CN106935352B - A kind of complex phase magnetic material and preparation method - Google Patents
A kind of complex phase magnetic material and preparation method Download PDFInfo
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- CN106935352B CN106935352B CN201710133666.8A CN201710133666A CN106935352B CN 106935352 B CN106935352 B CN 106935352B CN 201710133666 A CN201710133666 A CN 201710133666A CN 106935352 B CN106935352 B CN 106935352B
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- 239000000696 magnetic material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 71
- 239000000843 powder Substances 0.000 claims abstract description 49
- 239000002131 composite material Substances 0.000 claims abstract description 42
- 239000008187 granular material Substances 0.000 claims abstract description 34
- 239000002245 particle Substances 0.000 claims abstract description 32
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052718 tin Inorganic materials 0.000 claims abstract description 27
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 25
- 229910052796 boron Inorganic materials 0.000 claims abstract description 18
- 239000011159 matrix material Substances 0.000 claims abstract description 18
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 90
- 229910045601 alloy Inorganic materials 0.000 claims description 49
- 239000000956 alloy Substances 0.000 claims description 49
- 239000006247 magnetic powder Substances 0.000 claims description 49
- 229910052742 iron Inorganic materials 0.000 claims description 47
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 30
- 239000001257 hydrogen Substances 0.000 claims description 30
- 229910052739 hydrogen Inorganic materials 0.000 claims description 30
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 25
- 239000004615 ingredient Substances 0.000 claims description 25
- 238000002844 melting Methods 0.000 claims description 17
- 230000008018 melting Effects 0.000 claims description 17
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 230000006698 induction Effects 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 13
- 238000005496 tempering Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 229910052779 Neodymium Inorganic materials 0.000 claims description 10
- 238000005266 casting Methods 0.000 claims description 10
- 239000011812 mixed powder Substances 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- LBFUKZWYPLNNJC-UHFFFAOYSA-N cobalt(ii,iii) oxide Chemical compound [Co]=O.O=[Co]O[Co]=O LBFUKZWYPLNNJC-UHFFFAOYSA-N 0.000 claims description 9
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000000470 constituent Substances 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 238000010891 electric arc Methods 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 239000010959 steel Substances 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 238000003723 Smelting Methods 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 229910021281 Co3O4In Inorganic materials 0.000 claims 1
- 239000000284 extract Substances 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 abstract description 5
- 238000005259 measurement Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 230000010287 polarization Effects 0.000 abstract description 4
- 230000001737 promoting effect Effects 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000002156 mixing Methods 0.000 description 7
- 238000007670 refining Methods 0.000 description 7
- 239000010941 cobalt Substances 0.000 description 6
- 229910017052 cobalt Inorganic materials 0.000 description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 229910052761 rare earth metal Inorganic materials 0.000 description 5
- 229910000838 Al alloy Inorganic materials 0.000 description 4
- 238000007605 air drying Methods 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 239000011833 salt mixture Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002114 nanocomposite Substances 0.000 description 3
- 239000002159 nanocrystal Substances 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- 229910052692 Dysprosium Inorganic materials 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229910001004 magnetic alloy Inorganic materials 0.000 description 2
- 230000008520 organization Effects 0.000 description 2
- 238000007788 roughening Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
Classifications
-
- 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
-
- B22F1/0003—
-
- 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
-
- 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
- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
-
- 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
-
- 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
- C22C38/008—Ferrous alloys, e.g. steel alloys containing tin
-
- 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
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
-
- 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
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
-
- 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
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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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
- H01F1/12—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 soft-magnetic materials
- H01F1/34—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 soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/36—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 soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles
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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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- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention discloses a kind of complex phase magnetic material and preparation methods, by iron-base permanent-magnet powder, soft-magnetic powder-Co3O4Composite granule is sintered；The component and mass percent of the iron-base permanent-magnet dusty material matrix are as follows: Nd 22-25%, La 5-8%, B 3.0-5.3%, Sn 0.25-0.33%, Al 0.20-0.24%, surplus Fe；It is 0.1-0.4%TiN particle that weight percent is also distributed on the iron-base permanent-magnet dusty material matrix.Complex phase magnetic material provided by the invention has high remanent magnetic polarization, high density and high energy product.And comparative example measurement result is compared it can be found that the magnetic property of complex phase magnetic material of the present invention is related with the mass percent of each component.The complex phase magnetic material preparation method does not use your excessive dilute material, and at low cost, simple process is easy to operate, is suitable for promoting.
Description
Technical field
The invention belongs to functional composite material fields, and in particular to a kind of complex phase magnetic material and preparation method.
Background technique
CN201610671450.2 provides a kind of preparation method of Nanocomposite rare earth permanent-magnetic material, comprising the following steps:
Amorphous state magnetically hard alloy powder and amorphous soft magnetic alloy powder are provided；Keep amorphous state magnetically hard alloy powder crystallization nanocrystalline hard
Magnetic powder, and make amorphous soft magnetic alloy powder crystallization nano-crystal soft-magnetic powder；It is nanocrystalline by discharge plasma sintering
Hard Magnetic powder and nano-crystal soft-magnetic powder obtain Nanocomposite rare earth permanent-magnetic material.Nanocomposite rare earth permanent magnet material of the invention
The ratio of previously prepared nanocrystalline Hard Magnetic powder and the mixing of nano-crystal soft-magnetic powder can be effectively controlled in the preparation method of material, in turn
The variation range of magnetic property can accurately be controlled.But the performance of material and not up to certain application requirements.
Summary of the invention
For overcome the deficiencies in the prior art, an object of the present disclosure is to provide a kind of with excellent magnetic comprehensive performance
Complex phase magnetic material；The present invention second is designed to provide the preparation method of the complex phase magnetic material.
Above-mentioned purpose is achieved by the following technical solution:
A kind of complex phase magnetic material, by iron-base permanent-magnet powder, soft-magnetic powder-Co3O4Composite granule is sintered；It is iron-based forever
The component and mass percent of magnetic powder material matrix are as follows: Nd 22-25%, La 5-8%, B 3.0-5.3%, Sn 0.25-
0.33%, Al 0.20-0.24%, surplus Fe；It is 0.1- that weight percent is also distributed on iron-base permanent-magnet dusty material matrix
0.4%TiN particle.
Preferably, iron-base permanent-magnet powder, soft-magnetic powder-Co3O4The weight ratio of composite granule is 100:6-8.
Preferably, TiN particle average diameter 0.2-0.6 microns.
Preferably, soft-magnetic powder-Co3O4Iron base soft magnetic powder and cobalt oxide powder weight ratio are 5:1-3 in composite granule；It is iron-based
Each Ingredients Weight percentage composition in soft-magnetic powder material are as follows: 1-3%Al, 2-6%Si, 0.05-0.2%Co, 0.01-0.05%S,
Remaining is Fe.
The preparation method of above-mentioned complex phase magnetic material, comprising: press iron-base permanent-magnet powder, soft-magnetic powder-Co3O4Composite granule
Weight ratio ingredient, be then added in three-dimensional mixer be uniformly mixed, obtain mixed powder；By mixed powder in Magnetic field press
Orientation is formed using vertical steel mill pressure plus isostatic cool pressing mode；Molded blank is put into sintering furnace under protection of argon gas to burn
Knot is first warming up to 580-740 DEG C, keeps the temperature 2-4h, then heats to 1010-1060 DEG C of sintering 3-4h, after being cooled to room temperature, carries out
Double tempering processing, i.e., respectively 820-850 DEG C and 540-580 DEG C of tempering heat treatment 1-2h to get.
The iron-base permanent-magnet powder the preparation method comprises the following steps: according to each component mass percent carry out ingredient, Nd, La, Sn,
Al, Fe are pure metal, and for B with the addition of ferro-boron intermediate alloy, TiN particle is pure material；Raw material is put into electric arc furnaces copper crucible and is melted
Refining, smelting temperature are 1550-1580 DEG C, obtain mother alloy ingot after casting；Then mother alloy ingot is placed into common induction
Melting in furnace, smelting temperature are 1510-1530 DEG C, obtain master alloy liquid；Master alloy liquid is contacted to form band with chill roll
Material is obtained with high saturated magnetic induction microcrystallizing alloy thin-band material, wherein and the frequency of induction heating circle is 50-100kHz,
Chill roll and injector spacing are 0.2-0.6mm, and the linear velocity of chill roll wheel rim is 24-26m/s, thin-band material with a thickness of
50-80 microns, width 10-50mm；Above-mentioned thin-band material is placed in hydrogen broken furnace be evacuated to vacuum degree be 1Pa hereinafter,
It is passed through hydrogen at room temperature, keeps pressure in 2-3 × 105Pa, the time, cooling, then the remaining hydrogen of extraction, started to warm up in 3-5h
Dehydrogenation, dehydrogenating technology use 500-600 DEG C of heat preservation 4-6h, and dehydrogenation is forced down when 10Pa, and dehydrogenation terminates, and stop heating, cooling
To room temperature and dehydrogenation air pressure is controlled, so that hydrogen breaks powder hydrogen content between 2000-2500ppm after dehydrogenation, airflow milling after hydrogen is broken
The magnetic powder that average particle size is 3-4 μm is made in magnetic powder processed.
Preferably, described Nd, La, Sn, Al, Fe are the pure metal that constituent content is greater than 99.9%.
Preferably, the amount containing B of ferro-boron intermediate alloy is 24-26%.
Soft-magnetic powder-Co3O4Composite granule the preparation method comprises the following steps:
(1) first, in accordance in iron-based soft magnetic powder material each ingredient weight percentage carry out ingredient, raw material A l, Si, Co,
Fe is pure material, and S is added in a manner of iron sulphur intermediate alloy；The material prepared is put into melting in vacuum rapid hardening piece casting furnace, melting temperature
Degree is 1480-1580 DEG C, after obtaining master alloy solution, and aluminium alloy is poured onto the water cooling round roller rotated in furnace, the rotation linear speed of roller
Degree is 1-5m/s, and molten metal is cooled rapidly solidification, to make freezable liquid, forms the thin slice of microstructure, gained thin slice
Then thin slice is put into air-flow and grinds magnetic powder by thickness 0.5-1.2mm, the soft-magnetic powder that average particle size is 4-6 μm is made；
(2) 1:30 moles of Co (NO is weighed3)2·6H2O and NH4HCO3It is put into mortar, grinding 10-20min forming salt is mixed
Then soft-magnetic powder and salt mixture are mixed to form whole mixt by zoarium, and continue to grind 20-40min；It then will be whole
Mixture is successively washed through distilled water, ethyl alcohol, and natural air drying, which is placed in Muffle furnace, is heated to 240-250 DEG C, keeps 1-
To get soft-magnetic powder-Co after 3h3O4Composite granule.
Preferably, it is 15- that raw material A l, Si, Co, Fe purity, which is greater than 99.9%, S in the weight percent of iron sulphur intermediate alloy,
18%.
Beneficial effects of the present invention:
1, complex phase magnetic material of the present invention is sintered by iron-base permanent-magnet powder and soft-magnetic powder-oxidation cobalt composite powder, by
Iron-base permanent-magnet powder is surrounded in iron-based soft magnetic magnetic powder-oxidation cobalt composite powder dispersion；It is micro- that TiN is distributed on iron-base permanent-magnet dusty material matrix
Grain can separate iron-base permanent-magnet main phase.After oversintering, tempering, by the iron base soft magnetic powder and nonmetallic cobalt oxide powder packet of metal
It wraps up in outside iron-base permanent-magnet body of powder, iron-base permanent-magnet powder particle is separated from each other, crystal grain can not only effectively be inhibited to grow up roughening,
Crystal boundary is purified, moreover it is possible to which the consistency for greatly improving agglomerated material is prepared with high remanent magnetic polarization, high density and height
The complex phase magnetic material of magnetic energy product.TiN, iron-based soft magnetic magnetic powder-oxidation cobalt composite powder play the pinning effect for hindering crystal grain to grow up,
Prepare the tiny Ultra-fine Grained permanent-magnet material of crystal grain.Under conditions of not adding the heavy rare earth elements such as Dy, Tb, make material obtain compared with
High-performance.
2, complex phase magnetic material preparation method of the invention does not use your excessive dilute material, at low cost, simple process,
It is easy to operate, it is suitable for promoting.
Detailed description of the invention
Fig. 1 is the organization chart of complex phase magnetic material of the present invention, it can be seen that the dense structure of the complex phase magnetic material is uniform.
Specific embodiment
Technical solution of the present invention is specifically introduced below with reference to embodiment.
Embodiment 1:
A kind of complex phase magnetic material is by iron-base permanent-magnet powder and soft-magnetic powder-Co3O4Composite granule is sintered；It is described
The component and mass percent of iron-base permanent-magnet dusty material matrix are as follows: Nd 22%, La 5%, B 3.0%, Sn 0.25%, Al
0.20%, surplus Fe.It is 0.1%TiN particle that weight percent is also distributed on iron-base permanent-magnet dusty material matrix, particle
Average diameter is 0.2 micron.Soft-magnetic powder-Co3O4The weight ratio of iron base soft magnetic powder and cobalt oxide powder is 5:1 in composite granule.Iron
The weight percentage of each ingredient in base soft-magnetic powder material are as follows: 1%Al, 2%Si, 0.05%Co, 0.01%S, remaining is Fe.This
Iron-base permanent-magnet powder, the soft-magnetic powder-Co of embodiment complex phase magnetic material3O4The weight ratio of composite granule is 100:6.
Preparation method
Iron-base permanent-magnet powder the preparation method comprises the following steps: according to each component mass percent carry out ingredient, Nd, La, Sn, Al, Fe
For pure metal, for B with the addition of ferro-boron intermediate alloy, TiN particle is pure material；Raw material is put into melting in electric arc furnaces copper crucible, is melted
Refining temperature is 1570 DEG C, and mother alloy ingot is obtained after casting；Then mother alloy ingot is placed into melting in common induction furnace, melted
Refining temperature is 1520 DEG C, obtains master alloy liquid；Master alloy liquid is contacted to form band with chill roll, obtains that there is high saturation
Magnetic induction intensity microcrystallizing alloy thin-band material, wherein the frequency of induction heating circle is 80kHz, and chill roll and injector spacing are
0.4mm, the linear velocity of chill roll wheel rim are 25m/s, thin-band material with a thickness of 70 microns, width 30mm；It will be above-mentioned
It is 1Pa hereinafter, being passed through hydrogen under room temperature (24-26 DEG C, similarly hereinafter) that thin-band material, which is placed in hydrogen broken furnace and is evacuated to vacuum degree, is protected
Pressure is held 2.5 × 105Pa, the time, cooling, then the remaining hydrogen of extraction, started to warm up dehydrogenation, and dehydrogenating technology uses in 4h
550 DEG C of heat preservation 5h, dehydrogenation are forced down when 10Pa, and dehydrogenation terminates, and are stopped heating, are cooled to room temperature and control dehydrogenation air pressure,
So that hydrogen breaks powder hydrogen content between 2000-2500ppm after dehydrogenation, air-flow grinds magnetic powder after hydrogen is broken, that is, average particle size, which is made, is
3-4 μm of magnetic powder.Nd, La, Sn, Al, Fe are the pure metal that constituent content is greater than 99.9%.The amount containing B of ferro-boron intermediate alloy is
Within the scope of 25%, 24-26%.
Soft-magnetic powder-Co3O4Composite granule the preparation method comprises the following steps:
(1) first, in accordance in iron-based soft magnetic powder material each ingredient weight percentage carry out ingredient, raw material A l, Si, Co,
Fe is pure material, and S is added in a manner of iron sulphur intermediate alloy；The material prepared is put into melting in vacuum rapid hardening piece casting furnace, melting temperature
Degree is 1530 DEG C, after obtaining master alloy solution, and aluminium alloy is poured onto the water cooling round roller rotated in furnace, and the rotation linear velocity of roller is
3m/s, molten metal is cooled rapidly solidification, to make freezable liquid, forms the thin slice of microstructure, gained sheet thickness
Then thin slice is put into air-flow and grinds magnetic powder by 0.8mm, the soft-magnetic powder that average particle size is 4-6 μm is made；
(2) 1:30 moles of Co (NO is weighed3)2·6H2O and NH4HCO3It is put into mortar, grinding 15min forming salt mixing
Then soft-magnetic powder and salt mixture are mixed to form whole mixt by body, and continue to grind 30min；Then by whole mixing
Object is successively washed through distilled water, ethyl alcohol, and natural air drying, which is placed in Muffle furnace, is heated to 245 DEG C, is kept after 2h to get soft
Magnetic magnetic powder-Co3O4Composite granule.Raw material A l, Si, Co, Fe purity is greater than 99.9%, S in the weight percent of iron sulphur intermediate alloy
For within the scope of 17%, 15-18%.
The preparation method of complex phase magnetic material includes: by iron-base permanent-magnet powder, soft-magnetic powder-Co3O4The weight of composite granule
Than ingredient, it is then added in three-dimensional mixer and is uniformly mixed, obtain mixed powder；Mixed powder is orientated in Magnetic field press,
It is formed using vertical steel mill pressure plus isostatic cool pressing mode；Molded blank is put into sintering furnace under protection of argon gas to be sintered, first
660 DEG C are warming up to, 3h is kept the temperature, then heats to 1040 DEG C of sintering 3.5h, after being cooled to room temperature, carries out double tempering processing, i.e.,
Respectively 835 DEG C and 560 DEG C of tempering heat treatment 1.5h to get.
Complex phase magnetic material organization chart is as shown in Figure 1, it can be seen that the dense structure of the complex phase magnetic material is uniform.
Embodiment 2:
A kind of complex phase magnetic material is by iron-base permanent-magnet powder and soft-magnetic powder-Co3O4Composite granule is sintered；It is described
The component and mass percent of iron-base permanent-magnet dusty material matrix are as follows: Nd 25%, La 8%, B 5.3%, Sn 0.33%, Al
0.24%, surplus Fe.It is 0.4%TiN particle that weight percent is also distributed on iron-base permanent-magnet dusty material matrix, particle
Average diameter is 0.6 micron.Soft-magnetic powder-Co3O4The weight ratio of iron base soft magnetic powder and cobalt oxide powder is 5:3 in composite granule.Iron
The weight percentage of each ingredient in base soft-magnetic powder material are as follows: 3%Al, 6%Si, 0.2%Co, 0.05%S, remaining is Fe.This
Iron-base permanent-magnet powder, the soft-magnetic powder-Co of embodiment complex phase magnetic material3O4The weight ratio of composite granule is 100:8.
Preparation method
Iron-base permanent-magnet powder the preparation method comprises the following steps: according to each component mass percent carry out ingredient, Nd, La, Sn, Al, Fe
For pure metal, for B with the addition of ferro-boron intermediate alloy, TiN particle is pure material；Raw material is put into melting in electric arc furnaces copper crucible, is melted
Refining temperature is 1570 DEG C, and mother alloy ingot is obtained after casting；Then mother alloy ingot is placed into melting in common induction furnace, melted
Refining temperature is 1520 DEG C, obtains master alloy liquid；Master alloy liquid is contacted to form band with chill roll, obtains that there is high saturation
Magnetic induction intensity microcrystallizing alloy thin-band material, wherein the frequency of induction heating circle is 80kHz, and chill roll and injector spacing are
0.4mm, the linear velocity of chill roll wheel rim are 25m/s, thin-band material with a thickness of 70 microns, width 30mm；It will be above-mentioned
It is 1Pa hereinafter, being passed through hydrogen under room temperature (24-26 DEG C, similarly hereinafter) that thin-band material, which is placed in hydrogen broken furnace and is evacuated to vacuum degree, is protected
Pressure is held 2.5 × 105Pa, the time, cooling, then the remaining hydrogen of extraction, started to warm up dehydrogenation, and dehydrogenating technology uses in 4h
550 DEG C of heat preservation 5h, dehydrogenation are forced down when 10Pa, and dehydrogenation terminates, and are stopped heating, are cooled to room temperature and control dehydrogenation air pressure,
So that hydrogen breaks powder hydrogen content between 2000-2500ppm after dehydrogenation, air-flow grinds magnetic powder after hydrogen is broken, that is, average particle size, which is made, is
3-4 μm of magnetic powder.Nd, La, Sn, Al, Fe are the pure metal that constituent content is greater than 99.9%.The amount containing B of ferro-boron intermediate alloy is
Within the scope of 25%, 24-26%.
Soft-magnetic powder-Co3O4Composite granule the preparation method comprises the following steps:
(1) first, in accordance in iron-based soft magnetic powder material each ingredient weight percentage carry out ingredient, raw material A l, Si, Co,
Fe is pure material, and S is added in a manner of iron sulphur intermediate alloy；The material prepared is put into melting in vacuum rapid hardening piece casting furnace, melting temperature
Degree is 1530 DEG C, after obtaining master alloy solution, and aluminium alloy is poured onto the water cooling round roller rotated in furnace, and the rotation linear velocity of roller is
3m/s, molten metal is cooled rapidly solidification, to make freezable liquid, forms the thin slice of microstructure, gained sheet thickness
Then thin slice is put into air-flow and grinds magnetic powder by 0.8mm, the soft-magnetic powder that average particle size is 4-6 μm is made；
(2) 1:30 moles of Co (NO is weighed3)2·6H2O and NH4HCO3It is put into mortar, grinding 15min forming salt mixing
Then soft-magnetic powder and salt mixture are mixed to form whole mixt by body, and continue to grind 30min；Then by whole mixing
Object is successively washed through distilled water, ethyl alcohol, and natural air drying, which is placed in Muffle furnace, is heated to 245 DEG C, is kept after 2h to get soft
Magnetic magnetic powder-Co3O4Composite granule.Raw material A l, Si, Co, Fe purity is greater than 99.9%, S in the weight percent of iron sulphur intermediate alloy
For within the scope of 17%, 15-18%.
The preparation method of complex phase magnetic material includes: by iron-base permanent-magnet powder, soft-magnetic powder-Co3O4The weight of composite granule
Than ingredient, it is then added in three-dimensional mixer and is uniformly mixed, obtain mixed powder；Mixed powder is orientated in Magnetic field press,
It is formed using vertical steel mill pressure plus isostatic cool pressing mode；Molded blank is put into sintering furnace under protection of argon gas to be sintered, first
660 DEG C are warming up to, 3h is kept the temperature, then heats to 1040 DEG C of sintering 3.5h, after being cooled to room temperature, carries out double tempering processing, i.e.,
Respectively 835 DEG C and 560 DEG C of tempering heat treatment 1.5h to get.
Embodiment 3:
A kind of complex phase magnetic material is by iron-base permanent-magnet powder and soft-magnetic powder-Co3O4Composite granule is sintered；It is described
The component and mass percent of iron-base permanent-magnet dusty material matrix are as follows: Nd 23%, La 7%, B 4%, Sn 0.28%, Al
0.22%, surplus Fe.It is 0.3%TiN particle that weight percent is also distributed on iron-base permanent-magnet dusty material matrix, particle
Average diameter is 0.4 micron.Soft-magnetic powder-Co3O4The weight ratio of iron base soft magnetic powder and cobalt oxide powder is 5:2 in composite granule.Iron
The weight percentage of each ingredient in base soft-magnetic powder material are as follows: 2%Al, 4%Si, 0.1%Co, 0.03%S, remaining is Fe.This
Iron-base permanent-magnet powder, the soft-magnetic powder-Co of embodiment complex phase magnetic material3O4The weight ratio of composite granule is 100:7.
Preparation method
Iron-base permanent-magnet powder the preparation method comprises the following steps: according to each component mass percent carry out ingredient, Nd, La, Sn, Al, Fe
For pure metal, for B with the addition of ferro-boron intermediate alloy, TiN particle is pure material；Raw material is put into melting in electric arc furnaces copper crucible, is melted
Refining temperature is 1570 DEG C, and mother alloy ingot is obtained after casting；Then mother alloy ingot is placed into melting in common induction furnace, melted
Refining temperature is 1520 DEG C, obtains master alloy liquid；Master alloy liquid is contacted to form band with chill roll, obtains that there is high saturation
Magnetic induction intensity microcrystallizing alloy thin-band material, wherein the frequency of induction heating circle is 80kHz, and chill roll and injector spacing are
0.4mm, the linear velocity of chill roll wheel rim are 25m/s, thin-band material with a thickness of 70 microns, width 30mm；It will be above-mentioned
It is 1Pa hereinafter, being passed through hydrogen under room temperature (24-26 DEG C, similarly hereinafter) that thin-band material, which is placed in hydrogen broken furnace and is evacuated to vacuum degree, is protected
Pressure is held 2.5 × 105Pa, the time, cooling, then the remaining hydrogen of extraction, started to warm up dehydrogenation, and dehydrogenating technology uses in 4h
550 DEG C of heat preservation 5h, dehydrogenation are forced down when 10Pa, and dehydrogenation terminates, and are stopped heating, are cooled to room temperature and control dehydrogenation air pressure,
So that hydrogen breaks powder hydrogen content between 2000-2500ppm after dehydrogenation, air-flow grinds magnetic powder after hydrogen is broken, that is, average particle size, which is made, is
3-4 μm of magnetic powder.Nd, La, Sn, Al, Fe are the pure metal that constituent content is greater than 99.9%.The amount containing B of ferro-boron intermediate alloy is
Within the scope of 25%, 24-26%.
Soft-magnetic powder-Co3O4Composite granule the preparation method comprises the following steps:
(1) first, in accordance in iron-based soft magnetic powder material each ingredient weight percentage carry out ingredient, raw material A l, Si, Co,
Fe is pure material, and S is added in a manner of iron sulphur intermediate alloy；The material prepared is put into melting in vacuum rapid hardening piece casting furnace, melting temperature
Degree is 1530 DEG C, after obtaining master alloy solution, and aluminium alloy is poured onto the water cooling round roller rotated in furnace, and the rotation linear velocity of roller is
3m/s, molten metal is cooled rapidly solidification, to make freezable liquid, forms the thin slice of microstructure, gained sheet thickness
Then thin slice is put into air-flow and grinds magnetic powder by 0.8mm, the soft-magnetic powder that average particle size is 4-6 μm is made；
(2) 1:30 moles of Co (NO is weighed3)2·6H2O and NH4HCO3It is put into mortar, grinding 15min forming salt mixing
Then soft-magnetic powder and salt mixture are mixed to form whole mixt by body, and continue to grind 30min；Then by whole mixing
Object is successively washed through distilled water, ethyl alcohol, and natural air drying, which is placed in Muffle furnace, is heated to 245 DEG C, is kept after 2h to get soft
Magnetic magnetic powder-Co3O4Composite granule.Raw material A l, Si, Co, Fe purity is greater than 99.9%, S in the weight percent of iron sulphur intermediate alloy
For within the scope of 17%, 15-18%.
The preparation method of complex phase magnetic material includes: by iron-base permanent-magnet powder, soft-magnetic powder-Co3O4The weight of composite granule
Than ingredient, it is then added in three-dimensional mixer and is uniformly mixed, obtain mixed powder；Mixed powder is orientated in Magnetic field press,
It is formed using vertical steel mill pressure plus isostatic cool pressing mode；Molded blank is put into sintering furnace under protection of argon gas to be sintered, first
660 DEG C are warming up to, 3h is kept the temperature, then heats to 1040 DEG C of sintering 3.5h, after being cooled to room temperature, carries out double tempering processing, i.e.,
Respectively 835 DEG C and 560 DEG C of tempering heat treatment 1.5h to get.
Comparative example 1: proportioning components are not in scope of design of the present invention
A kind of complex phase magnetic material is by iron-base permanent-magnet powder and soft-magnetic powder-Co3O4Composite granule is sintered；It is described
The component and mass percent of iron-base permanent-magnet dusty material matrix are as follows: Nd 20%, La 3%, B 2%, Sn 0.1%, Al
0.1%, surplus Fe.It is 0.05%TiN particle that weight percent is also distributed on iron-base permanent-magnet dusty material matrix, particle
Average diameter is 0.1 micron.Soft-magnetic powder-Co3O4The weight ratio of iron base soft magnetic powder and cobalt oxide powder is 5:0.5 in composite granule.
The weight percentage of each ingredient in iron-based soft magnetic powder material are as follows: 0.5%Al, 1%Si, 0.02%Co, 0.005%S, remaining is
Fe.Iron-base permanent-magnet powder, the soft-magnetic powder-Co of the present embodiment complex phase magnetic material3O4The weight ratio of composite granule is 100:4.
The preparation method is the same as that of Example 1.
Comparative example 2: proportioning components are not in scope of design of the present invention
A kind of complex phase magnetic material is by iron-base permanent-magnet powder and soft-magnetic powder-Co3O4Composite granule is sintered；It is described
The component and mass percent of iron-base permanent-magnet dusty material matrix are as follows: Nd 27%, La 10%, B 6%, Sn 0.6%, Al
0.3%, surplus Fe.It is 0.5%TiN particle that weight percent is also distributed on iron-base permanent-magnet dusty material matrix, particle
Average diameter is 0.8 micron.Soft-magnetic powder-Co3O4The weight ratio of iron base soft magnetic powder and cobalt oxide powder is 5:4 in composite granule.Iron
Base soft-magnetic powder material, the weight percentage of ingredient are as follows: 4%Al, 8%Si, 0.4%Co, 0.07%S, remaining is Fe.This reality
Apply iron-base permanent-magnet powder, the soft-magnetic powder-Co of a complex phase magnetic material3O4The weight ratio of composite granule is 100:10.
The preparation method is the same as that of Example 1.
Effect example:
Complex phase magnetic material is prepared according to the composition ratio and preparation method of embodiment 1-3 and comparative example 1-2.With
The measurement of NIM-10000 type magnetism testing instrument measures the magnetic property of above-mentioned complex phase magnetic material.
Test result see the table below.
Above-mentioned measurement result shows: complex phase magnetic material provided by the invention has high remanent magnetic polarization, high density
And high energy product.Be compared with comparative example measurement result it can be found that the magnetic property of complex phase magnetic material of the present invention with
The mass percent of each component is related.
Complex phase magnetic material of the present invention is sintered by iron-base permanent-magnet powder and soft-magnetic powder-oxidation cobalt composite powder, by iron
Iron-base permanent-magnet powder is surrounded in base soft-magnetic powder-oxidation cobalt composite powder dispersion；TiN particle is distributed on iron-base permanent-magnet dusty material matrix
Iron-base permanent-magnet main phase can be separated.After oversintering, tempering, wrapped up by the iron base soft magnetic powder and nonmetallic cobalt oxide powder of metal
To outside iron-base permanent-magnet body of powder, iron-base permanent-magnet powder particle is separated from each other, can not only effectively inhibit crystal grain to grow up roughening, only
Crystal boundary is changed, moreover it is possible to which the consistency for greatly improving agglomerated material is prepared with high remanent magnetic polarization, high density and high magnetic
The complex phase magnetic material of energy product.TiN, iron-based soft magnetic magnetic powder-oxidation cobalt composite powder play the pinning effect for hindering crystal grain to grow up, system
The standby tiny Ultra-fine Grained permanent-magnet material of crystal grain out.Under conditions of not adding the heavy rare earth elements such as Dy, Tb, obtain material higher
Performance.The complex phase magnetic material preparation method does not use your excessive dilute material, and at low cost, simple process is easy to operate, fits
In popularization.
Claims (7)
1. a kind of complex phase magnetic material, it is characterised in that: by iron-base permanent-magnet powder, iron-based soft magnetic magnetic powder-Co3O4Composite granule is burnt
It ties；The component and mass percent of the iron-base permanent-magnet dusty material matrix are as follows: Nd 22-25%, La 5-8%, B
3.0-5.3%, Sn 0.25-0.33%, Al 0.20-0.24%, surplus Fe；On the iron-base permanent-magnet dusty material matrix also
It is 0.1-0.4%TiN particle that weight percent, which is distributed with,；Wherein, iron-base permanent-magnet powder, iron-based soft magnetic magnetic powder-Co3O4Composite powder
The weight ratio of body is 100:6-8.
2. complex phase magnetic material according to claim 1, it is characterised in that: 0.2-0.6 microns of TiN particle average diameter.
3. complex phase magnetic material according to claim 1, it is characterised in that: iron-based soft magnetic magnetic powder-Co3O4In composite granule
The weight ratio of iron base soft magnetic powder and cobalt oxide powder is 5:1-3；The weight percentage of each ingredient in the iron-based soft magnetic powder material
Are as follows: 1-3%Al, 2-6%Si, 0.05-0.2%Co, 0.01-0.05%S, remaining is Fe.
4. the preparation method of any complex phase magnetic material of claim 1-3, it is characterised in that: press iron-base permanent-magnet powder, iron
Base soft-magnetic powder-Co3O4The weight ratio ingredient of composite granule is then added in three-dimensional mixer and is uniformly mixed, obtains mixed powder
Material；Mixed powder is orientated in Magnetic field press, is formed using vertical steel mill pressure plus isostatic cool pressing mode；Molded blank is existed
Argon gas protection down enters sintering furnace and is sintered, and is first warming up to 580-740 DEG C, keeps the temperature 2-4h, then heats to 1010-1060 DEG C
It is sintered 3-4h, carries out double tempering processing after cooling, i.e., respectively in 820-850 DEG C and 540-580 DEG C of tempering heat treatment 1-2h, i.e.,
?.
5. the preparation method according to claim 4, which is characterized in that the iron-base permanent-magnet powder the preparation method comprises the following steps: pressing
Ingredient is carried out according to each component mass percent, Nd, La, Sn, Al, Fe are pure metal, and B is with the addition of ferro-boron intermediate alloy, TiN particle
For pure material；Raw material is put into melting in electric arc furnaces copper crucible, smelting temperature is 1550-1580 DEG C, obtains master alloy after casting
Ingot casting；Then mother alloy ingot is placed into melting in common induction furnace, smelting temperature is 1510-1530 DEG C, obtains master alloy
Liquid；Master alloy liquid is contacted to form band with chill roll, is obtained with high saturated magnetic induction microcrystallizing alloy thin strip
Material, wherein the frequency of induction heating circle is 50-100kHz, and chill roll and injector spacing are 0.2-0.6mm, chill roll wheel rim
Linear velocity is 24-26m/s, thin-band material with a thickness of 50-80 microns, width 10-50mm；Above-mentioned thin-band material is set
It is 1Pa hereinafter, being passed through hydrogen that vacuum degree is evacuated in hydrogen broken furnace, keeps pressure 2 × 105-3×105Pa, the time is in 3-
5h, it is cooling, it then extracts remaining hydrogen out, starts to warm up dehydrogenation, dehydrogenating technology uses 500-600 DEG C of heat preservation 4-6h, dehydrogenation air pressure
When lower than 10Pa, dehydrogenation terminates, and stops heating, cools down and controls dehydrogenation air pressure, so that the broken powder hydrogen content of hydrogen exists after dehydrogenation
Between 2000-2500ppm, air-flow grinds magnetic powder after hydrogen is broken, that is, the magnetic powder that average particle size is 3-4 μm is made.
6. preparation method according to claim 5, it is characterised in that: described Nd, La, Sn, Al, Fe are greater than for constituent content
99.9% pure metal.
7. preparation method according to claim 5, it is characterised in that: the amount containing B of ferro-boron intermediate alloy is 24-26%.
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