrogen content in neodymium iron boron coarse powder is controlled, the brittleness and inoxidizability of coarse powder are improved；
(4) airflow milling: cooling processing is carried out to airflow milling mill room, carrier gas and neodymium iron boron coarse powder, at low temperature to neodymium iron boron
Coarse powder carries out airflow milling, reduces powder size and oxygen content；Secondary cyclone separation is carried out to the powder after airflow milling, obtains granularity
The neodymium iron boron fine powder being evenly distributed；
(5) it forms: cooling processing being carried out to neodymium iron boron fine powder and molding die, is then pressed and molded at low temperature, improve
The neodymium iron boron fine powder degree of orientation；
(6) target product finally is obtained through oversintering, heat treatment.
Further scheme, in step (3), the hydrogen content of the neodymium iron boron coarse powder is 1800~3000ppm.
Further scheme, in step (3), temperature≤- 40 DEG C of airflow milling mill room after the cooling processing, carrier gas temperature
The temperature of neodymium iron boron coarse powder in room airflow milling mill room and is ground during airflow milling in≤- 60 DEG C, temperature≤- 40 DEG C of neodymium iron boron coarse powder
≤ -40 DEG C of degree.
Further scheme, in step (4), the particle diameter distribution of the neodymium iron boron fine powder of the even particle size distribution meet 3 μm≤
D50≤4 μm, D90/D10≤4.
Further scheme, in step (5), temperature≤- 40 DEG C of neodymium iron boron fine powder after the cooling processing, molding die
Temperature≤- 40 DEG C, during compression molding in molding die and die cavity neodymium iron boron fine powder temperature≤- 40 DEG C.
Further scheme, in step (6), the temperature of the sintering is 1030-1100 DEG C；The heat treatment includes including one
Grade heat treatment and two-stage are heat-treated two processes；Wherein, the temperature of level-one heat treatment is 850-900 DEG C, the temperature of second level heat treatment
Degree is 450-500 DEG C.
Compared with prior art, the beneficial effects of the present invention are:
(1) present invention carries out half Dehydroepiandrosterone derivative to material, controls the hydrogen content in neodymium iron boron coarse powder during hydrogen breaking
Neodymium iron is improved using the higher stronger feature of reproducibility with hydrogen of the brittleness of Nd Fe B alloys hydride for 1800~3000ppm
The brittleness and inoxidizability of boron coarse powder；
(2) this preparation method utilizes the Nd Fe B alloys feature that brittleness is higher, chemical activity is lower at low temperature, in low temperature
Under to neodymium iron boron coarse powder carry out airflow milling, can reduce powder size and oxygen content；And the powder after airflow milling is carried out secondary
Cyclonic separation, Control granularity distribution, improves powder uniformity, obtains the neodymium iron boron fine powder of even particle size distribution.
(3) present invention utilizes neodymium iron boron fine powder saturation magnetization and the higher feature of coercivity at low temperature, in low temperature
Lower compression molding, neodymium iron boron fine powder can be acted on by bigger external magnetic field power, and then improve the degree of orientation of powder, final to prepare
The magnetic property of Sintered NdFeB magnet significantly improve.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that
Described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the implementation in the present invention
Example, every other embodiment obtained by those of ordinary skill in the art without making creative efforts belong to
The scope of protection of the invention.
Embodiment 1
(1) the metallic iron Fe and boron that purity is 99.5wt% for the neodymium metal Nd of 99.5wt%, purity raw material preparation: are selected
The ferro-boron Fe-B that B content is 20wt% is raw material, is matched and is weighed each according to mass ratio Nd:Fe:B=31:68:1
Raw material；
(2) alloy melting: raw material being fitted into smelting equipment and carries out alloy melting, obtains Nd Fe B alloys thin slice；Wherein,
Copper roller revolving speed when alloy melting is 1m/s, and pouring temperature is 1400 DEG C；
(3) hydrogen breaking: carrying out suction hydrogen crushing treatment to Nd Fe B alloys thin slice, carry out half Dehydroepiandrosterone derivative after inhaling hydrogen breaking,
Neodymium iron boron coarse powder is obtained, controlling the hydrogen content in neodymium iron boron coarse powder is 2000ppm；
(4) airflow milling: cooling processing is carried out to airflow milling mill room, carrier gas and neodymium iron boron coarse powder using refrigerating plant, is cooled down
Airflow milling that treated mill room temperature is -45 DEG C, carrier gas temperature is -65 DEG C, neodymium iron boron meal temperatures are -45 DEG C, in airflow milling
In treatment process, mill room and temperature of charge≤- 40 DEG C are maintained；Secondary cyclone separation is carried out to the material after airflow milling, after separation
Obtaining particle diameter distribution is D50=3.4 μm, the neodymium iron boron fine powder of D90/D10=3.8；
(5) it forms: cooling processing is carried out to neodymium iron boron fine powder and molding die, after cooling processing, the temperature of neodymium iron boron fine powder
Degree is -45 DEG C, mold temperature is -45 DEG C, during compression molding, maintains temperature of charge≤- 40 DEG C in mold and die cavity, mould
The alignment magnetic field applied when molded is 2.0T；It is pressed and molded by low temperature, improves the neodymium iron boron fine powder degree of orientation；
(6) target product finally is obtained through oversintering, heat treatment；Wherein sintering temperature is 1030 DEG C, sintering time 5h；Heat
Processing includes level-one heat treatment and two-stage is heat-treated two processes, and the temperature of level-one heat treatment is 900 DEG C, time 3h, second level heat
The temperature of processing is 500 DEG C, time 3h.
Comparative example 1
(1) the metallic iron Fe and boron that purity is 99.5wt% for the neodymium metal Nd of 99.5wt%, purity raw material preparation: are selected
The ferro-boron Fe-B that B content is 20wt% is raw material, is matched and is weighed each according to mass ratio Nd:Fe:B=31:68:1
Raw material；
(1) alloy melting: raw material being fitted into smelting equipment and carries out alloy melting, obtains Nd Fe B alloys thin slice；Wherein,
Copper roller revolving speed when alloy melting is 1m/s, and pouring temperature is 1400 DEG C；
(2) hydrogen breaking: carrying out normal Dehydroepiandrosterone derivative to powder during hydrogen breaking, obtains neodymium iron boron coarse powder, controls neodymium iron
Hydrogen content in boron coarse powder is 900ppm；
(3) airflow milling: cooling processing is not carried out to airflow milling mill room, carrier gas and neodymium iron boron coarse powder, airflow milling grinds room temperature
For 25 DEG C, carrier gas temperature be 15 DEG C, neodymium iron boron meal temperatures are 25 DEG C, in airflow milling treatment process, maintains mill room and material
Temperature≤40 DEG C；Secondary cyclone separation is not carried out to the material after airflow milling, obtaining particle diameter distribution is D50=3.4 μm, D90/
The neodymium iron boron powder of D10=4.9；
(4) it forms: cooling processing not being carried out to neodymium iron boron powder and molding die, the temperature of neodymium iron boron fine powder is 25 DEG C,
Mold temperature is 25 DEG C, during compression molding, maintains temperature of charge≤40 DEG C in mold and die cavity, and when compression molding applies
Alignment magnetic field be 2.0T；
(5) target product finally is obtained through oversintering, heat treatment；Wherein sintering temperature is 1030 DEG C, sintering time 5h；Heat
Processing includes level-one heat treatment and two-stage is heat-treated two processes, and the temperature of level-one heat treatment is 900 DEG C, time 3h, second level heat
The temperature of processing is 500 DEG C, time 3h.
Embodiment 2
(1) raw material preparation: metallic iron Fe that purity is 99.5wt% for the neodymium metal Nd of 99.5wt%, purity, pure is selected
The ferro-boron Fe-B that the metal dysprosium Dy and boron content that degree is 99.5wt% are 20wt% is raw material, according to mass ratio Nd:Dy:
Fe:B=28:3:68:1 is matched and is weighed each raw material；
(2) alloy melting: raw material being fitted into smelting equipment and carries out alloy melting, obtains Nd Fe B alloys thin slice；Wherein,
Copper roller revolving speed when alloy melting is 1.1m/s, and pouring temperature is 1420 DEG C；
(3) hydrogen breaking: carrying out suction hydrogen crushing treatment to Nd Fe B alloys thin slice, carry out half Dehydroepiandrosterone derivative after inhaling hydrogen breaking,
Neodymium iron boron coarse powder is obtained, controlling the hydrogen content in neodymium iron boron coarse powder is 2300ppm；
(4) airflow milling: cooling processing is carried out to airflow milling mill room, carrier gas and neodymium iron boron coarse powder using refrigerating plant, is cooled down
Airflow milling that treated mill room temperature is -50 DEG C, carrier gas temperature is -65 DEG C, neodymium iron boron meal temperatures are -50 DEG C, in airflow milling
In treatment process, mill room and temperature of charge≤- 40 DEG C are maintained；Secondary cyclone separation is carried out to the material after airflow milling, after separation
Obtaining particle diameter distribution is D50=3.6 μm, the neodymium iron boron fine powder of D90/D10=3.8；
(5) it forms: cooling processing is carried out to neodymium iron boron fine powder and molding die, after cooling processing, the temperature of neodymium iron boron fine powder
Degree is -42 DEG C, mold temperature is -42 DEG C, during compression molding, maintains temperature of charge≤- 40 DEG C in mold and die cavity, mould
The alignment magnetic field applied when molded is 1.8T；It is pressed and molded by low temperature, improves the neodymium iron boron fine powder degree of orientation；
(6) target product finally is obtained through oversintering, heat treatment；Wherein sintering temperature is 1050 DEG C, sintering time 5h；Heat
Processing includes level-one heat treatment and two-stage is heat-treated two processes, and the temperature of level-one heat treatment is 900 DEG C, time 3h, second level heat
The temperature of processing is 500 DEG C, time 3h.
Comparative example 2
(1) raw material preparation: metallic iron Fe that purity is 99.5wt% for the neodymium metal Nd of 99.5wt%, purity, pure is selected
The ferro-boron Fe-B that the metal dysprosium Dy and boron content that degree is 99.5wt% are 20wt% is raw material, according to mass ratio Nd:Dy:
Fe:B=28:3:68:1 is matched and is weighed each raw material；；
(2) alloy melting: raw material being fitted into smelting equipment and carries out alloy melting, obtains Nd Fe B alloys thin slice；Wherein,
Copper roller revolving speed when alloy melting is 1.1m/s, and pouring temperature is 1420 DEG C；
(3) hydrogen breaking: carrying out normal Dehydroepiandrosterone derivative to powder during hydrogen breaking, obtains neodymium iron boron coarse powder, controls neodymium iron
Hydrogen content in boron coarse powder is 950ppm；
(4) airflow milling: cooling processing is not carried out to airflow milling mill room, carrier gas and neodymium iron boron coarse powder, airflow milling grinds room temperature
For 23 DEG C, carrier gas temperature be 18 DEG C, neodymium iron boron meal temperatures are 23 DEG C, in airflow milling treatment process, maintains mill room and material
Temperature≤40 DEG C；Secondary cyclone separation is not carried out to the material after airflow milling, obtaining particle diameter distribution is D50=3.6 μm, D90/
The neodymium iron boron powder of D10=4.8；
(5) it forms: cooling processing not being carried out to neodymium iron boron powder and molding die, the temperature of neodymium iron boron fine powder is 23 DEG C,
Mold temperature is 23 DEG C, during compression molding, maintains temperature of charge≤40 DEG C in mold and die cavity, and when compression molding applies
Alignment magnetic field be 1.8T；
(6) target product finally is obtained through oversintering, heat treatment；Wherein sintering temperature is 1050 DEG C, sintering time 5h；Heat
Processing includes level-one heat treatment and two-stage is heat-treated two processes, and the temperature of level-one heat treatment is 900 DEG C, time 3h, second level heat
The temperature of processing is 500 DEG C, time 3h.
Embodiment 3
(1) raw material preparation: metallic iron Fe that purity is 99.5wt% for the neodymium metal Nd of 99.5wt%, purity, pure is selected
Spend the holmium ferroalloy Ho- that the metallic cobalt Co for being 99.5wt%, the metallic copper Cu that purity is 99.5wt%, holmium Ho content are 80wt%
The ferro-boron Fe-B that Fe and boron content are 20% is raw material, according to Nd30Ho1Fe66.8Co1Cu0.2B1(wt.%) it is matched,
It is matched according to mass ratio Nd:Ho:Fe:Co:Cu:B=30:1:66.8:1:0.2:1 and weighs each raw material；
(2) alloy melting: raw material being fitted into smelting equipment and carries out alloy melting, obtains Nd Fe B alloys thin slice；Wherein,
Copper roller revolving speed when alloy melting is 1.1m/s, and pouring temperature is 1410 DEG C；
(3) hydrogen breaking: carrying out suction hydrogen crushing treatment to Nd Fe B alloys thin slice, carry out half Dehydroepiandrosterone derivative after inhaling hydrogen breaking,
Neodymium iron boron coarse powder is obtained, controlling the hydrogen content in neodymium iron boron coarse powder is 2500ppm；
(4) airflow milling: cooling processing is carried out to airflow milling mill room, carrier gas and neodymium iron boron coarse powder using refrigerating plant, is cooled down
Airflow milling that treated mill room temperature is -50 DEG C, carrier gas temperature is -65 DEG C, neodymium iron boron meal temperatures are -50 DEG C, in airflow milling
In treatment process, mill room and temperature of charge≤- 45 DEG C are maintained；Secondary cyclone separation is carried out to the material after airflow milling, after separation
Obtaining particle diameter distribution is D50=3.8 μm, the neodymium iron boron fine powder of D90/D10=3.6；
(5) it forms: cooling processing is carried out to neodymium iron boron fine powder and molding die, after cooling processing, the temperature of neodymium iron boron fine powder
Degree is -50 DEG C, mold temperature is -50 DEG C, during compression molding, maintains temperature of charge≤- 45 DEG C in mold and die cavity, mould
The alignment magnetic field applied when molded is 2.1T；It is pressed and molded by low temperature, improves the neodymium iron boron fine powder degree of orientation；
(6) target product finally is obtained through oversintering, heat treatment；Wherein sintering temperature is 1040 DEG C, sintering time 5h；Heat
Processing includes level-one heat treatment and two-stage is heat-treated two processes, and the temperature of level-one heat treatment is 900 DEG C, time 3h, second level heat
The temperature of processing is 480 DEG C, time 3h.
Comparative example 3
(1) raw material preparation: metallic iron Fe that purity is 99.5wt% for the neodymium metal Nd of 99.5wt%, purity, pure is selected
Spend the holmium ferroalloy Ho- that the metallic cobalt Co for being 99.5wt%, the metallic copper Cu that purity is 99.5wt%, holmium Ho content are 80wt%
The ferro-boron Fe-B that Fe and boron content are 20% is raw material, according to mass ratio Nd:Ho:Fe:Co:Cu:B=30:1:66.8:
1:0.2:1 is matched and is weighed each raw material；；
(2) alloy melting: raw material being fitted into smelting equipment and carries out alloy melting, obtains Nd Fe B alloys thin slice；Wherein,
Copper roller revolving speed when alloy melting is 1.1m/s, and pouring temperature is 1410 DEG C；
(3) hydrogen breaking: carrying out normal Dehydroepiandrosterone derivative to powder during hydrogen breaking, obtains neodymium iron boron coarse powder, controls neodymium iron
Hydrogen content in boron coarse powder is 880ppm；
(4) airflow milling: cooling processing is not carried out to airflow milling mill room, carrier gas and neodymium iron boron coarse powder, airflow milling grinds room temperature
For 28 DEG C, carrier gas temperature be 20 DEG C, neodymium iron boron meal temperatures are 28 DEG C, in airflow milling treatment process, maintains mill room and material
Temperature≤40 DEG C；Secondary cyclone separation is not carried out to the material after airflow milling, obtaining particle diameter distribution is D50=3.8 μm, D90/
The neodymium iron boron powder of D10=4.7；
(5) it forms: cooling processing not being carried out to neodymium iron boron powder and molding die, the temperature of neodymium iron boron fine powder is 28 DEG C,
Mold temperature is 28 DEG C, during compression molding, maintains temperature of charge≤40 DEG C in mold and die cavity, and when compression molding applies
Alignment magnetic field be 2.1T；
(6) target product finally is obtained through oversintering, heat treatment；Wherein sintering temperature is 1040 DEG C, sintering time 5h；Heat
Processing includes level-one heat treatment and two-stage is heat-treated two processes, and the temperature of level-one heat treatment is 900 DEG C, time 3h, second level heat
The temperature of processing is 480 DEG C, time 3h.
Embodiment 4
(1) raw material preparation: metallic iron Fe that purity is 99.5wt% for the neodymium metal Nd of 99.5wt%, purity, pure is selected
Spend metallic aluminium Al, the holmium Ho that the metallic cobalt Co for being 99.5wt%, the metallic copper Cu that purity is 99.5wt%, purity are 99.5wt%
The ferro-boron Fe-B that the holmium ferroalloy Ho-Fe and boron content that content is 80wt% are 20% is raw material, according to
Nd31Ho1Fe66.6Co1Cu0.2Al0.2B1(wt.%) after being matched, according to mass ratio Nd:Ho:Fe:Co:Cu:Al:B=31:1:
66.6:1:0.2:0.2:1 being matched and weighing each raw material；
(2) alloy melting: raw material being fitted into smelting equipment and carries out alloy melting, obtains Nd Fe B alloys thin slice；Wherein,
Copper roller revolving speed when alloy melting is 1.0m/s, and pouring temperature is 1400 DEG C；
(3) hydrogen breaking: carrying out suction hydrogen crushing treatment to Nd Fe B alloys thin slice, carry out half Dehydroepiandrosterone derivative after inhaling hydrogen breaking,
Neodymium iron boron coarse powder is obtained, controlling the hydrogen content in neodymium iron boron coarse powder is 2800ppm；
(4) airflow milling: cooling processing is carried out to airflow milling mill room, carrier gas and neodymium iron boron coarse powder using refrigerating plant, is cooled down
Airflow milling that treated mill room temperature is -55 DEG C, carrier gas temperature is -65 DEG C, neodymium iron boron meal temperatures are -55 DEG C, in airflow milling
In treatment process, mill room and temperature of charge≤- 50 DEG C are maintained；Secondary cyclone separation is carried out to the material after airflow milling, after separation
Obtaining particle diameter distribution is D50=3.6 μm, the neodymium iron boron fine powder of D90/D10=3.8；
(5) it forms: cooling processing is carried out to neodymium iron boron fine powder and molding die, after cooling processing, the temperature of neodymium iron boron fine powder
Degree is -55 DEG C, mold temperature is -55 DEG C, during compression molding, maintains temperature of charge≤- 50 DEG C in mold and die cavity, mould
The alignment magnetic field applied when molded is 2.0T；It is pressed and molded by low temperature, improves the neodymium iron boron fine powder degree of orientation；
(6) target product finally is obtained through oversintering, heat treatment；Wherein sintering temperature is 1030 DEG C, sintering time 5h；Heat
Processing includes level-one heat treatment and two-stage is heat-treated two processes, and the temperature of level-one heat treatment is 900 DEG C, time 3h, second level heat
The temperature of processing is 500 DEG C, time 3h.
Comparative example 4
(1) raw material preparation: metallic iron Fe that purity is 99.5wt% for the neodymium metal Nd of 99.5wt%, purity, pure is selected
Spend metallic aluminium Al, the holmium Ho that the metallic cobalt Co for being 99.5wt%, the metallic copper Cu that purity is 99.5wt%, purity are 99.5wt%
The ferro-boron Fe-B that the holmium ferroalloy Ho-Fe and boron content that content is 80wt% are 20% is raw material, according to mass ratio Nd:
Ho:Fe:Co:Cu:Al:B=31:1:66.6:1:0.2:0.2:1 is matched and is weighed each raw material；
(2) alloy melting: raw material being fitted into smelting equipment and carries out alloy melting, obtains Nd Fe B alloys thin slice；Wherein,
Copper roller revolving speed when alloy melting is 1.0m/s, and pouring temperature is 1400 DEG C；
(3) hydrogen breaking: carrying out normal Dehydroepiandrosterone derivative to powder during hydrogen breaking, obtains neodymium iron boron coarse powder, controls neodymium iron
Hydrogen content in boron coarse powder is 980ppm；
(4) airflow milling: cooling processing is not carried out to airflow milling mill room, carrier gas and neodymium iron boron coarse powder, airflow milling grinds room temperature
For 20 DEG C, carrier gas temperature be 15 DEG C, neodymium iron boron meal temperatures are 20 DEG C, in airflow milling treatment process, maintains mill room and material
Temperature≤40 DEG C；Secondary cyclone separation is not carried out to the material after airflow milling, obtaining particle diameter distribution is D50=3.6 μm, D90/
The neodymium iron boron powder of D10=4.8；
(5) it forms: cooling processing not being carried out to neodymium iron boron powder and molding die, the temperature of neodymium iron boron fine powder is 20 DEG C,
Mold temperature is 20 DEG C, during compression molding, maintains temperature of charge≤30 DEG C in mold and die cavity, and when compression molding applies
Alignment magnetic field be 2.0T；
(6) target product finally is obtained through oversintering, heat treatment；Wherein sintering temperature is 1030 DEG C, sintering time 5h；Heat
Processing includes level-one heat treatment and two-stage is heat-treated two processes, and the temperature of level-one heat treatment is 900 DEG C, time 3h, second level heat
The temperature of processing is 500 DEG C, time 3h.
Using magnetism testing instrument, according to the requirement of GB/T 3217-2013 permanent magnetism (Hard Magnetic) material-magnetism test method,
Test embodiment 1, embodiment 2, embodiment 3, embodiment 4, comparative example 1, comparative example 2, right respectively under room temperature (23 ± 1 DEG C)
The magnetic property of Sintered NdFeB magnet prepared by ratio 3, comparative example 4, is listed in table 1.
The main magnetic property of 1 embodiment of table and comparative example magnet
In conclusion the main magnetic property of the Sintered NdFeB magnet prepared using technical solution of the present invention is significantly improved.
Although this specification is described in terms of embodiments, but not each embodiment only includes an independent skill
Art scheme, this description of the specification is merely for the sake of clarity, and those skilled in the art should be using specification as one
A entirety, the technical solutions in the various embodiments may also be suitably combined, formed it will be appreciated by those skilled in the art that other
Embodiment.Therefore the foregoing is merely the preferred embodiments of the application, not are used to limit the practical range of the application；It is i.e. all according to
The various equivalents that claims hereof range is done are the protection scope of the claim of this application.
Claims (7)
1. a kind of preparation method of performance Nd Fe B sintered magnet, characterized by the following steps:
(1) raw material raw material preparation: is prepared according to the constituent for the Sintered NdFeB magnet finally to be obtained；
(2) alloy melting: raw material being fitted into smelting equipment and carries out alloy melting, obtains Nd Fe B alloys thin slice；
(3) hydrogen breaking: suction hydrogen crushing treatment is carried out to Nd Fe B alloys thin slice, half Dehydroepiandrosterone derivative is carried out after inhaling hydrogen breaking, obtains
Neodymium iron boron coarse powder；
(4) airflow milling: cooling processing is carried out to airflow milling mill room, carrier gas and neodymium iron boron coarse powder, at low temperature to neodymium iron boron coarse powder
Carry out airflow milling；Secondary cyclone separation is carried out to the powder after airflow milling, obtains the neodymium iron boron fine powder of even particle size distribution；
(5) it forms: cooling processing being carried out to neodymium iron boron fine powder and molding die, is then pressed and molded at low temperature, improve neodymium iron
The boron fine powder degree of orientation；
(6) target product finally is obtained through oversintering, heat treatment.
2. preparation method according to claim 1, it is characterised in that: in step (3), the hydrogen content of the neodymium iron boron coarse powder
For 1800~3000ppm.
3. preparation method according to claim 1, it is characterised in that: in step (4), airflow milling is ground after the cooling processing
Temperature≤- 40 DEG C of room, temperature≤- 60 DEG C of carrier gas, neodymium iron boron coarse powder temperature≤- 40 DEG C, airflow milling during airflow milling
It grinds room and grinds temperature≤- 40 DEG C of neodymium iron boron coarse powder in room.
4. preparation method according to claim 1, it is characterised in that: in step (4), the neodymium iron of the even particle size distribution
The particle diameter distribution of boron fine powder meets 3 μm≤D50≤4 μm, D90/D10≤4.
5. preparation method according to claim 1, it is characterised in that: in step (5), neodymium iron boron is thin after the cooling processing
Temperature≤- 40 DEG C of powder, temperature≤- 40 DEG C of molding die, neodymium iron boron is thin in molding die and die cavity during compression molding
Temperature≤- 40 DEG C of powder.
6. preparation method according to claim 1, it is characterised in that: in step (6), the temperature of the sintering is 1030-
1100℃。
7. preparation method according to claim 1, it is characterised in that: in step (6), the heat treatment includes including level-one
Heat treatment and two-stage are heat-treated two processes；Wherein, the temperature of level-one heat treatment is 850-900 DEG C, the temperature of second level heat treatment
It is 450-500 DEG C.
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Denomination of invention: A preparation method for high-performance sintered neodymium iron boron magnets Effective date of registration: 20231012 Granted publication date: 20210723 Pledgee: Hefei Science and Technology Rural Commercial Bank Co.,Ltd. Lujiang Branch Pledgor: EARTH-PANDA ADVANCE MAGNETIC MATERIAL Co.,Ltd. Registration number: Y2023980060901 |