CN100595850C - Soft magnetic composite organically/inorganically compound insulation coating powdered iron and preparation method thereof - Google Patents
Soft magnetic composite organically/inorganically compound insulation coating powdered iron and preparation method thereof Download PDFInfo
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- CN100595850C CN100595850C CN200710186855A CN200710186855A CN100595850C CN 100595850 C CN100595850 C CN 100595850C CN 200710186855 A CN200710186855 A CN 200710186855A CN 200710186855 A CN200710186855 A CN 200710186855A CN 100595850 C CN100595850 C CN 100595850C
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- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000009413 insulation Methods 0.000 title claims description 29
- 150000001875 compounds Chemical class 0.000 title claims description 10
- 238000000576 coating method Methods 0.000 title abstract description 14
- 239000011248 coating agent Substances 0.000 title abstract description 13
- 230000005291 magnetic effect Effects 0.000 title abstract description 10
- 239000012256 powdered iron Substances 0.000 title description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 27
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 12
- 229920000642 polymer Polymers 0.000 claims abstract description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 55
- 238000005253 cladding Methods 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000003054 catalyst Substances 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 9
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 8
- 230000007062 hydrolysis Effects 0.000 claims description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims description 8
- 239000003822 epoxy resin Substances 0.000 claims description 7
- 229920000647 polyepoxide Polymers 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 239000005011 phenolic resin Substances 0.000 claims description 4
- 229910000077 silane Inorganic materials 0.000 claims description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229920001568 phenolic resin Polymers 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 25
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 4
- 239000012212 insulator Substances 0.000 abstract description 3
- 239000012774 insulation material Substances 0.000 abstract 4
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 239000011162 core material Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 229910021332 silicide Inorganic materials 0.000 description 2
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 150000001845 chromium compounds Chemical class 0.000 description 1
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 235000019580 granularity Nutrition 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- Powder Metallurgy (AREA)
Abstract
The invention relates to a soft magnetic composite material, in particular to a soft magnetic composite material of organic/inorganic insulator-coated ferrous powder and a process for preparation by sol-gel. In the soft magnetic composite material of organic/inorganic insulated-coated ferrous powder, the soft magnetic composite material comprises insulation material coated ferrous powder, whereinthe quantity of the insulation material is 0.05%-1.5% of quality of the coated ferrous powder according to percentage by weight, the insulation material uniformly and dispersedly compounded by materials containing sol and polymer of silicon dioxide, and the polymer is 5%-30% of the insulation material in accordance with percentage by weight. The invention has the advantages that 1) the sol of silicon dioxide is generated in-situ of the solution and coated on the surface of the ferrous powder, 2) by employing the organic/inorganic insulator to coat the ferrous powder, combining the advantages of organic and inorganic coatings, the coating effect and mechanical property of insulated layers is excellent, and 3) the technique is simple and cost is low.
Description
Technical field
The present invention relates to soft-magnetic composite material, relate in particular to a kind of soft-magnetic composite material of organic/inorganic insulation cladding iron powder and pass through colloidal sol---the method for preparing gel.
Background technology
Soft-magnetic composite material (SMC) is made up of soft magnetism powder body material (as iron powder) and the surface insulation medium that accounts for seldom part, can one goes on foot be pressed into the parts with complicated shape by powder metallurgy technology, and has good isotropism magnetic property.The physical property of material has determined it to be suitable as very much the core material of motor, and has brought revolutionary variation to design of electrical motor.Existing studies show that, the performance of magnetic core and its insulating material and addition thereof are closely related.It determines its density to a great extent, magnetic flux, resistance, the mechanical strength of eddy current loss and pressed magnetic powder core.But up to the present, the application of these materials in industry and commerce also do not have major progress, and simultaneously for factors such as trade secrets, relevant achievement in research report is less.At present, SMC is mainly based on the macromolecular material coating, and the material of its shortcoming after compacting can not carry out sintering processes, and the density of material, mechanical performance and relevant magnetic performance can not satisfy its application under situations such as machine field and high temperature.Thereby the researcher begins to turn to the employing inorganic matter to coat.
The grand grade of the Zou Lian of powder metallurgy National Key Laboratory of Zhongnan Polytechnic Univ adds an amount of magnesium bichromate, phosphoric acid, urea and glycerine and is mixed with coating solution in 1000ml distilled water.To spray iron powder in hydrogen, behind 800 ℃ of reductase 12s hour, sieve, and get the powder that certain particle size distributes and evenly mixes according to a certain percentage,, dry at 200 ℃ times at last, obtain cladding iron powder then at the stirred in water bath preliminarily dried with covering liquid.
Chinese patent (application number: 97102244.5, publication number: CN1167990) the report ferrocart core, be used for the preparation method of the iron powder and the ferrocart core of ferrocart core.The silicon dioxide gel, silicone resin and the organic titanic compound that in iron powder, have added.By making said iron powder through the cured under 50～250 ℃, powder compact, at 550～650 ℃ of annealing in inert atmosphere, a kind of basic ferrous powder granules of acquisition by particle size with 75～200 μ m.This silicon dioxide gel is not to adopt sol-gel technology synthetic, silicon dioxide dispersed bad, and be difficult to realize even the mixing with silicone resin and organic titanic compound, and there is not gel process, be difficult to obtain the uniform insulation film.
Chinese invention patent (application number: 200610053628.3) disclose a kind of manufacture method of high temperature resistant iron powder core.It is in 100 weight portion granularities less than 300 purpose electrolytic iron powders, add 10～20 weight portions, concentration is 0.02%～0.20%, pH value is 6.3～6.8 chromium anhydride solution, puts into the drum-type powder-frying machine and fries and do, frying dried temperature is 100～150 ℃; Add 0.1～0.5 weight portion basic magnesium carbonate, mix granulation, add the organic epoxy type binding agent of 0.2～0.6 weight portion and the zinc stearate of 0.2～0.6 weight portion, compression molding.The dielectric film that this invention adopts the chromium anhydride solution method to produce is more firm than the dielectric film of phosphoric acid and acetone method generation, the resistivity height, survivable when compression molding, and also its core loss is less, finished product can use 200 ℃ of temperature, and shortcoming can not be carried out sintering processes in material.
Chinese invention patent (application number: 02120634.1, the feeromagnetic metal based powders, with the manufacture method of its ferrocart core made and feeromagnetic metal based powders) a kind of iron-based powder and ferrocart core that contains the high temperature insulation coating be provided.The coating that will contain silicones and pigment joins in the raw material powder that mainly contains ferromagnetic metal, particularly iron, stirs and mixes, and after this carries out dried to form the coating that contains silicones and pigment on the surface of iron-based powder.Pigment is a kind of in metal oxide, metal nitride, metal carbides, mineral matter and the glass.Coating is ejected into form on the iron-based powder that is in the fluidisation attitude and contains at least a coating in silicide, titaniferous compound, zirconium thing, phosphide and the chromium compounds.
(Journal of Magnetism and Magnetic Materials (2006) doi:10.1016/j.jmmm.2006.08.002) directly adopts SiO to S.N.B.Hodgson etc.
2Colloidal sol (being obtained by hydrolysis by tetraethoxysilane or tetraethoxysilane and methyl trimethoxy base silane) mixes, and adopts SiO
2Coated iron powder.Since the fragility of silicon dioxide, the coated iron powder that this technology obtains, the SiO that it is surperficial
2The easy embrittlement of dielectric film, coated effect are not very desirable.
It is all not really desirable to be equipped with dielectric film in order to the top legal system, as has the easy embrittlement of dielectric film, coats aspect problem such as inhomogeneous, complicated process of preparation.Up to the present, this type of research application in industry does not also have major progress, and the SMC dielectric film of further seeking excellent performance is very important.
Summary of the invention
In order to solve the easy embrittlement of above-mentioned dielectric film, coat inhomogeneous, complicated process of preparation, can not carry out after its compacting of soft magnet composite material the technical problem of sintering processes, an object of the present invention is to provide a kind of soft-magnetic composite material of organic/inorganic insulation cladding iron powder.It has has taken into account advantage, the covered effect of insulating barrier and the mechanical property excellent characteristics that organic and inorganic thing coats.
Another object of the present invention provides the preparation method of the soft-magnetic composite material of above-mentioned organic/inorganic insulation cladding iron powder.This preparation method has adopted colloidal sol---and gel has the advantages that technology is simple, cost is low.
In order to realize first above-mentioned purpose, the present invention has adopted following method:
The soft-magnetic composite material of organic/inorganic insulation cladding iron powder, this soft-magnetic composite material comprises the iron powder that insulant coats, wherein the amount of this insulant is 0.05%～1.5% of institute's cladding iron powder quality by weight percentage, described insulant constitutes by the even dispersion of the material that comprises silicon dioxide gel and polymer is compound, and the percentage by weight that polymer accounts for insulant is 5%～30%.As preferably, the amount of above-mentioned by weight percentage insulant is 0.05%～1% of institute's cladding iron powder quality.
As preferably, above-mentioned insulant can also comprise the nanometer additive of 5%～10% percentage by weight.Described nanometer additive can be nano magnesia powder or nano alumina powder.Nano magnesia powder or nano alumina powder have high-temperature stability, help sintering processes, and the adhesive property of sintering is good.
As preferably, above-mentioned polymer is one or more in epoxy resin, methyl methacrylate and the phenolic resins.
In order to realize second above-mentioned purpose, the present invention has adopted following method:
The preparation method of the soft-magnetic composite material of above-mentioned organic/inorganic insulation cladding iron powder, it comprises the steps:
1. with the silicon dioxide gel precursor, hydrolysis in organic solvent and water adds the Preparation of Catalyst silicon dioxide gel;
2. in above-mentioned silicon dioxide gel, add polymer, be uniformly dispersed, preparation insulant colloidal sol;
3. add iron powder then in above-mentioned insulant colloidal sol, mix, by adding catalyst control sol system gel, last ageing obtains the soft-magnetic composite material of organic/inorganic insulation cladding iron powder.
As preferably, the silicon dioxide gel precursor of above-mentioned step in 1. is selected from a kind of in tetraethoxysilane, the methyl trimethoxy base silane or 2 kinds.
As preferably, the organic solvent of above-mentioned step in 1. is selected from a kind of in ethanol, ethylene glycol, the acetone or 2 kinds.Adding ethanol is because the solubility of silicon dioxide gel precursor in water is little, and the solubility in ethanol is more much bigger than the solubility in water.Ethanol can not only the silicon dioxide gel precursor with dissolve each other, can dissolve each other with water again, can guarantee that like this hydrolysis of alkoxide carries out in homogeneous phase solution.
As preferably, above-mentioned step 1., the catalyst in 3. is selected from HCI, HNO
3, HClO
4, HF, H
3PO
4, NaOH, NH
3H
2O, CaCl
2Silicon dioxide gel precursor hydrolysis rate is accelerated with the acid-base value of solution, polycondensation reaction speed is then very fast in neutrality, alkalescence or strongly acidic solution, therefore by control pH value, adopt the two-step method of back under alkali condition under acid condition earlier, hydrolysis and polycondensation reaction are carried out fast, can be saved time greatly.
As preferably, above-mentioned step 1. in the mol ratio of silicon in water and the silicon dioxide gel precursor be 2～4.It is generally acknowledged when amount of water is less than isocenter (water silicon is than R=2), be polymerized to the dealcoholysis condensation; And when amount of water during greater than isocenter, polymerization is then based on dehydrating condensation.Increase the R value, help promoting hydrolysis on the one hand, the concentration that can dilute silicide on the other hand causes the prolongation of gel time indirectly.When because water still is one of product of dehydrating condensation,, can cause the hydrolysis again of established silicon oxygen bond so amount of water is excessive.Simultaneously, high water silicon ratio also can cause not dissolving each other between liquid phase.Therefore, in actual production, in order to improve reaction speed, water silicon ratio can select between 2～4.
The present invention coats one deck organic/inorganic composite insulation layer on the iron powder surface, developing organic/inorganic is insulating material, having solved the organic insulator coating is can not carry out sintering processes after its compacting of soft magnet composite material of leading, the density of material, mechanical performance and relevant magnetic performance can not well satisfy its shortcoming in the application of machine field, also overcome the fragility of simple inorganic matter coated insulation layer, for a kind of new method that provides is provided for the insulation of SMC material.
The present invention adopts colloidal sol---and gel process prepares the advantage of the compound insulant cladding iron powder soft-magnetic composite material method of organic/inorganic: 1) silicon dioxide original position in colloidal sol generates and is coated on the iron powder surface; 2) adopt organically/inorganically compound insulation coating powdered iron, taken into account the advantage that organic and inorganic thing coats, the covered effect of insulating barrier and mechanical property excellence; 3) technology is simple, cost is low.
Description of drawings
Fig. 1 is the stereoscan photograph that the product of the embodiment of the invention 1 amplifies 500 multiples.
Fig. 2 is the stereoscan photograph that the product of the embodiment of the invention 1 amplifies 1000 multiples.
Fig. 3 is the stereoscan photograph that the product of the embodiment of the invention 1 amplifies 2000 multiples.
Embodiment
Embodiment 1
Water 13ml, tetraethoxysilane 40ml, ethanol 21ml are mixed stirring 30 minutes, whipping process splashes into several hydrochloric acid (catalyst) and obtains transparent aqueous silicon dioxide gel, add epoxy resin (5g is dissolved in the epoxy resin solution of 50ml ethanol), continue to stir, the transparent insulant colloidal sol that formation mixes joins the 5000g iron powder in this insulant colloidal sol ageing at room temperature then, behind the collosol and gel, obtain the soft-magnetic composite material of organic/inorganic insulation cladding iron powder.The stereoscan photograph of the different amplification of cladding iron powder as Figure 1-3.Can see that from Fig. 1-3 to prepare the iron powder surfacing of silicon dioxide and the compound coating of epoxy resin with sol-gel technology even, not have the crack.
Embodiment 2
Water 10ml, tetraethoxysilane 10ml, methyl trimethoxy base silane 20ml, ethanol 20ml are mixed stirring 30 minutes, whipping process splashes into several hydrochloric acid (catalyst) and obtains transparent aqueous silicon dioxide gel, add phenolic resins (5g is dissolved in the phenol resin solution of 50ml ethanol), continue to stir, the transparent insulant colloidal sol that formation mixes, the 5000g iron powder is joined in this insulant colloidal sol, put into temperature then and be made as 60 ℃ baking oven ageing, behind the collosol and gel, obtain the soft-magnetic composite material of organic/inorganic insulation cladding iron powder.
Embodiment 3
Water 15ml, tetraethoxysilane 35ml, ethanol 25ml are mixed stirring 30 minutes, whipping process splashes into several ammoniacal liquor (catalyst) and obtains transparent aqueous silicon dioxide gel, add the 3g methyl methacrylate and splash into several azo initiators, continue to stir, the transparent insulant colloidal sol that formation mixes joins the 5000g iron powder in this insulant colloidal sol ageing at room temperature then, behind the collosol and gel, obtain the soft-magnetic composite material of organic/inorganic insulation cladding iron powder.
Embodiment 4
Water 10ml, tetraethoxysilane 20ml, ethanol 20ml are mixed stirring 30 minutes, whipping process splashes into several hydrochloric acid (catalyst) and obtains transparent aqueous silicon dioxide gel, add epoxy resin (5g is dissolved in the epoxy resin solution of 50ml ethanol), continue to stir, form transparent insulant colloidal sol, add the nano magnesia powder again, the 5000g iron powder is joined in this insulant colloidal sol, ageing at room temperature then behind the collosol and gel, obtains the soft-magnetic composite material of organic/inorganic insulation cladding iron powder.
Claims (9)
1. the soft-magnetic composite material of organic/inorganic insulation cladding iron powder, it is characterized in that: this soft-magnetic composite material comprises the iron powder that insulant coats, wherein the amount of insulant is 0.05%～1.5% of institute's cladding iron powder quality by weight percentage, described insulant constitutes by the even dispersion of the material of silicon dioxide gel, nanometer additive and polymer is compound, the percentage by weight that polymer accounts for insulant is 5%～30%, and the percentage by weight that nanometer additive accounts for insulant is 5%～10%.
2. the soft-magnetic composite material of organic/inorganic insulation cladding iron powder according to claim 1, it is characterized in that: the amount of insulant is 0.05%～1% of institute's cladding iron powder quality by weight percentage.
3. the soft-magnetic composite material of organic/inorganic insulation cladding iron powder according to claim 1, it is characterized in that: described nanometer additive is nano magnesia powder or nano alumina powder.
4. the soft-magnetic composite material of organic/inorganic insulation cladding iron powder according to claim 1 and 2, it is characterized in that: polymer is one or more in epoxy resin, methyl methacrylate and the phenolic resins.
5. the preparation method of the soft-magnetic composite material of organic/inorganic insulation cladding iron powder according to claim 1 is characterized in that comprising the steps:
1. with the silicon dioxide gel precursor, hydrolysis in organic solvent and water adds the Preparation of Catalyst silicon dioxide gel;
2. in above-mentioned silicon dioxide gel, add polymer, be uniformly dispersed, preparation insulant colloidal sol;
3. add iron powder then in above-mentioned insulant colloidal sol, mix, by adding catalyst control sol system gel, last ageing obtains the soft-magnetic composite material of organic/inorganic insulation cladding iron powder.
6. the preparation method of the soft-magnetic composite material of organic/inorganic according to claim 5 insulation cladding iron powder is characterized in that: the silicon dioxide gel precursor of step in 1. is selected from a kind of in tetraethoxysilane, the methyl trimethoxy base silane or 2 kinds.
7. according to the preparation method of the soft-magnetic composite material of the described organic/inorganic of claim 6 insulation cladding iron powder, it is characterized in that: the organic solvent of step in 1. is selected from a kind of in ethanol, ethylene glycol, the acetone or 2 kinds.
8. according to the preparation method of the soft-magnetic composite material of the described organic/inorganic of claim 7 insulation cladding iron powder, it is characterized in that: step 1., the catalyst in 3. is selected from HCl, HNO
3, HClO
4, HF, H
3PO
4, NaOH, NH
3H
2O, CaCl
2
9. according to the preparation method of the soft-magnetic composite material of the described organic/inorganic of claim 7 insulation cladding iron powder, it is characterized in that: step 1. in the mol ratio of silicon in water and the silicon dioxide gel precursor be 2～4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710186855A CN100595850C (en) | 2007-09-05 | 2007-11-22 | Soft magnetic composite organically/inorganically compound insulation coating powdered iron and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710071107 | 2007-09-05 | ||
| CN200710071107.5 | 2007-09-05 | ||
| CN200710186855A CN100595850C (en) | 2007-09-05 | 2007-11-22 | Soft magnetic composite organically/inorganically compound insulation coating powdered iron and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101226807A CN101226807A (en) | 2008-07-23 |
| CN100595850C true CN100595850C (en) | 2010-03-24 |
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| CN103240411A (en) * | 2013-05-20 | 2013-08-14 | 哈尔滨工业大学 | Production methods of inorganic-organic insulation layer soft magnetic composites |
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| CN112366056A (en) * | 2020-10-23 | 2021-02-12 | 浙江工业大学 | High-frequency low-loss soft magnetic composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103240411A (en) * | 2013-05-20 | 2013-08-14 | 哈尔滨工业大学 | Production methods of inorganic-organic insulation layer soft magnetic composites |
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