CN102136329A - Iron-based composite soft magnetic material and preparation method thereof - Google Patents
Iron-based composite soft magnetic material and preparation method thereof Download PDFInfo
- Publication number
- CN102136329A CN102136329A CN2011100814222A CN201110081422A CN102136329A CN 102136329 A CN102136329 A CN 102136329A CN 2011100814222 A CN2011100814222 A CN 2011100814222A CN 201110081422 A CN201110081422 A CN 201110081422A CN 102136329 A CN102136329 A CN 102136329A
- Authority
- CN
- China
- Prior art keywords
- powder
- iron
- atomizing
- borate
- particle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 239000000696 magnetic material Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 137
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims abstract description 34
- 239000011230 binding agent Substances 0.000 claims abstract description 24
- -1 boric acid ester Chemical class 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000004327 boric acid Substances 0.000 claims abstract description 13
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims description 63
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 48
- 239000000956 alloy Substances 0.000 claims description 48
- 229910045601 alloy Inorganic materials 0.000 claims description 48
- 239000003960 organic solvent Substances 0.000 claims description 37
- 239000005955 Ferric phosphate Substances 0.000 claims description 29
- 229940032958 ferric phosphate Drugs 0.000 claims description 29
- 229910000399 iron(III) phosphate Inorganic materials 0.000 claims description 29
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 238000000137 annealing Methods 0.000 claims description 19
- 238000000935 solvent evaporation Methods 0.000 claims description 17
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 claims description 14
- LGQXXHMEBUOXRP-UHFFFAOYSA-N tributyl borate Chemical compound CCCCOB(OCCCC)OCCCC LGQXXHMEBUOXRP-UHFFFAOYSA-N 0.000 claims description 13
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 9
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 239000011812 mixed powder Substances 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 7
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 6
- 150000002148 esters Chemical class 0.000 claims description 6
- AJSTXXYNEIHPMD-UHFFFAOYSA-N triethyl borate Chemical compound CCOB(OCC)OCC AJSTXXYNEIHPMD-UHFFFAOYSA-N 0.000 claims description 6
- BMQDAIUNAGXSKR-UHFFFAOYSA-N (3-hydroxy-2,3-dimethylbutan-2-yl)oxyboronic acid Chemical compound CC(C)(O)C(C)(C)OB(O)O BMQDAIUNAGXSKR-UHFFFAOYSA-N 0.000 claims description 4
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 4
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 4
- 229920000151 polyglycol Polymers 0.000 claims description 4
- 239000010695 polyglycol Substances 0.000 claims description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 3
- HJVAFZMYQQSPHF-UHFFFAOYSA-N 2-[bis(2-hydroxyethyl)amino]ethanol;boric acid Chemical compound OB(O)O.OCCN(CCO)CCO HJVAFZMYQQSPHF-UHFFFAOYSA-N 0.000 claims description 3
- ZZPNDIHOQDQVNU-UHFFFAOYSA-N 2-hydroxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane Chemical compound CC1(C)OB(O)OC1(C)C ZZPNDIHOQDQVNU-UHFFFAOYSA-N 0.000 claims description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 3
- BEIBCTXWWNQLRO-HPWRNOGASA-N B(O)(O)O.C(C)N(C(CCCCCCC\C=C/CCCCCCCC)=O)CC Chemical compound B(O)(O)O.C(C)N(C(CCCCCCC\C=C/CCCCCCCC)=O)CC BEIBCTXWWNQLRO-HPWRNOGASA-N 0.000 claims description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000005642 Oleic acid Substances 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- SLINHMUFWFWBMU-UHFFFAOYSA-N Triisopropanolamine Chemical group CC(O)CN(CC(C)O)CC(C)O SLINHMUFWFWBMU-UHFFFAOYSA-N 0.000 claims description 3
- WKQUFJLZDFIAKF-UHFFFAOYSA-N boric acid;propane-1,2,3-triol Chemical compound OB(O)O.OCC(O)CO.OCC(O)CO WKQUFJLZDFIAKF-UHFFFAOYSA-N 0.000 claims description 3
- POULHZVOKOAJMA-UHFFFAOYSA-M dodecanoate Chemical compound CCCCCCCCCCCC([O-])=O POULHZVOKOAJMA-UHFFFAOYSA-M 0.000 claims description 3
- 238000005984 hydrogenation reaction Methods 0.000 claims description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 3
- 229940070765 laurate Drugs 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 230000026731 phosphorylation Effects 0.000 claims description 3
- 238000006366 phosphorylation reaction Methods 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- WRECIMRULFAWHA-UHFFFAOYSA-N trimethyl borate Chemical compound COB(OC)OC WRECIMRULFAWHA-UHFFFAOYSA-N 0.000 claims description 3
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 238000005538 encapsulation Methods 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 229910000398 iron phosphate Inorganic materials 0.000 abstract description 5
- 238000004663 powder metallurgy Methods 0.000 abstract description 4
- 230000004907 flux Effects 0.000 abstract description 2
- 238000005461 lubrication Methods 0.000 abstract 5
- 238000010438 heat treatment Methods 0.000 description 16
- 238000001125 extrusion Methods 0.000 description 14
- 239000002994 raw material Substances 0.000 description 14
- 239000000203 mixture Substances 0.000 description 12
- 239000000314 lubricant Substances 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 5
- 230000035699 permeability Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000005253 cladding Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 229910000976 Electrical steel Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention belongs to the field of powder metallurgy, and relates to an iron-based composite soft magnetic material and a preparation method thereof using a powder metallurgy method to prepare soft magnetic parts of complex shapes in particular. The invention provides a composite soft magnetic material which takes an iron phosphate as an insulating compound and takes boric acid ester as a lubrication binder. The composite soft magnetic material consists of atomized iron-based powder, nanometer iron phosphate and the lubrication binder. The surfaces of the atomized iron-based powder articles are uniformly coated by a layer of nanometer iron phosphate and lubrication binder, wherein the lubrication binder is boric acid ester, and the lubrication binder is 0.01-1.5 percent of the atomized iron-based powder in percentage by weight; and the nanometer iron phosphate is 0.01-1.5 percent of the of the atomized iron-based powder in percentage by weight. The invention has simple preparation technique, low material cost, high density, and high magnetic flux density.
Description
Technical field
The invention belongs to field of powder metallurgy, be specifically related to a kind of iron-based compound soft magnetic material for preparing soft magnetic property parts with powder metallurgy process and preparation method thereof with complicated shape.
Background technology
Compare with traditional silicon steel stack technology, the soft magnetic powder metallurgical technology shows exclusive advantage when producing complicated form part.The parts of complicated shape can directly be produced after sintering process, and do not need expensive shaping processing, as turning, wash cut, boring or grinding etc.The soft magnetic material application is extensive, can be used for the stator of motor and the iron core of rotor, transformer and inductor etc.This material can be pressed knot after selecting examples of suitable lubricants and/or binding agent to coat iron-based powder, then heat treatment at a certain temperature or sintering.But selected lubricant is very crucial for the high density that realizes material and the pressed part demoulding.
Summary of the invention
The object of the present invention is to provide iron-based compound soft magnetic material of a kind of novel high-density, high magnetic strength and preparation method thereof, with ferric phosphate as insulating compound, borate as lubricated binding agent, can realize the demoulding that is easy to of the high density of material and pressed part.
In order to achieve the above object, the invention provides following technical scheme:
A kind of iron-based compound soft magnetic material is made up of atomizing iron-based powder, nano ferric phosphate and lubricated binding agent, and this atomizing iron-based powder particle surface evenly coats this nano ferric phosphate particle of one deck and lubricated binding agent; Wherein said lubricated binding agent is that borate is lubricated, and quality is the 0.01-1.5% of atomizing iron-based powder quality; The nano ferric phosphate quality is the 0.01-1.5% of atomizing iron-based powder quality.
Described atomizing iron-based powder is atomizing straight iron powder, atomizing iron nickel powder or its mixed powder, and the quality of atomizing iron nickel powder accounts for ratio≤9% of atomizing ferrous alloy powder quality in wherein atomize straight iron powder and the atomizing iron nickel powder mixed powder.
The particle size range of described atomizing iron-based powder satisfies: at least 30%, preferred at least 50% atomizing iron-based powder is made up of the particle that particle diameter surpasses 200 μ m, and particle diameter is greater than particle≤5% of 400 μ m, powder particle≤10% of particle diameter below 10 μ m.
Described nano ferric phosphate grain diameter≤100nm, preferred 10-50nm.
Described lubricated binding agent is a kind of in the following compounds:
Butyl borate, boric acid three n-propyls, triethyl borate, trimethylborate, the polyethylene glycol borate, the triethanolamine borate, triisopropanolamine ring borate, triisopropyl borate ester, the oleic acid diethyl amide borate, the poly glycol monomethyl ether borate, connection boric acid pinacol ester, boric acid three isobutyl esters, isopropyl alcohol pinacol borate, 4-nitrobenzene boric acid pinacol ester, polyoxyethylene glycerol borate fatty acid ester, polyoxyethylene glyceryl borate oleic acid ester, diglycerol borate oleic acid (stearic acid, laurate) ester, the preferred boric acid tributyl, boric acid three n-propyls, triethyl borate.
A kind of method for preparing above-mentioned iron-based compound soft magnetic material comprises the steps:
To atomize iron-based powder and nano ferric phosphate and lubricated binding agent fully is dissolved or dispersed in the organic solvent, makes atomizing ferrous alloy powder particle surface evenly coat this nano ferric phosphate of one deck and lubricated binding agent; To coat good atomizing ferrous alloy powder particle again and suppress under the pressure of 550-750MPa, the parts that suppress again at 500-600 ℃ of following vacuum annealing 30-180 minute, obtained required iron-based composite soft-magnetic parts at 120-200 ℃ of following vacuum annealing 10-60 minute.
Described encapsulation steps is that mechanical agitation is mixed coating, sonic oscillation coats, and places until organic solvent evaporation then.
Starting powder described atomizing iron-based powder can be atomizing before carrying out the coating of ferric phosphate and lubricated binding agent after also can be through the atomized powder after hydrogenation treatment or the phosphorylation processing.
Described pressing step is 50-60 ℃ of compacting down, or normal temperature compacting down.
Described organic solvent is a kind of in ethanol, isopropyl alcohol, acetone, the butanone, preferred alcohol.
Atomizing iron-based powder particle size range satisfies: at least 30%, preferred at least 50% iron-based powder is made up of the particle that particle diameter surpasses 200 μ m, and particle diameter accounts for 5% at most greater than the particle of 400 μ m, and the powder particle of particle diameter below 10 μ m is less than 10%.Selecting the ferrous alloy powder of suitable particle size, is the prerequisite that can obtain high density material.
Lubricated binding agent in the inventive method is selected from: butyl borate, boric acid three n-propyls, triethyl borate, trimethylborate, the polyethylene glycol borate, the triethanolamine borate, triisopropanolamine ring borate, triisopropyl borate ester, the oleic acid diethyl amide borate, the poly glycol monomethyl ether borate, connection boric acid pinacol ester, boric acid three isobutyl esters, isopropyl alcohol pinacol borate, 4-nitrobenzene boric acid pinacol ester, polyoxyethylene glycerol borate, polyoxyethylene glyceryl borate oleic acid ester, diglycerol borate oleic acid (stearic acid, laurate) ester, the preferred boric acid tributyl, boric acid three n-propyls, triethyl borate.Above-mentioned lubricated binding agent is dispersed in atomizing ferrous alloy powder particle surface, increases the flowability of ferrous alloy powder particle.The selected lubricated binding agent energy while of the present invention is as the release agent of profiled part.
The cladding process on atomizing ferrous alloy powder surface comprises in the inventive method: mechanical agitation is mixed coating, and sonic oscillation coats, and can also be that fluidized-bed process coats in principle.The advantage of mechanical agitation hybrid packet coating process is can be quick, large batch of coating; The sonic oscillation cladding process can guarantee that the iron powder powder surface coats the combined lubrication agent uniformly; Fluidized-bed process coats can be wrapped in the iron powder powder surface with the combined lubrication agent in enormous quantities, evenly and apace.
Organic solvent in the inventive method is selected ethanol, isopropyl alcohol, acetone or butanone, preferred alcohol for use.The effect of organic solvent is the even coating that can better help the combined lubrication agent.
In a word, the invention provides a kind of novel iron-based compound soft magnetic material and preparation method thereof.Its abundant, low price in raw material source, the cost of material is low, press knot pressure low, and density is higher.Advantages such as the preparation method has that technology is simple, the cost of material is low, and density height, magnetic flux density are big.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is further set forth:
Embodiment 1:
To atomize straight iron powder and iron nickel powder mixed powder as raw material, and the quality of the iron nickel powder that wherein atomizes accounts for 5% of atomizing ferrous alloy powder gross mass, and the atomizing ferrous alloy powder has the particle mean size between the 80-200 μ m, and the powder particle of granularity below 10 μ m is less than 10%.The iron phosphate grains (particle diameter 10-20nm) that accounts for the butyl borate of atomizing ferrous alloy powder quality 0.2% and will account for atomizing ferrous alloy powder quality 0.3% is joined in the iron-based powder, add in the organic solvent-acetone and fully mix, ultrasonator vibration 10 minutes, treat organic solvent evaporation again.With the pressure single shaft of 600MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 30 minutes, and 600 ℃ of following heat treatment elements 60 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.47g/cm
3, magnetic strength B
8000Be 1.20T, maximum permeability μ
mBe 0.3mH/m.
Embodiment 2:
To atomize straight iron powder and iron nickel powder mixed powder as raw material, and wherein iron nickel powder quality accounts for 9% of atomizing ferrous alloy powder gross mass, and the atomizing ferrous alloy powder has the particle mean size between the 100-300 μ m, and the powder particle of granularity below 10 μ m is less than 5%.Boric acid three isobutyl esters that account for atomizing ferrous alloy powder quality 0.5% are joined in the iron-based powder with the 10-20nm ferric phosphate that accounts for atomizing ferrous alloy powder quality 0.1%, add in the organic solvent ethanol and fully mix, ultrasonator vibration 15 minutes, treat organic solvent evaporation again.With the pressure single shaft of 700MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 150 ℃ of following vacuum annealings 30 minutes, and 500 ℃ of following heat treatment elements 40 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.58g/cm
3, magnetic strength B
8000Be 1.092T, maximum permeability μ
mBe 0.2mH/m.
Embodiment 3:
The straight iron powder powder that will atomize is as raw material, and this iron powder has the particle mean size between the 100-200 μ m, and the powder particle of granularity below 10 μ m is less than 9%.The poly glycol monomethyl ether borate that accounts for atomizing ferrous alloy powder quality 0.3% is joined in the iron powder powder with the 10-20nm ferric phosphate that accounts for atomizing ferrous alloy powder quality 0.05%, adding the organic solvent absolute ethyl alcohol fully mixes, ultrasonator vibration 15 minutes, treat organic solvent evaporation again.With the pressure single shaft of 650MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 180 ℃ of following vacuum annealings 40 minutes, and 600 ℃ of following heat treatment elements 60 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.52g/cm
3, magnetic strength B
8000Be 1.22T, maximum permeability μ
mBe 0.1mH/m.
Embodiment 4:
The straight iron powder powder that will atomize is as raw material, and this iron powder has the particle mean size between the 100-300 μ m, and the powder particle of granularity below 10 μ m is less than 10%.The 10-20nm ferric phosphate that accounts for atomizing ferrous alloy powder quality 1.0% is joined in the iron powder powder with the butyl borate that accounts for atomizing ferrous alloy powder quality 1.3%, add in the organic solvent isopropyl alcohol and fully mix, ultrasonator vibration 20 minutes, treat organic solvent evaporation again.With the pressure single shaft of 600MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 30 minutes, and 550 ℃ of following heat treatment elements 100 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.02g/cm
3, magnetic strength B
8000Be 0.879T, maximum permeability μ
mBe 0.1mH/m.
Embodiment 5:
To atomize straight iron powder and iron nickel powder mixed powder as raw material, and wherein iron nickel powder quality accounts for 4% of atomizing ferrous alloy powder gross mass, and ferrous alloy powder has the particle mean size between the 300-500 μ m, and the powder particle of granularity below 10 μ m is less than 10%.The adding of lubricant is implemented as follows: boric acid three n-propyls that will account for atomizing ferrous alloy powder quality 0.1% join in the iron-based powder with the 20-100nm ferric phosphate that accounts for atomizing ferrous alloy powder quality 0.2%, add in the organic solvent butanone and fully mix, ultrasonator vibration 15 minutes, treat organic solvent evaporation again.With the pressure single shaft of 600MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 120 ℃ of following vacuum annealings 30 minutes, and 500 ℃ of following heat treatment elements 40 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.07g/cm
3, magnetic strength B
8000Be 1.02T, maximum permeability μ
mBe 0.1mH/m.
Embodiment 6:
To atomize straight iron powder and iron nickel powder mixed powder as raw material, and wherein iron nickel powder quality accounts for atomizing ferrous alloy powder gross mass 2%, and ferrous alloy powder has the particle mean size between the 100-300 μ m, and the powder particle of granularity below 10 μ m is less than 5%.The isopropyl alcohol pinacol borate that accounts for atomizing ferrous alloy powder quality 0.6% is joined in the iron-based powder with the nano ferric phosphate that accounts for atomizing ferrous alloy powder quality 0.2%, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 15 minutes, treat organic solvent evaporation again.Under 60 ℃, with the pressure single shaft of 550MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 15 minutes, and 500 ℃ of following heat treatment elements 40 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.23g/cm
3
Embodiment 7:
The straight iron powder powder that will atomize is as raw material, and this iron powder has the particle mean size between the 100-300 μ m, and the powder particle of granularity below 10 μ m is less than 5%.The butyl borate that accounts for atomizing ferrous alloy powder quality 0.1% is joined in the iron powder powder with the 10-50nm ferric phosphate that accounts for atomizing ferrous alloy powder quality 0.4%, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 15 minutes, treat organic solvent evaporation again.Under 50 ℃ of conditions, with the pressure single shaft of 650Mpa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 60 minutes, and 500 ℃ of following heat treatment elements 90 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.32g/cm
3
Embodiment 8:
The straight iron powder powder that will atomize is as raw material, and this iron powder has the particle mean size between the 100-500 μ m, and the powder particle of granularity below 10 μ m is less than 10%.The butyl borate that accounts for atomizing ferrous alloy powder quality 0.6% is joined in the iron powder powder with the 10-40nm ferric phosphate that accounts for atomizing ferrous alloy powder quality 0.5%, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 10 minutes, treat organic solvent evaporation again.Under 60 ℃ of conditions, with the pressure single shaft of 650MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 40 minutes, and 500 ℃ of following heat treatment elements 90 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.39g/cm
3
Embodiment 9:
The straight iron powder powder that will atomize is as raw material, and this iron powder has the particle mean size between the 200-300 μ m, and the powder particle of granularity below 10 μ m is less than 5%.The butyl borate that accounts for atomizing ferrous alloy powder quality 0.2% is joined in the iron powder powder with the nano ferric phosphate that accounts for atomizing ferrous alloy powder quality 1.0%, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 20 minutes, treat organic solvent evaporation again.Under 60 ℃, with the pressure single shaft of 600MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 150 ℃ of following vacuum annealings 45 minutes, and 600 ℃ of following heat treatment elements 150 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.22g/cm
3
Embodiment 10:
The straight iron powder powder that will atomize is as raw material, and this iron powder has the particle mean size between the 100-500 μ m, and the powder particle of granularity below 10 μ m is less than 10%.The butyl borate that accounts for atomizing ferrous alloy powder quality 1% is joined in the iron powder powder with the nano ferric phosphate that accounts for atomizing ferrous alloy powder quality 1%, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 25 minutes, treat organic solvent evaporation again.With the pressure single shaft of 750MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 30 minutes, and 500 ℃ of following heat treatment elements 120 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.2g/cm
3
Embodiment 11:
The straight iron powder powder that will atomize is as raw material, and this iron powder has the particle mean size between the 200-400 μ m, and the powder particle of granularity below 10 μ m is less than 5%.The nano ferric phosphate that accounts for atomizing ferrous alloy powder quality 1% is joined in the iron powder powder with the butyl borate that accounts for atomizing ferrous alloy powder quality 1.5%, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 25 minutes, treat organic solvent evaporation again.Under 60 ℃ of conditions, with the pressure single shaft of 600MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 150 ℃ of following vacuum annealings 30 minutes, and 500 ℃ of following heat treatment elements 180 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.41g/cm
3
Embodiment 12:
The straight iron powder powder that will atomize is as raw material, and this iron powder has the particle mean size between the 100-300 μ m, and the powder particle of granularity below 10 μ m is less than 10%.The nano ferric phosphate that accounts for atomizing ferrous alloy powder quality 1.5% is joined in the iron powder powder with the polyoxyethylene glycerol borate that accounts for atomizing ferrous alloy powder quality 0.01%, adding organic solvent fully mixes, ultrasonator vibration 20 minutes, treat organic solvent evaporation again.With the pressure single shaft of 500MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 30 minutes, and 550 ℃ of following heat treatment elements 30 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density only is 6g/cm
3
Embodiment 13:
The straight iron powder powder that will atomize is as raw material, and this iron powder has the particle mean size between the 100-300 μ m, and the powder particle of granularity below 10 μ m is less than 10%.The 10-20nm ferric phosphate that accounts for atomizing ferrous alloy powder quality 0.01% is joined in the iron powder powder with the polyoxyethylene glycerol borate that accounts for atomizing ferrous alloy powder quality 0.01%, adding organic solvent fully mixes, ultrasonator vibration 20 minutes, treat organic solvent evaporation again.With the pressure single shaft of 500MPa to being squeezed into the ring-type sample.The parts that suppress are 200 ℃ of following vacuum annealings 30 minutes, and 550 ℃ of following heat treatment elements 30 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density only is 6.6g/cm
3
Embodiment 14:
The straight iron powder powder that will atomize carries out hydrogenation treatment earlier, and this iron powder has the particle mean size between the 100-300 μ m, and the powder particle of granularity below 10 μ m is less than 10%.The nano ferric phosphate that accounts for atomizing ferrous alloy powder quality 0.01% is joined in the iron powder powder with the polyoxyethylene glycerol borate that accounts for atomizing ferrous alloy powder quality 0.01%, add organic solvent and fully mix, mechanical agitation is 20 minutes again, treats organic solvent evaporation.Under 60 ℃ of conditions, with the pressure single shaft of 500MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 60 minutes, and 550 ℃ of following heat treatment elements 30 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density only is 7.2g/cm
3
Embodiment 15:
The straight iron powder powder that makes water fogging carries out phosphorylation to be handled, and this iron powder has the particle mean size between the 100-300 μ m, and the powder particle of granularity below 10 μ m is less than 10%.The 10-20nm ferric phosphate that accounts for atomizing ferrous alloy powder quality 1.5% is joined in the iron powder powder with the polyoxyethylene glycerol borate that accounts for atomizing ferrous alloy powder quality 0.4%, add organic solvent and fully mix, mechanical agitation is 20 minutes again, treats organic solvent evaporation.Under 50 ℃ of conditions, with the pressure single shaft of 600MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 10 minutes, and 550 ℃ of following heat treatment elements 100 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density only is 6.92g/cm
3
It should be noted last that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed among the claim scope of the present invention.
Claims (10)
1. iron-based compound soft magnetic material is characterized in that: it is made up of atomizing iron-based powder, nano ferric phosphate and lubricated binding agent, and this atomizing iron-based powder particle surface evenly coats this nano ferric phosphate particle of one deck and lubricated binding agent; Wherein said lubricated binding agent is that borate is lubricated, and quality is the 0.01-1.5% of atomizing iron-based powder quality; The nano ferric phosphate quality is the 0.01-1.5% of atomizing iron-based powder quality.
2. material as claimed in claim 1, it is characterized in that: described atomizing iron-based powder is atomizing straight iron powder, atomizing iron nickel powder or its mixed powder, and the quality of atomizing iron nickel powder accounts for ratio≤9% of atomizing ferrous alloy powder quality in wherein atomize straight iron powder and the atomizing iron nickel powder mixed powder.
3. material as claimed in claim 1 or 2, it is characterized in that: the particle size range of described atomizing iron-based powder satisfies: at least 30%, preferred at least 50% atomizing iron-based powder is made up of the particle that particle diameter surpasses 200 μ m, particle diameter is greater than particle≤5% of 400 μ m, powder particle≤10% of particle diameter below 10 μ m.
4. material as claimed in claim 1 is characterized in that: described nano ferric phosphate grain diameter≤100nm, preferred 10-50nm.
5. material as claimed in claim 1, it is characterized in that: described lubricated binding agent is a kind of in the following compounds: butyl borate, boric acid three n-propyls, triethyl borate, trimethylborate, the polyethylene glycol borate, the triethanolamine borate, triisopropanolamine ring borate, triisopropyl borate ester, the oleic acid diethyl amide borate, the poly glycol monomethyl ether borate, connection boric acid pinacol ester, boric acid three isobutyl esters, isopropyl alcohol pinacol borate, 4-nitrobenzene boric acid pinacol ester, polyoxyethylene glycerol borate fatty acid ester, polyoxyethylene glyceryl borate oleic acid ester, diglycerol borate oleic acid (stearic acid, laurate) ester, the preferred boric acid tributyl, boric acid three n-propyls, triethyl borate.
6. a method for preparing iron-based compound soft magnetic material as claimed in claim 1 is characterized in that: comprise the steps:
To atomize iron-based powder and nano ferric phosphate and lubricated binding agent fully is dissolved or dispersed in the organic solvent, makes atomizing ferrous alloy powder particle surface evenly coat this nano ferric phosphate of one deck and lubricated binding agent; To coat good atomizing ferrous alloy powder particle again and suppress under the pressure of 550-750MPa, the parts that suppress again at 500-600 ℃ of following vacuum annealing 30-180 minute, obtained required iron-based composite soft-magnetic parts at 120-200 ℃ of following vacuum annealing 10-60 minute.
7. method as claimed in claim 6 is characterized in that: described encapsulation steps is that mechanical agitation is mixed coating, sonic oscillation coats, and places until organic solvent evaporation then.
8. method as claimed in claim 6 is characterized in that: the starting powder described atomizing iron-based powder can be atomizing before carrying out the coating of ferric phosphate and lubricated binding agent after also can be through the atomized powder after hydrogenation treatment or the phosphorylation processing.
9. method as claimed in claim 6 is characterized in that: described pressing step is 50-60 ℃ of compacting down, or normal temperature compacting down.
10. method as claimed in claim 6 is characterized in that: described organic solvent is a kind of in ethanol, isopropyl alcohol, acetone, the butanone, preferred alcohol.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100814222A CN102136329A (en) | 2011-04-01 | 2011-04-01 | Iron-based composite soft magnetic material and preparation method thereof |
| CN2011101522166A CN102360662A (en) | 2011-04-01 | 2011-06-08 | Iron-based composite soft magnetic material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100814222A CN102136329A (en) | 2011-04-01 | 2011-04-01 | Iron-based composite soft magnetic material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102136329A true CN102136329A (en) | 2011-07-27 |
Family
ID=44296079
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011100814222A Pending CN102136329A (en) | 2011-04-01 | 2011-04-01 | Iron-based composite soft magnetic material and preparation method thereof |
| CN2011101522166A Pending CN102360662A (en) | 2011-04-01 | 2011-06-08 | Iron-based composite soft magnetic material and preparation method thereof |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101522166A Pending CN102360662A (en) | 2011-04-01 | 2011-06-08 | Iron-based composite soft magnetic material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN102136329A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102189260A (en) * | 2011-05-05 | 2011-09-21 | 王晨兰 | Method for preparing diamond blade by using special metal bond |
| CN104028762A (en) * | 2014-05-28 | 2014-09-10 | 浙江大学 | Preparation method of soft magnetic composite material |
| CN104321839A (en) * | 2012-04-26 | 2015-01-28 | 香港科技大学 | Soft Magnetic Composite |
| CN105070479A (en) * | 2015-08-10 | 2015-11-18 | 天长市昭田磁电科技有限公司 | Magnetic core material for transformer high in magnetic permeability |
| CN105798287A (en) * | 2016-04-29 | 2016-07-27 | 河海大学 | Scattering method for surface covalent modification modification of nickel nanowires |
| CN112166479A (en) * | 2018-05-30 | 2021-01-01 | 霍加纳斯股份有限公司 | Ferromagnetic Powder Composition |
| CN118571637A (en) * | 2024-06-24 | 2024-08-30 | 安徽大地熊新材料股份有限公司 | High-magnetic energy product neodymium-iron-boron magnet and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106373695B (en) * | 2016-08-31 | 2019-05-14 | 香磁磁业(深圳)有限公司 | A kind of magnet composite material and preparation method |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045680C (en) * | 1993-12-28 | 1999-10-13 | 住友金属工业株式会社 | Molding material for producing rare earth iron-based permanent magnet and production method |
| CN100380537C (en) * | 2005-05-27 | 2008-04-09 | 罗计添 | Soft-magnetic composite material and process for making magnetic conduction component by using same |
| JP4710485B2 (en) * | 2005-08-25 | 2011-06-29 | 住友電気工業株式会社 | Method for producing soft magnetic material and method for producing dust core |
-
2011
- 2011-04-01 CN CN2011100814222A patent/CN102136329A/en active Pending
- 2011-06-08 CN CN2011101522166A patent/CN102360662A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102189260A (en) * | 2011-05-05 | 2011-09-21 | 王晨兰 | Method for preparing diamond blade by using special metal bond |
| CN104321839A (en) * | 2012-04-26 | 2015-01-28 | 香港科技大学 | Soft Magnetic Composite |
| CN104028762A (en) * | 2014-05-28 | 2014-09-10 | 浙江大学 | Preparation method of soft magnetic composite material |
| CN104028762B (en) * | 2014-05-28 | 2016-08-24 | 浙江大学 | A kind of preparation method of soft-magnetic composite material |
| CN105070479A (en) * | 2015-08-10 | 2015-11-18 | 天长市昭田磁电科技有限公司 | Magnetic core material for transformer high in magnetic permeability |
| CN105798287A (en) * | 2016-04-29 | 2016-07-27 | 河海大学 | Scattering method for surface covalent modification modification of nickel nanowires |
| CN105798287B (en) * | 2016-04-29 | 2017-12-22 | 河海大学 | The process for dispersing that a kind of nickel nanowire surface covalent modification is modified |
| CN112166479A (en) * | 2018-05-30 | 2021-01-01 | 霍加纳斯股份有限公司 | Ferromagnetic Powder Composition |
| CN118571637A (en) * | 2024-06-24 | 2024-08-30 | 安徽大地熊新材料股份有限公司 | High-magnetic energy product neodymium-iron-boron magnet and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102360662A (en) | 2012-02-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102136329A (en) | Iron-based composite soft magnetic material and preparation method thereof | |
| CN104505209B (en) | A kind of soft magnetic metal composite core and preparation method thereof | |
| CN102360671B (en) | Preparation method for mu75 magnetic powder core of ferrosilicon aluminum | |
| KR101352214B1 (en) | Production process of dust core and dust core obtained thereby | |
| CN105185560A (en) | Preparation method of Fe-based metal soft magnetic powder core | |
| CN103189936A (en) | Soft magnetic powder, powder granules, dust core, electromagnetic component, and method for manufacturing dust core | |
| CN104070161A (en) | Preparation method for inorganic-organic composite adhesive-coated soft magnetic composite | |
| CN101579738A (en) | Double pressing molding method for preparing high-density powder metallurgical iron-base part | |
| CN101755313A (en) | Iron-based soft magnetic powder for dust core and dust core | |
| CN104361968A (en) | Preparation method of low-loss high permeability Fe-Si-Al magnetic powder core | |
| CN102974821A (en) | Method for preparing iron silicon soft magnetic alloy powder core | |
| CN113555178B (en) | Double-main-phase soft magnetic composite material and preparation method thereof | |
| CN113380483A (en) | Composite soft magnetic material and preparation method thereof | |
| CN103377786B (en) | A kind of preparation method of iron-silicon-aluminualloy alloy magnetic powder core | |
| CN103506618B (en) | Powder used in metallurgy is containing Mn mixing comminuted steel shot and preparation method | |
| JP2011171346A (en) | Iron-based soft magnetic powder for dust core, method of manufacturing the same, and dust core | |
| CN114334347A (en) | A kind of high frequency and low loss amorphous soft magnetic composite film material and preparation method thereof | |
| CN104036903B (en) | A kind of preparation method of ferrum tantnickel powder core | |
| CN107256752B (en) | A kind of preparation method of sintered iron powder-based soft magnetic composite material | |
| CN105855555B (en) | A kind of preparation method of iron cobalt magnetically soft alloy device | |
| CN112475288B (en) | Preparation method of soft magnetic composite material for stator | |
| CN102129908A (en) | A novel composite soft magnetic material and its preparation method | |
| JP2015012188A (en) | Dust core manufacturing method and dust core | |
| CN102136330A (en) | Composite soft magnetic material and preparation method thereof | |
| CN119694701A (en) | A kind of iron-based soft magnetic composite material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication |