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CN103240411B - Production methods of inorganic-organic insulation layer soft magnetic composites - Google Patents

Production methods of inorganic-organic insulation layer soft magnetic composites Download PDF

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CN103240411B
CN103240411B CN201310187791.9A CN201310187791A CN103240411B CN 103240411 B CN103240411 B CN 103240411B CN 201310187791 A CN201310187791 A CN 201310187791A CN 103240411 B CN103240411 B CN 103240411B
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performed polymer
magnetic
polymer
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inorganic
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CN103240411A (en
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武高辉
丁伟
姜龙涛
修子扬
陈国钦
武锐
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The invention relates to production methods of soft magnetic materials, discloses production methods of inorganic-organic insulation layer soft magnetic composites, and solves the problem that good soft magnetic composites cannot be produced in the prior art. The first production method includes 1 preparing solid-liquid mixtures; 2 preparing solid-liquid mixtures with a silica layer wrapped on the magnetic powder surface; 3 preparing solid-liquid mixtures with silicate glass wrapped on the magnetic powder surface; 4 performing cleaning and drying; 5 performing mixing; 6 performing primary pressing; 7 wrapping organic polymers; and 8 performing heat treatment to obtain the inorganic-organic insulation layer soft magnetic composites. The second production method includes 1 preparing solid-liquid mixtures; 2 preparing solid-liquid mixtures with a silica layer wrapped on the magnetic powder surface; 3 performing cleaning and drying; 4 performing mixing; 5 performing primary pressing; 6 wrapping organic polymers; and 7 performing heat treatment to obtain the inorganic-organic insulation layer soft magnetic composites. The production methods are mainly applied to production of the inorganic-organic insulation layer soft magnetic composites.

Description

The preparation method of inorganic-organic insulating barrier soft-magnetic composite material
Technical field
The present invention relates to a kind of preparation method of soft magnetic materials.
Background technology
Soft-magnetic composite material refers to a class soft magnetic materials independently mutual between magnetic and that couple together by insulating layer material.The outstanding advantages of this soft-magnetic composite material is under AC magnetic field, to have low iron loss and Three-Dimensional Isotropic character.Therefore can prepare a lot of conventional soft magnetic materials and be difficult to the parts of realizing, be applied in switching magnetic-resistance, resonant inductance, anti-lock brake sensor, electromagnetic actuator device, brshless DC motor, rotating machinery, the fields such as low-frequency filter.The preparation technology of soft-magnetic composite material is normally to metal or alloy Magnaglo surface coated inorganic thing and organic electric insulation layer, or adopt Magnaglo matrix-high resistivity continuous fiber complex method to form composite soft-magnetic powder, then adopt powder metallurgy compaction process to be prepared into closely knit block soft magnetic materials.
The method that adopts powder metallurgy compaction process to be prepared into closely knit block soft magnetic materials is reported in lot of documents, for these soft-magnetic composite materials, in its preparation process, need to apply the pressure that is greater than 800MPa, to reach the compacted density needing, but meet again good saturation induction density and magnetic conductivity simultaneously, just need to anneal and remove the residual stress of material the soft-magnetic composite material that contains Coated with Organic Matter layer, because pure organic matter is higher as the soft-magnetic composite material eddy-current loss of electric insulation layer, therefore be to be all coated again organic insulator outward at phosphate coating conventionally.But phosphate coating non-refractory conventionally, so be difficult to effectively remove its residual stress.For the soft-magnetic composite material of existing inorganic matter clad, the insulating properties of clad does not reach requirement, and existing clad environmental pollution containing P or S is serious, so there is using SiO 2, MgO, SiO 2powder, Al 2o 3powder, ZrO 2inorganic insulation layer prepared by the mixture of powder and mica powder is as inorganic matter clad, and inorganic insulation layer generally has high-temperature stable, and it has overcome the shortcoming of the common non-refractory of Coated with Organic Matter layer.But existing inorganic insulation layer also has shortcoming, the own thermal coefficient of expansion that the thermal coefficient of expansion of inorganic insulation layer and magnetic differs large and inorganic insulation layer can not change, can in magnetic, produce thermal stress at the larger environment of the temperature difference or in long-time use procedure, cause the soft-magnetic composite material of inorganic matter clad cannot there is good magnetic property.These problems are all restricting development and the application of soft-magnetic composite material.Therefore existing soft-magnetic composite material exists the poor and prior art of magnetic property cannot prepare the problem of the soft-magnetic composite material having excellent magnetic characteristics.
Summary of the invention
The present invention will solve the problem that prior art cannot be prepared the soft-magnetic composite material having excellent magnetic characteristics, and the preparation method of inorganic-organic insulating barrier soft-magnetic composite material is provided.
A preparation method for inorganic-organic insulating barrier soft-magnetic composite material, specifically completes according to the following steps:
One, prepare solidliquid mixture: magnetic is put into cleaning agent, then be ultrasonic cleaning 10min～20min under 24KHz～35KHz in supersonic frequency, filtration obtains cleaning rear magnetic, after cleaning, add ethanol and oleic acid in magnetic, and the ammoniacal liquor that is 20%～30% by mass concentration is adjusted to 8.5～9.5 by pH value, then carry out ultrasonic dispersion or dispersed with stirring, obtain solidliquid mixture; The mass ratio of the oleic acid described in step 1 and magnetic is (0.03～0.2): 1; The volume ratio of the oleic acid described in step 1 and ethanol is 1:(40～75); Cleaning agent described in step 1 is distilled water;
Two, prepare the solidliquid mixture of magnetic surface coated silica layer: in the solidliquid mixture obtaining to step 1, add ethanol, then adopting mass concentration is that 20%～30% ammoniacal liquor is adjusted to 8.5～9.5 by pH value, then low whipping speed is stirring reaction under 600r/min～1200r/min and the pH value condition that is 8.5～9.5, ethyl orthosilicate is divided into 2～4 parts, in stirring reaction process, add 1 part of ethyl orthosilicate at interval of 0.5h～1.5h, add for the last time after ethyl orthosilicate, stirring reaction 0.5h～3h under condition that to continue low whipping speed and be 600r/min～1200r/min and pH value be 8.5～9.5, obtain the solidliquid mixture of magnetic surface coated silica layer, the volume ratio of the ethanol adding described in step 2 and solidliquid mixture is (2～4): 1, in the gross mass of the ethyl orthosilicate adding described in step 2 and solidliquid mixture, the mass ratio of magnetic is (0.25～0.4): 1,
Three, prepare the solidliquid mixture of magnetic surface coated Si silicate glass: in the solidliquid mixture of the magnetic surface coated silica layer obtaining to step 2, adding oleic acid, ethyl orthosilicate and mass concentration is metal alkoxide/organic solution of 10%～20%, then adopting mass concentration is that 20%～30% ammoniacal liquor is adjusted to 8.5～9.5 by pH value, and low whipping speed is stirring reaction 1h～6h under 600r/min～1200r/min and the pH value condition that is 8.5～9.5, obtain the solidliquid mixture of magnetic surface coated Si silicate glass; In the solidliquid mixture of the oleic acid adding described in step 3 and magnetic surface coated silica layer, the mass ratio of magnetic is (0.05～0.1): 1; The volume ratio of the solidliquid mixture of the ethyl orthosilicate adding described in step 3 and magnetic surface coated silica layer is (0.25～0.6): 1; In metal alkoxide/organic solution that the mass concentration adding described in step 3 is 10%～20%, in the solidliquid mixture of metal alkoxide and magnetic surface coated silica layer, the mass ratio of magnetic is (0.05～0.6): 1; In metal alkoxide/organic solution described in step 3, the chemical formula of lower metal alkoxide is M (OR) x; Wherein said M (OR) xin M be a kind of in Ti, B, Be, Mn, In, Ge, Al, Zr, Na, K, Li, Mg, Ca, Mg and Ba or wherein several combination; Wherein said M (OR) xin R be C nh 2n+1, and described C nh 2n+1middle n is 1～4; Wherein said M (OR) xin x be 1～5, and described M (OR) xbe electroneutral;
Four, cleaning-drying: the solidliquid mixture of the magnetic surface coated Si silicate glass obtaining in step 3 is left standstill to 10min～30min, then separate, clean separating the solid obtaining, solid after cleaning is put into drying box, be dry 20min～360min at 40 DEG C～80 DEG C in temperature, dried solid is screened with electromagnet, obtain the coated magnetic of silicate glass;
Five, mix: it is in the coupling agent solution of 10mPas～10000mPas that magnetic coated silicate glass is added to viscosity, then take vibratory milling polishing, planetary type ball-milling polishing or mechanical agitation to mix, finally be dried, till being dried to constant weight, obtain mixture; In the coated magnetic of silicate glass described in step 5, in magnetic and coupling agent solution, the mass ratio of solute is 100:(0.2～3.0); In coupling agent solution described in step 5, solute is coupling agent, and solvent is one or more the mixture in water, methyl alcohol, ethanol, isopropyl alcohol, butanols, ethanol, toluene, benzene, dimethylbenzene, stearic acid and atoleine; Wherein said coupling agent is silane coupler, titanate coupling agent or aluminate coupling agent;
Six, compacting for the first time: the mixture that step 5 is obtained is transferred in mould, is then compressing under 0.2MPa～10MPa in mechanical pressure, obtains preform in mould;
Seven, be coated with organic polymer: in the mixture first obtaining by organic polymer performed polymer and step 5, the mass ratio of magnetic is (0.2～7): 100 take organic polymer performed polymer, then organic polymer performed polymer is added in organic solvent, after mixing, obtaining viscosity is organic polymer performed polymer/ORGANIC SOLVENT MIXTURES of 10mpas～10000mpas, organic polymer performed polymer/the ORGANIC SOLVENT MIXTURES that is 10mpas～10000mpas by viscosity again adds in the mould with preform that step 6 obtains, then be to suppress 1min～10min under 0.2MPa～10MPa in mechanical pressure, obtain the preform of coated Si silicate glass/organic polymer performed polymer,
Eight, heat treatment: the preform that step 7 is obtained to coated Si silicate glass/organic polymer performed polymer carries out protective atmosphere heat treatment or vacuum heat, obtains inorganic-organic insulating barrier soft-magnetic composite material;
Protective atmosphere heat treatment concrete operations described in step 8 are as follows: the preform that first step 7 is obtained to coated Si silicate glass/organic polymer performed polymer is placed in nitrogen, under argon gas or hydrogen atmosphere, then be warming up to 200 DEG C～900 DEG C with 8 DEG C of heating rates/min～12 DEG C/min, and at nitrogen, under argon gas or hydrogen shield and temperature be that the preform that under 200 DEG C～900 DEG C conditions, step 7 is obtained to coated Si silicate glass/organic polymer performed polymer is heat-treated 10min～300min, then be cooled to room temperature with 8 DEG C of rate of temperature fall/min～12 DEG C/min, obtain inorganic-organic insulating barrier soft-magnetic composite material,
Vacuum heat concrete operations described in step 8 are as follows: the preform that first step 7 is obtained to coated Si silicate glass/organic polymer performed polymer is placed under vacuum condition, then so that 8 DEG C of heating rates/min～12 DEG C/min is warming up to 200 DEG C～900 DEG C, is 10 in vacuum -1pa～10 -3pa and temperature are that the preform that under 200 DEG C～900 DEG C conditions, step 7 is obtained to coated Si silicate glass/organic polymer performed polymer is heat-treated 10min～300min, then be cooled to room temperature, obtain inorganic-organic insulating barrier soft-magnetic composite material with 8 DEG C of rate of temperature fall/min～12 DEG C/min.
Magnetic described in step 1 is pure Fe powder, Fe-Ni-Co based metal powder, Fe-Ni based metal powder, Fe-Si-Al based metal powder, Fe-Co based metal powder, Fe-Si based metal powder, Fe-P based metal powder, Fe 3o 4powder or Fe-Cr based metal powder, and the particle diameter of described magnetic is 10 μ m～500 μ m.
Ultrasonic dispersion concrete operations described in step 1 are as follows: be ultrasonic dispersion 1h～2h under 24KHz～35KHz in supersonic frequency.
Dispersed with stirring concrete operations described in step 1 are as follows: low whipping speed is dispersed with stirring 1h～2h under 200r/min～1200r/min.
Organic polymer performed polymer described in step 7 is polyethylene performed polymer, polypropylene performed polymer, ethylene-ethyl acetate copolymer performed polymer, nylon 6 performed polymers, nylon 66 performed polymers, nylon 6/66 performed polymer, poly phenylene sulfoether performed polymer, poly-sub-benzene thioketones performed polymer, PET performed polymer, polybutylene terephthalate performed polymer, polyimide prepolymer, PEI performed polymer, polyamidoimide performed polymer, polystyrene performed polymer, acrylonitritrile-styrene resin performed polymer, polyvinyl chloride performed polymer, Vingon performed polymer, vinyl chloride-vinylidene chloride copolymer performed polymer, haloflex performed polymer, PMA performed polymer, polymethyl methacrylate performed polymer, polyacrylonitrile performed polymer, polymethacrylonitrile performed polymer, tetrafluoroethylene/perfluoro alkyl vinyl ether copolymer performed polymer, tetrafluoroethylene/hexafluoropropylene performed polymer, Kynoar performed polymer, dimethyl silicone polymer performed polymer, polyphenylene oxide performed polymer, polyether-ether-ketone performed polymer, polyether-ketone performed polymer, polyarylate performed polymer, polysulfones performed polymer, polyether sulfone performed polymer, polyformaldehyde performed polymer, Merlon performed polymer, polyvinyl acetate performed polymer, polyvinyl formal performed polymer, polyvinyl butyral resin performed polymer, polybutene performed polymer, polyisobutene performed polymer, polymethylpentene performed polymer, butadiene resin performed polymer, polyethylene oxide performed polymer, hydroxy phenyl estrodur performed polymer, Parylene resin prepolymer, silicones performed polymer, epoxy resin prepolymer, phenolic resin performed polymer, EP rubbers performed polymer, polybutadiene rubber performed polymer, SBR styrene butadiene rubbers performed polymer, a kind of or two kinds and two or more mixture in chloroprene rubber performed polymer and SBS performed polymer.
A preparation method for inorganic-organic insulating barrier soft-magnetic composite material, specifically completes according to the following steps:
One, prepare solidliquid mixture: magnetic is put into cleaning agent, then be ultrasonic cleaning 10min～20min under 24KHz～35KHz in supersonic frequency, filtration obtains cleaning rear magnetic, after cleaning, add ethanol and oleic acid in magnetic, and the ammoniacal liquor that is 20%～30% by mass concentration is adjusted to 8.5～9.5 by pH value, then carry out ultrasonic dispersion or dispersed with stirring, obtain solidliquid mixture; The mass ratio of the oleic acid described in step 1 and magnetic is (0.03～0.2): 1; The volume ratio of the oleic acid described in step 1 and ethanol is 1:(40～75); Cleaning agent described in step 1 is distilled water;
Two, prepare the solidliquid mixture of magnetic surface coated silica layer: in the solidliquid mixture obtaining to step 1, add ethanol, then adopting mass concentration is that 20%～30% ammoniacal liquor is adjusted to 8.5～9.5 by pH value, then low whipping speed is stirring reaction under 600r/min～1200r/min and the pH value condition that is 8.5～9.5, ethyl orthosilicate is divided into 2～4 parts, in stirring reaction process, add 1 part of ethyl orthosilicate at interval of 0.5h～1.5h, add for the last time after ethyl orthosilicate, stirring reaction 0.5h～3h under condition that to continue low whipping speed and be 600r/min～1200r/min and pH value be 8.5～9.5, obtain the solidliquid mixture of magnetic surface coated silica layer, the volume ratio of the ethanol adding described in step 2 and solidliquid mixture is (2～4): 1, in the gross mass of the ethyl orthosilicate adding described in step 2 and solidliquid mixture, the mass ratio of magnetic is (0.25～0.4): 1,
Three, cleaning-drying: the solidliquid mixture of the magnetic surface coated silica layer obtaining in step 2 is left standstill to 10min～30min, then separate, clean separating the solid obtaining, solid after cleaning is put into drying box, be dry 20min～360min at 40 DEG C～80 DEG C in temperature, dried solid is screened with electromagnet, obtain the magnetic of coated with silica;
Four, mix: it is in the coupling agent solution of 10mpas～10000mpas that the magnetic of coated with silica is added to viscosity, then take vibratory milling polishing, planetary type ball-milling polishing or mechanical agitation to mix, finally be dried, till being dried to constant weight, obtain mixture; In the magnetic of the coated with silica described in step 4, in magnetic and coupling agent solution, the mass ratio of solute is 100:(0.2～3.0); In coupling agent solution described in step 4, solute is coupling agent, and solvent is one or more the mixture in water, methyl alcohol, ethanol, isopropyl alcohol, butanols, ethanol, toluene, benzene, dimethylbenzene, stearic acid and atoleine; Wherein said coupling agent is silane coupler, titanate coupling agent or aluminate coupling agent;
Five, compacting for the first time: the mixture that step 4 is obtained is transferred in mould, is then compressing under 0.2MPa～10MPa in mechanical pressure, obtains preform in mould;
Six, be coated with organic polymer: in the mixture first obtaining by organic polymer performed polymer and step 4, the mass ratio of magnetic is (0.2～7): 100 take organic polymer performed polymer, then organic polymer performed polymer is added in organic solvent, after mixing, obtaining viscosity is organic polymer performed polymer/ORGANIC SOLVENT MIXTURES of 10mpas～10000mpas, organic polymer performed polymer/the ORGANIC SOLVENT MIXTURES that is 10mpas～10000mpas by viscosity again adds in the mould with preform that step 5 obtains, then be to suppress 1min～10min under 0.2MPa～10MPa in mechanical pressure, obtain the preform of coated silica/organic polymer performed polymer,
Seven, heat treatment: the preform that step 6 is obtained to coated silica/organic polymer performed polymer carries out protective atmosphere heat treatment or vacuum heat, obtains inorganic-organic insulating barrier soft-magnetic composite material;
Protective atmosphere heat treatment concrete operations described in step 7 are as follows: the preform that first step 6 is obtained to coated silica/organic polymer performed polymer is placed in nitrogen, under argon gas or hydrogen atmosphere, then be warming up to 200 DEG C～900 DEG C with 8 DEG C of heating rates/min～12 DEG C/min, and at nitrogen, under argon gas or hydrogen shield and temperature be that the preform that under 200 DEG C～900 DEG C conditions, step 6 is obtained to coated silica/organic polymer performed polymer is heat-treated 10min～300min, then be cooled to room temperature with 8 DEG C of rate of temperature fall/min～12 DEG C/min, obtain inorganic-organic insulating barrier soft-magnetic composite material,
Vacuum heat concrete operations described in step 7 are as follows: the preform that first step 6 is obtained to coated silica/organic polymer performed polymer is placed under vacuum condition, then so that 8 DEG C of heating rates/min～12 DEG C/min is warming up to 200 DEG C～900 DEG C, is 10 in vacuum -1pa～10 -3pa and temperature are that the preform that under 200 DEG C～900 DEG C conditions, step 6 is obtained to coated silica/organic polymer performed polymer is heat-treated 10min～300min, then be cooled to room temperature, obtain inorganic-organic insulating barrier soft-magnetic composite material with 8 DEG C of rate of temperature fall/min～12 DEG C/min.
Magnetic described in step 1 is pure Fe powder, Fe-Ni-Co based metal powder, Fe-Ni based metal powder, Fe-Si-Al based metal powder, Fe-Co based metal powder, Fe-Si based metal powder, Fe-P based metal powder, Fe 3o 4powder or Fe-Cr based metal powder, and the particle diameter of described magnetic is 10 μ m～500 μ m.
Ultrasonic dispersion concrete operations described in step 1 are as follows: be ultrasonic dispersion 1h～2h under 24KHz～35KHz in supersonic frequency.
Dispersed with stirring concrete operations described in step 1 are as follows: low whipping speed is dispersed with stirring 1h～2h under 200r/min～1200r/min.
Organic polymer performed polymer described in step 6 is polyethylene performed polymer, polypropylene performed polymer, ethylene-ethyl acetate copolymer performed polymer, nylon 6 performed polymers, nylon 66 performed polymers, nylon 6/66 performed polymer, poly phenylene sulfoether performed polymer, poly-sub-benzene thioketones performed polymer, PET performed polymer, polybutylene terephthalate performed polymer, polyimide prepolymer, PEI performed polymer, polyamidoimide performed polymer, polystyrene performed polymer, acrylonitritrile-styrene resin performed polymer, polyvinyl chloride performed polymer, Vingon performed polymer, vinyl chloride-vinylidene chloride copolymer performed polymer, haloflex performed polymer, PMA performed polymer, polymethyl methacrylate performed polymer, polyacrylonitrile performed polymer, polymethacrylonitrile performed polymer, tetrafluoroethylene/perfluoro alkyl vinyl ether copolymer performed polymer, tetrafluoroethylene/hexafluoropropylene performed polymer, Kynoar performed polymer, dimethyl silicone polymer performed polymer, polyphenylene oxide performed polymer, polyether-ether-ketone performed polymer, polyether-ketone performed polymer, polyarylate performed polymer, polysulfones performed polymer, polyether sulfone performed polymer, polyformaldehyde performed polymer, Merlon performed polymer, polyvinyl acetate performed polymer, polyvinyl formal performed polymer, polyvinyl butyral resin performed polymer, polybutene performed polymer, polyisobutene performed polymer, polymethylpentene performed polymer, butadiene resin performed polymer, polyethylene oxide performed polymer, hydroxy phenyl estrodur performed polymer, Parylene resin prepolymer, silicones performed polymer, epoxy resin prepolymer, phenolic resin performed polymer, EP rubbers performed polymer, polybutadiene rubber performed polymer, SBR styrene butadiene rubbers performed polymer, a kind of or two kinds and two or more mixture in chloroprene rubber performed polymer and SBS performed polymer.
Advantage of the present invention: one, the present invention on magnetic surface coated Si silicate glass or silica as insulating barrier, re-use coupling agent and mixed with resin, obtain the blank of inorganic-organic insulating barrier soft-magnetic composite material by cure under pressure, obtaining inorganic-organic insulating barrier soft-magnetic composite material through annealing; Owing to adopting silicate glass or silica as clad, therefore the soft-magnetic composite material of preparing with this Magnaglo can be annealed under higher temperature, make soft-magnetic composite material have excellent magnetic property, this provides wide space in the application in larger field for soft-magnetic composite material; More than the fracture strength of the soft-magnetic composite material that two, prepared by the present invention reaches 45MPa, maximum permeability reaches more than 330; Three, the soft-magnetic composite material of preparing due to the present invention has good magnetic, so can be applicable to the fields such as switching magnetic-resistance, resonant inductance, anti-lock brake sensor, electromagnetic actuator device, brshless DC motor, rotating machinery and low-frequency filter.
Brief description of the drawings
Fig. 1 is 200 times of scanning electron microscope diagrams of inorganic-organic insulating barrier soft-magnetic composite material of test one preparation.
Detailed description of the invention
Detailed description of the invention one: present embodiment is a kind of preparation method of inorganic-organic insulating barrier soft-magnetic composite material, specifically completes according to the following steps:
One, prepare solidliquid mixture: magnetic is put into cleaning agent, then be ultrasonic cleaning 10min～20min under 24KHz～35KHz in supersonic frequency, filtration obtains cleaning rear magnetic, after cleaning, add ethanol and oleic acid in magnetic, and the ammoniacal liquor that is 20%～30% by mass concentration is adjusted to 8.5～9.5 by pH value, then carry out ultrasonic dispersion or dispersed with stirring, obtain solidliquid mixture; The mass ratio of the oleic acid described in step 1 and magnetic is (0.03～0.2): 1; The volume ratio of the oleic acid described in step 1 and ethanol is 1:(40～75); Cleaning agent described in step 1 is distilled water;
Two, prepare the solidliquid mixture of magnetic surface coated silica layer: in the solidliquid mixture obtaining to step 1, add ethanol, then adopting mass concentration is that 20%～30% ammoniacal liquor is adjusted to 8.5～9.5 by pH value, then low whipping speed is stirring reaction under 600r/min～1200r/min and the pH value condition that is 8.5～9.5, ethyl orthosilicate is divided into 2～4 parts, in stirring reaction process, add 1 part of ethyl orthosilicate at interval of 0.5h～1.5h, add for the last time after ethyl orthosilicate, stirring reaction 0.5h～3h under condition that to continue low whipping speed and be 600r/min～1200r/min and pH value be 8.5～9.5, obtain the solidliquid mixture of magnetic surface coated silica layer, the volume ratio of the ethanol adding described in step 2 and solidliquid mixture is (2～4): 1, in the gross mass of the ethyl orthosilicate adding described in step 2 and solidliquid mixture, the mass ratio of magnetic is (0.25～0.4): 1,
Three, prepare the solidliquid mixture of magnetic surface coated Si silicate glass: in the solidliquid mixture of the magnetic surface coated silica layer obtaining to step 2, adding oleic acid, ethyl orthosilicate and mass concentration is metal alkoxide/organic solution of 10%～20%, then adopting mass concentration is that 20%～30% ammoniacal liquor is adjusted to 8.5～9.5 by pH value, and low whipping speed is stirring reaction 1h～6h under 600r/min～1200r/min and the pH value condition that is 8.5～9.5, obtain the solidliquid mixture of magnetic surface coated Si silicate glass; In the solidliquid mixture of the oleic acid adding described in step 3 and magnetic surface coated silica layer, the mass ratio of magnetic is (0.05～0.1): 1; The volume ratio of the solidliquid mixture of the ethyl orthosilicate adding described in step 3 and magnetic surface coated silica layer is (0.25～0.6): 1; In metal alkoxide/organic solution that the mass concentration adding described in step 3 is 10%～20%, in the solidliquid mixture of metal alkoxide and magnetic surface coated silica layer, the mass ratio of magnetic is (0.05～0.6): 1; In metal alkoxide/organic solution described in step 3, the chemical formula of lower metal alkoxide is M (OR) x; Wherein said M (OR) xin M be a kind of in Ti, B, Be, Mn, In, Ge, Al, Zr, Na, K, Li, Mg, Ca, Mg and Ba or wherein several combination; Wherein said M (OR) xin R be C nh 2n+1, and described C nh 2n+1middle n is 1～4; Wherein said M (OR) xin x be 1～5, and described M (OR) xbe electroneutral;
Four, cleaning-drying: the solidliquid mixture of the magnetic surface coated Si silicate glass obtaining in step 3 is left standstill to 10min～30min, then separate, clean separating the solid obtaining, solid after cleaning is put into drying box, be dry 20min～360min at 40 DEG C～80 DEG C in temperature, dried solid is screened with electromagnet, obtain the coated magnetic of silicate glass;
Five, mix: it is in the coupling agent solution of 10mPas～10000mPas that magnetic coated silicate glass is added to viscosity, then take vibratory milling polishing, planetary type ball-milling polishing or mechanical agitation to mix, finally be dried, till being dried to constant weight, obtain mixture; In the coated magnetic of silicate glass described in step 5, in magnetic and coupling agent solution, the mass ratio of solute is 100:(0.2～3.0); In coupling agent solution described in step 5, solute is coupling agent, and solvent is one or more the mixture in water, methyl alcohol, ethanol, isopropyl alcohol, butanols, ethanol, toluene, benzene, dimethylbenzene, stearic acid and atoleine; Wherein said coupling agent is silane coupler, titanate coupling agent or aluminate coupling agent;
Six, compacting for the first time: the mixture that step 5 is obtained is transferred in mould, is then compressing under 0.2MPa～10MPa in mechanical pressure, obtains preform in mould;
Seven, be coated with organic polymer: in the mixture first obtaining by organic polymer performed polymer and step 5, the mass ratio of magnetic is (0.2～7): 100 take organic polymer performed polymer, then organic polymer performed polymer is added in organic solvent, after mixing, obtaining viscosity is organic polymer performed polymer/ORGANIC SOLVENT MIXTURES of 10mpas～10000mpas, organic polymer performed polymer/the ORGANIC SOLVENT MIXTURES that is 10mpas～10000mpas by viscosity again adds in the mould with preform that step 6 obtains, then be to suppress 1min～10min under 0.2MPa～10MPa in mechanical pressure, obtain the preform of coated Si silicate glass/organic polymer performed polymer,
Eight, heat treatment: the preform that step 7 is obtained to coated Si silicate glass/organic polymer performed polymer carries out protective atmosphere heat treatment or vacuum heat, obtains inorganic-organic insulating barrier soft-magnetic composite material;
Protective atmosphere heat treatment concrete operations described in step 8 are as follows: the preform that first step 7 is obtained to coated Si silicate glass/organic polymer performed polymer is placed in nitrogen, under argon gas or hydrogen atmosphere, then be warming up to 200 DEG C～900 DEG C with 8 DEG C of heating rates/min～12 DEG C/min, and at nitrogen, under argon gas or hydrogen shield and temperature be that the preform that under 200 DEG C～900 DEG C conditions, step 7 is obtained to coated Si silicate glass/organic polymer performed polymer is heat-treated 10min～300min, then be cooled to room temperature with 8 DEG C of rate of temperature fall/min～12 DEG C/min, obtain inorganic-organic insulating barrier soft-magnetic composite material,
Vacuum heat concrete operations described in step 8 are as follows: the preform that first step 7 is obtained to coated Si silicate glass/organic polymer performed polymer is placed under vacuum condition, then so that 8 DEG C of heating rates/min～12 DEG C/min is warming up to 200 DEG C～900 DEG C, is 10 in vacuum -1pa～10 -3pa and temperature are that the preform that under 200 DEG C～900 DEG C conditions, step 7 is obtained to coated Si silicate glass/organic polymer performed polymer is heat-treated 10min～300min, then be cooled to room temperature, obtain inorganic-organic insulating barrier soft-magnetic composite material with 8 DEG C of rate of temperature fall/min～12 DEG C/min.
Present embodiment on magnetic surface coated Si silicate glass as insulating barrier, re-use coupling agent and mixed with resin, obtain the blank of inorganic-organic insulating barrier soft-magnetic composite material by cure under pressure, obtaining inorganic-organic insulating barrier soft-magnetic composite material through annealing; Owing to adopting silicate glass as clad, therefore the soft-magnetic composite material of preparing with this Magnaglo can be annealed under higher temperature, make soft-magnetic composite material have excellent magnetic property, this provides wide space in the application in larger field for soft-magnetic composite material.
More than the fracture strength of soft-magnetic composite material prepared by present embodiment reaches 45MPa, maximum permeability reaches more than 330.
The soft-magnetic composite material of preparing due to present embodiment has good magnetic, so can be applicable to the fields such as switching magnetic-resistance, resonant inductance, anti-lock brake sensor, electromagnetic actuator device, brshless DC motor, rotating machinery and low-frequency filter.
Detailed description of the invention two: the difference of present embodiment and detailed description of the invention one is: the magnetic described in step 1 is pure Fe powder, Fe-Ni-Co based metal powder, Fe-Ni based metal powder, Fe-Si-Al based metal powder, Fe-Co based metal powder, Fe-Si based metal powder, Fe-P based metal powder, Fe 3o 4powder or Fe-Cr based metal powder, and the particle diameter of described magnetic is 10 μ m～500 μ m.Other are identical with detailed description of the invention one.
Detailed description of the invention three: one of present embodiment and detailed description of the invention one or two difference is: the ultrasonic dispersion concrete operations described in step 1 are as follows: be ultrasonic dispersion 1h～2h under 24KHz～35KHz in supersonic frequency.Other are identical with detailed description of the invention one or two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one or two difference is: the dispersed with stirring concrete operations described in step 1 are as follows: low whipping speed is dispersed with stirring 1h～2h under 200r/min～1200r/min.Other are identical with detailed description of the invention one or two.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to three difference is: the organic polymer performed polymer described in step 7 is polyethylene performed polymer, polypropylene performed polymer, ethylene-ethyl acetate copolymer performed polymer, nylon 6 performed polymers, nylon 66 performed polymers, nylon 6/66 performed polymer, poly phenylene sulfoether performed polymer, poly-sub-benzene thioketones performed polymer, PET performed polymer, polybutylene terephthalate performed polymer, polyimide prepolymer, PEI performed polymer, polyamidoimide performed polymer, polystyrene performed polymer, acrylonitritrile-styrene resin performed polymer, polyvinyl chloride performed polymer, Vingon performed polymer, vinyl chloride-vinylidene chloride copolymer performed polymer, haloflex performed polymer, PMA performed polymer, polymethyl methacrylate performed polymer, polyacrylonitrile performed polymer, polymethacrylonitrile performed polymer, tetrafluoroethylene/perfluoro alkyl vinyl ether copolymer performed polymer, tetrafluoroethylene/hexafluoropropylene performed polymer, Kynoar performed polymer, dimethyl silicone polymer performed polymer, polyphenylene oxide performed polymer, polyether-ether-ketone performed polymer, polyether-ketone performed polymer, polyarylate performed polymer, polysulfones performed polymer, polyether sulfone performed polymer, polyformaldehyde performed polymer, Merlon performed polymer, polyvinyl acetate performed polymer, polyvinyl formal performed polymer, polyvinyl butyral resin performed polymer, polybutene performed polymer, polyisobutene performed polymer, polymethylpentene performed polymer, butadiene resin performed polymer, polyethylene oxide performed polymer, hydroxy phenyl estrodur performed polymer, Parylene resin prepolymer, silicones performed polymer, epoxy resin prepolymer, phenolic resin performed polymer, EP rubbers performed polymer, polybutadiene rubber performed polymer, SBR styrene butadiene rubbers performed polymer, a kind of or two kinds and two or more mixture in chloroprene rubber performed polymer and SBS performed polymer.Other are identical with detailed description of the invention one to three.
When organic polymer performed polymer described in present embodiment is mixture, between each component, be mixed by any ratio.
Detailed description of the invention six: present embodiment is a kind of preparation method of inorganic-organic insulating barrier soft-magnetic composite material, specifically completes according to the following steps:
One, prepare solidliquid mixture: magnetic is put into cleaning agent, then be ultrasonic cleaning 10min～20min under 24KHz～35KHz in supersonic frequency, filtration obtains cleaning rear magnetic, after cleaning, add ethanol and oleic acid in magnetic, and the ammoniacal liquor that is 20%～30% by mass concentration is adjusted to 8.5～9.5 by pH value, then carry out ultrasonic dispersion or dispersed with stirring, obtain solidliquid mixture; The mass ratio of the oleic acid described in step 1 and magnetic is (0.03～0.2): 1; The volume ratio of the oleic acid described in step 1 and ethanol is 1:(40～75); Cleaning agent described in step 1 is distilled water;
Two, prepare the solidliquid mixture of magnetic surface coated silica layer: in the solidliquid mixture obtaining to step 1, add ethanol, then adopting mass concentration is that 20%～30% ammoniacal liquor is adjusted to 8.5～9.5 by pH value, then low whipping speed is stirring reaction under 600r/min～1200r/min and the pH value condition that is 8.5～9.5, ethyl orthosilicate is divided into 2～4 parts, in stirring reaction process, add 1 part of ethyl orthosilicate at interval of 0.5h～1.5h, add for the last time after ethyl orthosilicate, stirring reaction 0.5h～3h under condition that to continue low whipping speed and be 600r/min～1200r/min and pH value be 8.5～9.5, obtain the solidliquid mixture of magnetic surface coated silica layer, the volume ratio of the ethanol adding described in step 2 and solidliquid mixture is (2～4): 1, in the gross mass of the ethyl orthosilicate adding described in step 2 and solidliquid mixture, the mass ratio of magnetic is (0.25～0.4): 1,
Three, cleaning-drying: the solidliquid mixture of the magnetic surface coated silica layer obtaining in step 2 is left standstill to 10min～30min, then separate, clean separating the solid obtaining, solid after cleaning is put into drying box, be dry 20min～360min at 40 DEG C～80 DEG C in temperature, dried solid is screened with electromagnet, obtain the magnetic of coated with silica;
Four, mix: it is in the coupling agent solution of 10mpas～10000mpas that the magnetic of coated with silica is added to viscosity, then take vibratory milling polishing, planetary type ball-milling polishing or mechanical agitation to mix, finally be dried, till being dried to constant weight, obtain mixture; In the magnetic of the coated with silica described in step 4, in magnetic and coupling agent solution, the mass ratio of solute is 100:(0.2～3.0); In coupling agent solution described in step 4, solute is coupling agent, and solvent is one or more the mixture in water, methyl alcohol, ethanol, isopropyl alcohol, butanols, ethanol, toluene, benzene, dimethylbenzene, stearic acid and atoleine; Wherein said coupling agent is silane coupler, titanate coupling agent or aluminate coupling agent;
Five, compacting for the first time: the mixture that step 4 is obtained is transferred in mould, is then compressing under 0.2MPa～10MPa in mechanical pressure, obtains preform in mould;
Six, be coated with organic polymer: in the mixture first obtaining by organic polymer performed polymer and step 4, the mass ratio of magnetic is (0.2～7): 100 take organic polymer performed polymer, then organic polymer performed polymer is added in organic solvent, after mixing, obtaining viscosity is organic polymer performed polymer/ORGANIC SOLVENT MIXTURES of 10mpas～10000mpas, organic polymer performed polymer/the ORGANIC SOLVENT MIXTURES that is 10mpas～10000mpas by viscosity again adds in the mould with preform that step 5 obtains, then be to suppress 1min～10min under 0.2MPa～10MPa in mechanical pressure, obtain the preform of coated silica/organic polymer performed polymer,
Seven, heat treatment: the preform that step 6 is obtained to coated silica/organic polymer performed polymer carries out protective atmosphere heat treatment or vacuum heat, obtains inorganic-organic insulating barrier soft-magnetic composite material;
Protective atmosphere heat treatment concrete operations described in step 7 are as follows: the preform that first step 6 is obtained to coated silica/organic polymer performed polymer is placed in nitrogen, under argon gas or hydrogen atmosphere, then be warming up to 200 DEG C～900 DEG C with 8 DEG C of heating rates/min～12 DEG C/min, and at nitrogen, under argon gas or hydrogen shield and temperature be that the preform that under 200 DEG C～900 DEG C conditions, step 6 is obtained to coated silica/organic polymer performed polymer is heat-treated 10min～300min, then be cooled to room temperature with 8 DEG C of rate of temperature fall/min～12 DEG C/min, obtain inorganic-organic insulating barrier soft-magnetic composite material,
Vacuum heat concrete operations described in step 7 are as follows: the preform that first step 6 is obtained to coated silica/organic polymer performed polymer is placed under vacuum condition, then so that 8 DEG C of heating rates/min～12 DEG C/min is warming up to 200 DEG C～900 DEG C, is 10 in vacuum -1pa～10 -3pa and temperature are that the preform that under 200 DEG C～900 DEG C conditions, step 6 is obtained to coated silica/organic polymer performed polymer is heat-treated 10min～300min, then be cooled to room temperature, obtain inorganic-organic insulating barrier soft-magnetic composite material with 8 DEG C of rate of temperature fall/min～12 DEG C/min.
Present embodiment on magnetic surface coated Si silicate glass or silica as insulating barrier, re-use coupling agent and mixed with resin, obtain the blank of inorganic-organic insulating barrier soft-magnetic composite material by cure under pressure, obtaining inorganic-organic insulating barrier soft-magnetic composite material through annealing; Owing to adopting silicate glass or silica as clad, therefore the soft-magnetic composite material of preparing with this Magnaglo can be annealed under higher temperature, make soft-magnetic composite material have excellent magnetic property, this provides wide space in the application in larger field for soft-magnetic composite material.
More than the fracture strength of soft-magnetic composite material prepared by present embodiment reaches 45MPa, maximum permeability reaches more than 330.
The soft-magnetic composite material of preparing due to present embodiment has good magnetic, so can be applicable to the fields such as switching magnetic-resistance, resonant inductance, anti-lock brake sensor, electromagnetic actuator device, brshless DC motor, rotating machinery and low-frequency filter.
Detailed description of the invention seven: the difference of present embodiment and detailed description of the invention six is: the magnetic described in step 1 is pure Fe powder, Fe-Ni-Co based metal powder, Fe-Ni based metal powder, Fe-Si-Al based metal powder, Fe-Co based metal powder, Fe-Si based metal powder, Fe-P based metal powder, Fe 3o 4powder or Fe-Cr based metal powder, and the particle diameter of described magnetic is 10 μ m～500 μ m.Other are identical with detailed description of the invention six.
Detailed description of the invention eight: one of present embodiment and detailed description of the invention six or seven difference is: the ultrasonic dispersion concrete operations described in step 1 are as follows: be ultrasonic dispersion 1h～2h under 24KHz～35KHz in supersonic frequency.Other are identical with detailed description of the invention six or seven.
Detailed description of the invention nine: one of present embodiment and detailed description of the invention six or seven difference is: the dispersed with stirring concrete operations described in step 1 are as follows: low whipping speed is dispersed with stirring 1h～2h under 200r/min～1200r/min.Other are identical with detailed description of the invention six or seven.
Detailed description of the invention ten: one of present embodiment and detailed description of the invention six to nine difference is: the organic polymer performed polymer described in step 6 is polyethylene performed polymer, polypropylene performed polymer, ethylene-ethyl acetate copolymer performed polymer, nylon 6 performed polymers, nylon 66 performed polymers, nylon 6/66 performed polymer, poly phenylene sulfoether performed polymer, poly-sub-benzene thioketones performed polymer, PET performed polymer, polybutylene terephthalate performed polymer, polyimide prepolymer, PEI performed polymer, polyamidoimide performed polymer, polystyrene performed polymer, acrylonitritrile-styrene resin performed polymer, polyvinyl chloride performed polymer, Vingon performed polymer, vinyl chloride-vinylidene chloride copolymer performed polymer, haloflex performed polymer, PMA performed polymer, polymethyl methacrylate performed polymer, polyacrylonitrile performed polymer, polymethacrylonitrile performed polymer, tetrafluoroethylene/perfluoro alkyl vinyl ether copolymer performed polymer, tetrafluoroethylene/hexafluoropropylene performed polymer, Kynoar performed polymer, dimethyl silicone polymer performed polymer, polyphenylene oxide performed polymer, polyether-ether-ketone performed polymer, polyether-ketone performed polymer, polyarylate performed polymer, polysulfones performed polymer, polyether sulfone performed polymer, polyformaldehyde performed polymer, Merlon performed polymer, polyvinyl acetate performed polymer, polyvinyl formal performed polymer, polyvinyl butyral resin performed polymer, polybutene performed polymer, polyisobutene performed polymer, polymethylpentene performed polymer, butadiene resin performed polymer, polyethylene oxide performed polymer, hydroxy phenyl estrodur performed polymer, Parylene resin prepolymer, silicones performed polymer, epoxy resin prepolymer, phenolic resin performed polymer, EP rubbers performed polymer, polybutadiene rubber performed polymer, SBR styrene butadiene rubbers performed polymer, a kind of or two kinds and two or more mixture in chloroprene rubber performed polymer and SBS performed polymer.Other are identical with detailed description of the invention six to nine.
When organic polymer performed polymer described in present embodiment is mixture, between each component, be mixed by any ratio.
Adopt following verification experimental verification effect of the present invention
Test one: a kind of preparation method of soft-magnetic composite material, specifically completes according to the following steps:
One, prepare solidliquid mixture: pure 150g Fe powder is put into distilled water, then be ultrasonic cleaning 10min under 30KHz in supersonic frequency, filtration obtains cleaning rear magnetic, after cleaning, add 660mL ethanol and 10.72g oleic acid in magnetic, and the ammoniacal liquor that is 25% by mass concentration is adjusted to 9 by pH value, then low whipping speed is dispersed with stirring 1.5h under 800r/min, obtains solidliquid mixture;
Two, prepare the solidliquid mixture of magnetic surface coated silica layer: in the solidliquid mixture obtaining to step 1, add 2340mL ethanol, then adopting mass concentration is that 25% ammoniacal liquor is adjusted to 9 by pH value, then low whipping speed is stirring reaction under 800r/min and the pH value condition that is 9,44.64g ethyl orthosilicate is divided into 2 parts, in stirring reaction process, add 1 part of ethyl orthosilicate at interval of 1h, add for the last time after ethyl orthosilicate stirring reaction 2h under condition that to continue low whipping speed and be 800r/min and pH value be 9; Obtain the solidliquid mixture of magnetic surface coated silica layer;
Three, prepare the solidliquid mixture of magnetic surface coated Si silicate glass: in the solidliquid mixture of the magnetic surface coated silica layer obtaining to step 2, add caustic alcohol/ethanolic solution that 12.95g oleic acid, 61.38g ethyl orthosilicate and 120mL mass concentration are 15%, then adopting mass concentration is that 25% ammoniacal liquor is adjusted to 9 by pH value, and low whipping speed is stirring reaction 3h under 800r/min and the pH value condition that is 9, obtain the solidliquid mixture of magnetic surface coated Si silicate glass;
Four, cleaning-drying: the solidliquid mixture of the magnetic surface coated Si silicate glass obtaining in step 3 is left standstill to 30min, then separate, adopt washed with de-ionized water 1 time to separating the solid obtaining, adopt again ethanol to clean 1 time, solid after cleaning is put into drying box, be dry 240min at 60 DEG C in temperature, dried solid is screened with electromagnet, obtain the coated magnetic of silicate glass;
Five, mixing: magnetic coated 100g silicate glass is added in coupling agent solution, and then low whipping speed is to mix under 30r/min, is finally dry 30min (solid constant weight) at 60 DEG C in temperature, obtains mixture; In coupling agent solution described in step 5, solute is 0.3g silane coupler, and solvent is 2mL water, 5mL methyl alcohol and 10mL ethanol;
Six, compacting for the first time: the mixture that step 5 is obtained is transferred in mould, is then compressing under 1MPa in mechanical pressure, obtains preform in mould;
Seven, be coated with organic polymer: 3g epoxy resin (model 6101) performed polymer is added in toluene, after mixing, obtain epoxy resin prepolymer/toluene mixture that viscosity is 30mPas, epoxy resin prepolymer/the toluene mixture that is 30mPas by viscosity again adds in the mould with preform that step 6 obtains, then be to suppress 2min under 1.5MPa in mechanical pressure, obtain the preform of coated Si silicate glass/organic polymer performed polymer;
Eight, heat treatment: the protective atmosphere heat treatment concrete operations described in step 8 are as follows: the preform that first step 7 is obtained to coated Si silicate glass/organic polymer performed polymer is placed under nitrogen atmosphere; then be warming up to 650 DEG C with 10 DEG C/min of heating rate; and under nitrogen protection and temperature be that the preform that under 650 DEG C of conditions, step 7 is obtained to coated Si silicate glass/organic polymer performed polymer is heat-treated 40min; then be cooled to room temperature with 10 DEG C/min of rate of temperature fall, obtain inorganic-organic insulating barrier soft-magnetic composite material.
The ATOMET_1001HP water-atomized iron powder of the ChunFeFen Shi Canadian Quebec Metal Powder Company Ltd. described in this test.
Inorganic-organic insulating barrier soft-magnetic composite material to this test preparation detects, and the electromagnetic performance of the inorganic-organic insulating barrier soft-magnetic composite material of this test preparation and mechanical performance index are as table 1.
Table 1
μ mfor the maximum permeability of the inorganic-organic insulating barrier soft-magnetic composite material of this test preparation, the maximum permeability of the inorganic-organic insulating barrier soft-magnetic composite material of known test preparation is 371, B 10000represent the magnetic induction intensity value of the inorganic-organic insulating barrier soft-magnetic composite material of this test preparation when magnetizing field is 10000A/m, Br is the residual magnetic flux density of the inorganic-organic insulating barrier soft-magnetic composite material of this test preparation, Hc is the coercivity of the inorganic-organic insulating barrier soft-magnetic composite material of this test preparation, W (50Hz) and W (200Hz) represent that respectively the inorganic-organic insulating barrier soft-magnetic composite material of this test preparation is at maximum magnetic field strength 1T, the iron loss value under alternative frequency 50Hz and 200Hz.
Inorganic-organic insulating barrier soft-magnetic composite material by known test preparation of above-mentioned performance has excellent magnetic property, and therefore the inorganic-organic insulating barrier soft-magnetic composite material of this test preparation can be applicable to the fields such as switching magnetic-resistance, resonant inductance, anti-lock brake sensor, electromagnetic actuator device, brshless DC motor, rotating machinery and low-frequency filter.
Adopt the inorganic-organic insulating barrier soft-magnetic composite material of this test of sem observation preparation, as shown in Figure 1, Fig. 1 is 200 times of scanning electron microscope diagrams of inorganic-organic insulating barrier soft-magnetic composite material of test one preparation, can see that by Fig. 1 iron powder is evenly distributed in insulant, this is conducive to improve the resistivity of material, to reach isotropic magnetic property.
Test two: a kind of preparation method of soft-magnetic composite material, specifically completes according to the following steps:
One, prepare solidliquid mixture: pure 150g Fe powder is put into distilled water, then be ultrasonic cleaning 10min under 30KHz in supersonic frequency, filtration obtains cleaning rear magnetic, after cleaning, add 660mL ethanol and 10.72g oleic acid in magnetic, and the ammoniacal liquor that is 25% by mass concentration is adjusted to 9 by pH value, then low whipping speed is dispersed with stirring 1.5h under 800r/min., obtain solidliquid mixture;
Two, prepare the solidliquid mixture of magnetic surface coated silica layer: in the solidliquid mixture obtaining to step 1, add 2340mL ethanol, then adopting mass concentration is that 25% ammoniacal liquor is adjusted to 9 by pH value, then low whipping speed is stirring reaction under 800r/min and the pH value condition that is 9,44.64g ethyl orthosilicate is divided into 2 parts, in stirring reaction process, add 1 part of ethyl orthosilicate at interval of 1h, add for the last time after ethyl orthosilicate stirring reaction 2h under condition that to continue low whipping speed and be 800r/min and pH value be 9; Obtain the solidliquid mixture of magnetic surface coated silica layer;
Three, cleaning-drying: the solidliquid mixture of the magnetic surface coated silica layer obtaining in step 2 is left standstill to 30min, then separate, adopt washed with de-ionized water 1 time to separating the solid obtaining, adopt again ethanol to clean 1 time, solid after cleaning is put into drying box, be dry 240min at 60 DEG C in temperature, dried solid is screened with electromagnet, obtain the magnetic of coated with silica;
Four, mixing: the magnetic that 100g is obtained to coated with silica adds in coupling agent solution, and then low whipping speed is to mix under 30r/min, is finally dry 30min (solid constant weight) at 60 DEG C in temperature, obtains mixture; In coupling agent solution described in step 5, solute is 0.3g silane coupler, and solvent is 2mL water, 5mL methyl alcohol and 10mL ethanol;
Five, compacting for the first time: the mixture that step 4 is obtained is transferred in mould, is then compressing under 1MPa in mechanical pressure, obtains preform in mould;
Six, be coated with organic polymer: 3g epoxy resin (model 6101) performed polymer is added in toluene, after mixing, obtain epoxy resin prepolymer/toluene mixture that viscosity is 30mPas, epoxy resin prepolymer/the toluene mixture that is 30mPas by viscosity again adds in the mould with preform that step 5 obtains, then be to suppress 2min under 1.5MPa in mechanical pressure, obtain the preform of coated silica/organic polymer performed polymer;
Seven, heat treatment: the preform that first step 6 is obtained to coated silica/organic polymer performed polymer is placed under nitrogen atmosphere; then be warming up to 650 DEG C with 10 DEG C/min of heating rate; and under nitrogen protection and temperature be that the preform that under 650 DEG C of conditions, step 6 is obtained to coated silica/organic polymer performed polymer is heat-treated 40min; then be cooled to room temperature with 10 DEG C/min of rate of temperature fall, obtain inorganic-organic insulating barrier soft-magnetic composite material.
The ATOMET_1001HP water-atomized iron powder of the ChunFeFen Shi Canadian Quebec Metal Powder Company Ltd. described in this test.
Inorganic-organic insulating barrier soft-magnetic composite material to this test preparation detects, and the electromagnetic performance of the inorganic-organic insulating barrier soft-magnetic composite material of this test preparation and mechanical performance index are as table 2.
Table 2
μ mfor the maximum permeability of the inorganic-organic insulating barrier soft-magnetic composite material of this test preparation, the maximum permeability of the inorganic-organic insulating barrier soft-magnetic composite material of known test preparation is 334, B 10000represent the magnetic induction intensity value of the inorganic-organic insulating barrier soft-magnetic composite material of this test preparation when magnetizing field is 10000A/m, Br is the residual magnetic flux density of the inorganic-organic insulating barrier soft-magnetic composite material of this test preparation, Hc is the coercivity of the inorganic-organic insulating barrier soft-magnetic composite material of this test preparation, W (50Hz) and W (200Hz) represent that respectively the inorganic-organic insulating barrier soft-magnetic composite material of this test preparation is at maximum magnetic field strength 1T, the iron loss value under alternative frequency 50Hz and 200Hz.
Inorganic-organic insulating barrier soft-magnetic composite material by known test preparation of above-mentioned performance has excellent magnetic property, and therefore the inorganic-organic insulating barrier soft-magnetic composite material of this test preparation can be applicable to the fields such as switching magnetic-resistance, resonant inductance, anti-lock brake sensor, electromagnetic actuator device, brshless DC motor, rotating machinery and low-frequency filter.

Claims (10)

1. a preparation method for inorganic-organic insulating barrier soft-magnetic composite material, is characterized in that the preparation method of inorganic-organic insulating barrier soft-magnetic composite material completes according to the following steps:
One, prepare solidliquid mixture: magnetic is put into cleaning agent, then be ultrasonic cleaning 10min～20min under 24KHz～35KHz in supersonic frequency, filtration obtains cleaning rear magnetic, after cleaning, add ethanol and oleic acid in magnetic, and the ammoniacal liquor that is 20%～30% by mass concentration is adjusted to 8.5～9.5 by pH value, then carry out ultrasonic dispersion or dispersed with stirring, obtain solidliquid mixture; The mass ratio of the oleic acid described in step 1 and magnetic is (0.03～0.2): 1; The volume ratio of the oleic acid described in step 1 and ethanol is 1:(40～75); Cleaning agent described in step 1 is distilled water;
Two, prepare the solidliquid mixture of magnetic surface coated silica layer: in the solidliquid mixture obtaining to step 1, add ethanol, then adopting mass concentration is that 20%～30% ammoniacal liquor is adjusted to 8.5～9.5 by pH value, then low whipping speed is stirring reaction under 600r/min～1200r/min and the pH value condition that is 8.5～9.5, ethyl orthosilicate is divided into 2～4 parts, in stirring reaction process, add 1 part of ethyl orthosilicate at interval of 0.5h～1.5h, add for the last time after ethyl orthosilicate, stirring reaction 0.5h～3h under condition that to continue low whipping speed and be 600r/min～1200r/min and pH value be 8.5～9.5, obtain the solidliquid mixture of magnetic surface coated silica layer, the volume ratio of the ethanol adding described in step 2 and solidliquid mixture is (2～4): 1, in the gross mass of the ethyl orthosilicate adding described in step 2 and solidliquid mixture, the mass ratio of magnetic is (0.25～0.4): 1,
Three, prepare the solidliquid mixture of magnetic surface coated Si silicate glass: in the solidliquid mixture of the magnetic surface coated silica layer obtaining to step 2, adding oleic acid, ethyl orthosilicate and mass concentration is metal alkoxide/organic solution of 10%～20%, then adopting mass concentration is that 20%～30% ammoniacal liquor is adjusted to 8.5～9.5 by pH value, and low whipping speed is stirring reaction 1h～6h under 600r/min～1200r/min and the pH value condition that is 8.5～9.5, obtain the solidliquid mixture of magnetic surface coated Si silicate glass; In the solidliquid mixture of the oleic acid adding described in step 3 and magnetic surface coated silica layer, the mass ratio of magnetic is (0.05～0.1): 1; The volume ratio of the solidliquid mixture of the ethyl orthosilicate adding described in step 3 and magnetic surface coated silica layer is (0.25～0.6): 1; In metal alkoxide/organic solution that the mass concentration adding described in step 3 is 10%～20%, in the solidliquid mixture of metal alkoxide and magnetic surface coated silica layer, the mass ratio of magnetic is (0.05～0.6): 1; In metal alkoxide/organic solution described in step 3, the chemical formula of lower metal alkoxide is M (OR) x; Wherein said M (OR) xin M be a kind of in Ti, B, Be, Mn, In, Ge, Al, Zr, Na, K, Li, Mg, Ca, Mg and Ba or wherein several combination; Wherein said M (OR) xin R be C nh 2n+1, and described C nh 2n+1middle n is 1～4; Wherein said M (OR) xin x be 1～5, and described M (OR) xbe electroneutral;
Four, cleaning-drying: the solidliquid mixture of the magnetic surface coated Si silicate glass obtaining in step 3 is left standstill to 10min～30min, then separate, clean separating the solid obtaining, solid after cleaning is put into drying box, be dry 20min～360min at 40 DEG C～80 DEG C in temperature, dried solid is screened with electromagnet, obtain the coated magnetic of silicate glass;
Five, mix: it is in the coupling agent solution of 10mPas～10000mPas that magnetic coated silicate glass is added to viscosity, then take vibratory milling polishing, planetary type ball-milling polishing or mechanical agitation to mix, finally be dried, till being dried to constant weight, obtain mixture; In the coated magnetic of silicate glass described in step 5, in magnetic and coupling agent solution, the mass ratio of solute is 100:(0.2～3.0); In coupling agent solution described in step 5, solute is coupling agent, and solvent is one or more the mixture in water, methyl alcohol, ethanol, isopropyl alcohol, butanols, ethanol, toluene, benzene, dimethylbenzene, stearic acid and atoleine; Wherein said coupling agent is silane coupler, titanate coupling agent or aluminate coupling agent;
Six, compacting for the first time: the mixture that step 5 is obtained is transferred in mould, is then compressing under 0.2MPa～10MPa in mechanical pressure, obtains preform in mould;
Seven, be coated with organic polymer: in the mixture first obtaining by organic polymer performed polymer and step 5, the mass ratio of magnetic is (0.2～7): 100 take organic polymer performed polymer, then organic polymer performed polymer is added in organic solvent, after mixing, obtaining viscosity is organic polymer performed polymer/ORGANIC SOLVENT MIXTURES of 10mPas～10000mPas, organic polymer performed polymer/the ORGANIC SOLVENT MIXTURES that is 10mPas～10000mPas by viscosity again adds in the mould with preform that step 6 obtains, then be to suppress 1min～10min under 0.2MPa～10MPa in mechanical pressure, obtain the preform of coated Si silicate glass/organic polymer performed polymer,
Eight, heat treatment: the preform that step 7 is obtained to coated Si silicate glass/organic polymer performed polymer carries out protective atmosphere heat treatment or vacuum heat, obtains inorganic-organic insulating barrier soft-magnetic composite material;
Protective atmosphere heat treatment concrete operations described in step 8 are as follows: the preform that first step 7 is obtained to coated Si silicate glass/organic polymer performed polymer is placed in nitrogen, under argon gas or hydrogen atmosphere, then be warming up to 200 DEG C～900 DEG C with 8 DEG C of heating rates/min～12 DEG C/min, and at nitrogen, under argon gas or hydrogen shield and temperature be that the preform that under 200 DEG C～900 DEG C conditions, step 7 is obtained to coated Si silicate glass/organic polymer performed polymer is heat-treated 10min～300min, then be cooled to room temperature with 8 DEG C of rate of temperature fall/min～12 DEG C/min, obtain inorganic-organic insulating barrier soft-magnetic composite material,
Vacuum heat concrete operations described in step 8 are as follows: the preform that first step 7 is obtained to coated Si silicate glass/organic polymer performed polymer is placed under vacuum condition, then so that 8 DEG C of heating rates/min～12 DEG C/min is warming up to 200 DEG C～900 DEG C, is 10 in vacuum -1pa～10 -3pa and temperature are that the preform that under 200 DEG C～900 DEG C conditions, step 7 is obtained to coated Si silicate glass/organic polymer performed polymer is heat-treated 10min～300min, then be cooled to room temperature, obtain inorganic-organic insulating barrier soft-magnetic composite material with 8 DEG C of rate of temperature fall/min～12 DEG C/min.
2. the preparation method of a kind of inorganic-organic insulating barrier soft-magnetic composite material according to claim 1, is characterized in that the magnetic described in step 1 is pure Fe powder, Fe-Ni-Co based metal powder, Fe-Ni based metal powder, Fe-Si-Al based metal powder, Fe-Co based metal powder, Fe-Si based metal powder, Fe-P based metal powder, Fe 3o 4powder or Fe-Cr based metal powder, and the particle diameter of described magnetic is 10 μ m～500 μ m.
3. the preparation method of a kind of inorganic-organic insulating barrier soft-magnetic composite material according to claim 2, is characterized in that the ultrasonic dispersion concrete operations described in step 1 are as follows: be ultrasonic dispersion 1h～2h under 24KHz～35KHz in supersonic frequency.
4. the preparation method of a kind of inorganic-organic insulating barrier soft-magnetic composite material according to claim 2, is characterized in that the dispersed with stirring concrete operations described in step 1 are as follows: low whipping speed is dispersed with stirring 1h～2h under 200r/min～1200r/min.
5. the preparation method of a kind of inorganic-organic insulating barrier soft-magnetic composite material according to claim 1, is characterized in that the organic polymer performed polymer described in step 7 is polyethylene performed polymer, polypropylene performed polymer, ethylene-ethyl acetate copolymer performed polymer, nylon 6 performed polymers, nylon 66 performed polymers, nylon 6/66 performed polymer, poly phenylene sulfoether performed polymer, poly-sub-benzene thioketones performed polymer, PET performed polymer, polybutylene terephthalate performed polymer, polyimide prepolymer, PEI performed polymer, polyamidoimide performed polymer, polystyrene performed polymer, acrylonitritrile-styrene resin performed polymer, polyvinyl chloride performed polymer, Vingon performed polymer, vinyl chloride-vinylidene chloride copolymer performed polymer, haloflex performed polymer, PMA performed polymer, polymethyl methacrylate performed polymer, polyacrylonitrile performed polymer, polymethacrylonitrile performed polymer, tetrafluoroethylene/perfluoro alkyl vinyl ether copolymer performed polymer, tetrafluoroethylene/hexafluoropropylene performed polymer, Kynoar performed polymer, dimethyl silicone polymer performed polymer, polyphenylene oxide performed polymer, polyether-ether-ketone performed polymer, polyether-ketone performed polymer, polyarylate performed polymer, polysulfones performed polymer, polyether sulfone performed polymer, polyformaldehyde performed polymer, Merlon performed polymer, polyvinyl acetate performed polymer, polyvinyl formal performed polymer, polyvinyl butyral resin performed polymer, polybutene performed polymer, polyisobutene performed polymer, polymethylpentene performed polymer, butadiene resin performed polymer, polyethylene oxide performed polymer, hydroxy phenyl estrodur performed polymer, Parylene resin prepolymer, silicones performed polymer, epoxy resin prepolymer, phenolic resin performed polymer, EP rubbers performed polymer, polybutadiene rubber performed polymer, SBR styrene butadiene rubbers performed polymer, a kind of or two kinds and two or more mixture in chloroprene rubber performed polymer and SBS performed polymer.
6. a preparation method for inorganic-organic insulating barrier soft-magnetic composite material, is characterized in that the preparation method of inorganic-organic insulating barrier soft-magnetic composite material completes according to the following steps:
One, prepare solidliquid mixture: magnetic is put into cleaning agent, then be ultrasonic cleaning 10min～20min under 24KHz～35KHz in supersonic frequency, filtration obtains cleaning rear magnetic, after cleaning, add ethanol and oleic acid in magnetic, and the ammoniacal liquor that is 20%～30% by mass concentration is adjusted to 8.5～9.5 by pH value, then carry out ultrasonic dispersion or dispersed with stirring, obtain solidliquid mixture; The mass ratio of the oleic acid described in step 1 and magnetic is (0.03～0.2): 1; The volume ratio of the oleic acid described in step 1 and ethanol is 1:(40～75); Cleaning agent described in step 1 is distilled water;
Two, prepare the solidliquid mixture of magnetic surface coated silica layer: in the solidliquid mixture obtaining to step 1, add ethanol, then adopting mass concentration is that 20%～30% ammoniacal liquor is adjusted to 8.5～9.5 by pH value, then low whipping speed is stirring reaction under 600r/min～1200r/min and the pH value condition that is 8.5～9.5, ethyl orthosilicate is divided into 2～4 parts, in stirring reaction process, add 1 part of ethyl orthosilicate at interval of 0.5h～1.5h, add for the last time after ethyl orthosilicate, stirring reaction 0.5h～3h under condition that to continue low whipping speed and be 600r/min～1200r/min and pH value be 8.5～9.5, obtain the solidliquid mixture of magnetic surface coated silica layer, the volume ratio of the ethanol adding described in step 2 and solidliquid mixture is (2～4): 1, in the gross mass of the ethyl orthosilicate adding described in step 2 and solidliquid mixture, the mass ratio of magnetic is (0.25～0.4): 1,
Three, cleaning-drying: the solidliquid mixture of the magnetic surface coated silica layer obtaining in step 2 is left standstill to 10min～30min, then separate, clean separating the solid obtaining, solid after cleaning is put into drying box, be dry 20min～360min at 40 DEG C～80 DEG C in temperature, dried solid is screened with electromagnet, obtain the magnetic of coated with silica;
Four, mix: it is in the coupling agent solution of 10mPas～10000mPas that the magnetic of coated with silica is added to viscosity, then take vibratory milling polishing, planetary type ball-milling polishing or mechanical agitation to mix, finally be dried, till being dried to constant weight, obtain mixture; In the magnetic of the coated with silica described in step 4, in magnetic and coupling agent solution, the mass ratio of solute is 100:(0.2～3.0); In coupling agent solution described in step 4, solute is coupling agent, and solvent is one or more the mixture in water, methyl alcohol, ethanol, isopropyl alcohol, butanols, ethanol, toluene, benzene, dimethylbenzene, stearic acid and atoleine; Wherein said coupling agent is silane coupler, titanate coupling agent or aluminate coupling agent;
Five, compacting for the first time: the mixture that step 4 is obtained is transferred in mould, is then compressing under 0.2MPa～10MPa in mechanical pressure, obtains preform in mould;
Six, be coated with organic polymer: in the mixture first obtaining by organic polymer performed polymer and step 4, the mass ratio of magnetic is (0.2～7): 100 take organic polymer performed polymer, then organic polymer performed polymer is added in organic solvent, after mixing, obtaining viscosity is organic polymer performed polymer/ORGANIC SOLVENT MIXTURES of 10mPas～10000mPas, organic polymer performed polymer/the ORGANIC SOLVENT MIXTURES that is 10mPas～10000mPas by viscosity again adds in the mould with preform that step 5 obtains, then be to suppress 1min～10min under 0.2MPa～10MPa in mechanical pressure, obtain the preform of coated silica/organic polymer performed polymer,
Seven, heat treatment: the preform that step 6 is obtained to coated silica/organic polymer performed polymer carries out protective atmosphere heat treatment or vacuum heat, obtains inorganic-organic insulating barrier soft-magnetic composite material;
Protective atmosphere heat treatment concrete operations described in step 7 are as follows: the preform that first step 6 is obtained to coated silica/organic polymer performed polymer is placed in nitrogen, under argon gas or hydrogen atmosphere, then be warming up to 200 DEG C～900 DEG C with 8 DEG C of heating rates/min～12 DEG C/min, and at nitrogen, under argon gas or hydrogen shield and temperature be that the preform that under 200 DEG C～900 DEG C conditions, step 6 is obtained to coated silica/organic polymer performed polymer is heat-treated 10min～300min, then be cooled to room temperature with 8 DEG C of rate of temperature fall/min～12 DEG C/min, obtain inorganic-organic insulating barrier soft-magnetic composite material,
Vacuum heat concrete operations described in step 7 are as follows: the preform that first step 6 is obtained to coated silica/organic polymer performed polymer is placed under vacuum condition, then so that 8 DEG C of heating rates/min～12 DEG C/min is warming up to 200 DEG C～900 DEG C, is 10 in vacuum -1pa～10 -3pa and temperature are that the preform that under 200 DEG C～900 DEG C conditions, step 6 is obtained to coated silica/organic polymer performed polymer is heat-treated 10min～300min, then be cooled to room temperature, obtain inorganic-organic insulating barrier soft-magnetic composite material with 8 DEG C of rate of temperature fall/min～12 DEG C/min.
7. the preparation method of a kind of inorganic-organic insulating barrier soft-magnetic composite material according to claim 6, is characterized in that the magnetic described in step 1 is pure Fe powder, Fe-Ni-Co based metal powder, Fe-Ni based metal powder, Fe-Si-Al based metal powder, Fe-Co based metal powder, Fe-Si based metal powder, Fe-P based metal powder, Fe 3o 4powder or Fe-Cr based metal powder, and the particle diameter of described magnetic is 10 μ m～500 μ m.
8. the preparation method of a kind of inorganic-organic insulating barrier soft-magnetic composite material according to claim 7, is characterized in that the ultrasonic dispersion concrete operations described in step 1 are as follows: be ultrasonic dispersion 1h～2h under 24KHz～35KHz in supersonic frequency.
9. the preparation method of a kind of inorganic-organic insulating barrier soft-magnetic composite material according to claim 7, is characterized in that the dispersed with stirring concrete operations described in step 1 are as follows: low whipping speed is dispersed with stirring 1h～2h under 200r/min～1200r/min.
10. the preparation method of a kind of inorganic-organic insulating barrier soft-magnetic composite material according to claim 6, is characterized in that the organic polymer performed polymer described in step 6 is polyethylene performed polymer, polypropylene performed polymer, ethylene-ethyl acetate copolymer performed polymer, nylon 6 performed polymers, nylon 66 performed polymers, nylon 6/66 performed polymer, poly phenylene sulfoether performed polymer, poly-sub-benzene thioketones performed polymer, PET performed polymer, polybutylene terephthalate performed polymer, polyimide prepolymer, PEI performed polymer, polyamidoimide performed polymer, polystyrene performed polymer, acrylonitritrile-styrene resin performed polymer, polyvinyl chloride performed polymer, Vingon performed polymer, vinyl chloride-vinylidene chloride copolymer performed polymer, haloflex performed polymer, PMA performed polymer, polymethyl methacrylate performed polymer, polyacrylonitrile performed polymer, polymethacrylonitrile performed polymer, tetrafluoroethylene/perfluoro alkyl vinyl ether copolymer performed polymer, tetrafluoroethylene/hexafluoropropylene performed polymer, Kynoar performed polymer, dimethyl silicone polymer performed polymer, polyphenylene oxide performed polymer, polyether-ether-ketone performed polymer, polyether-ketone performed polymer, polyarylate performed polymer, polysulfones performed polymer, polyether sulfone performed polymer, polyformaldehyde performed polymer, Merlon performed polymer, polyvinyl acetate performed polymer, polyvinyl formal performed polymer, polyvinyl butyral resin performed polymer, polybutene performed polymer, polyisobutene performed polymer, polymethylpentene performed polymer, butadiene resin performed polymer, polyethylene oxide performed polymer, hydroxy phenyl estrodur performed polymer, Parylene resin prepolymer, silicones performed polymer, epoxy resin prepolymer, phenolic resin performed polymer, EP rubbers performed polymer, polybutadiene rubber performed polymer, SBR styrene butadiene rubbers performed polymer, a kind of or two kinds and two or more mixture in chloroprene rubber performed polymer and SBS performed polymer.
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