CN102528024B - Method for preparing insulated iron powder used by soft magnetic composite materials - Google Patents
Method for preparing insulated iron powder used by soft magnetic composite materials Download PDFInfo
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Abstract
A method for preparing insulated iron powder used by soft magnetic composite materials belongs to the technical field of magnetic function materials and powder metallurgy. The process is that a cladding process includes: adding high-purity iron powder with concentration of 0.1-5g/ml for industrialized production into hexafluorotitanic acid or hexafluorozirconic acid cladding solution with concentration of 0.002-0.05g/ml, stirring for 5-60 minutes for reacting at temperature of 20-70 DEG C, filtering and washing, and drying at 50-120 DEG C to obtain insulated iron powder. The method for preparing insulated iron powder used by soft magnetic composite materials has the advantages of being simple in preparing process, high in efficiency and complete in cladding. An insulated cladding layer on the surface of the iron powder can effectively reduce magnetic loss of powder cores of the soft magnetic composite materials, and comprehensive performance of the powder cores can be regulated by controlling thickness of the insulated layer.
Description
Technical field
The invention belongs to magnetic functional material and powder metallurgical technology, particularly a kind of preparation method of insulated iron powder used by soft magnetic composite materials.
Background technology
Soft-magnetic composite material (Soft Magnetic Composites, hereinafter to be referred as SMC) manufacturing of employing PM technique, metal powder granulates (as straight iron powder) by surface insulation forms, can a step be pressed into the parts with complicated shape, and have good Three-Dimensional Isotropic magnetic property and a thermal characteristics, and lower eddy-current loss under high frequency, can have in the motor of working under the motor of complicated shape and magnetic circuit and upper frequency at some and be used as core material, can bring revolutionary variation to the electrical convertors and generators design when obtaining extensive use.Development along with electronics miniaturization and high frequency, micro machine, low-power machine and anti-electromagnetic disturbance element etc. are widely used in automobile, robot, office and home automation device, and the application of SMC in these fields with special performance will produce huge economic benefit.
Insulated iron powder is the important source material of preparation SMC magnetic core, directly has influence on serviceability and the structural strength of magnetic core.In recent years, external leading company has successively developed insulated iron powder, as Sweden
The Somaloy of AB company
TMKIPMG270H of the ATOMET EM-1 of serial, Canadian QMP company and Japanese JFE company etc., and applied for Patents in China.The patent of the Robert Bosch Co., Ltd (Robert Bosch GmbH) of Germany (application number: 03811970.6, publication number: CN1656575A) and Sweden
The patent of AB company (application number: 97192452.X, publication number: CN1211943A) (application number: 200480025248.8, publication number: CN1845805A) all adopt phosphating process to obtain insulated iron powder in the technology; The patent of Japan JFE company (application number: 200480025248.8, publication number: CN1518011A) adopt phosphalugel to coat soft magnetic powder in the technology and make the insulation soft magnet powder.Japan TDK Corp. (application number: 97102244.5, publication number: CN1167990A) successfully made by add silica, silicone resin and organic titanic compound in iron powder the soft magnetism coated composite powder that is formed by iron powder and silicon titanyl rete.in addition, domestic also have similar patented technology to occur, patented technology (application number: 200610040493.7 as Tianyi Superfine Metal Powders Co., Ltd., Jiangsu, publication number: CN1895820A) provide a kind of coupling agent of using, adopt physical method to prepare the method for nano silicon coating carbonyl iron powder after ammoniacal liquor modified carbonyl iron powder or silica surface, the technology of Huzhou Keda Magnetoelectric Co. Ltd. (application number: 200710186855.8, publication number: CN101226807A) adopt sol-gal process to prepare the SMC of silica and organic polymer compound inslation cladding iron powder.
Above method prepares insulated iron powder and all more or less has some problems, and embrittlement as easy in insulating film layer, to coat inhomogeneous, complicated process of preparation, efficient low etc., and the SMC insulation soft magnetic powder of further seeking excellent performance is very important.Up to the present, domestic having no adopts hexafluoro metatitanic acid and hexafluoro zirconate to carry out the report that the iron powder insulating is processed.
Summary of the invention
The object of the present invention is to provide a kind of soft-magnetic composite material (SMC) preparation method of insulated iron powder.Prepared fluorine titanium/zirconic acid molysite inorganic insulating membrane can improve the resistivity of iron powder on the one hand, plays insulating effect, the magnetic loss of energy decrease SMC; This dielectric film resistance to elevated temperatures is better on the other hand, can stand heat treatment more than 550 ℃ and can not damage, and the heat treatment at this temperature can further reduce coercivity and the magnetic loss of SMC magnetic core.The method has advantages of that technique is simple, it is even to coat, efficient is high.
Main processes of the present invention: high-purity iron powder → insulating is processed (mechanical agitation) → filtration → washing → oven dry → insulated iron powder.For solving the problems of the technologies described above the technical scheme that adopts be: certain density iron powder is joined stirring reaction certain hour in fluotitanic acid or fluorine zirconic acid treatment fluid, control certain reaction condition, make the certain thickness high-quality fluorine titanium of iron powder coated with uniform/zirconates clad.Concrete processing step is as follows:
(1) preparation coats treatment fluid, and be specially: hexafluoro metatitanic acid or hexafluoro zirconate are solute, and absolute ethyl alcohol or acetone are solvent, and the control solute concentration is 0.002～0.05g/ml;
(2) high-purity iron powder is joined in the coating treatment fluid, controlling simultaneously iron powder concentration is 0.1～5g/ml, and controlling the treatment fluid temperature is 20～70 ℃, mechanical agitation reaction 5～60min;
(3) filtration washing, and obtain insulated iron powder in 50～120 ℃ of dryings.
Described high-purity iron powder is one or more the composition in the above atomized iron powder of purity 99%, reduced iron powder, electrolytic iron powder or carbonyl iron dust.
As preferably, the solvent in above-mentioned steps (1) can be absolute ethyl alcohol or acetone, and is preferably absolute ethyl alcohol; Solute concentration is preferably 0.005～0.01g/ml.
As preferably, the high-purity iron powder in above-mentioned steps (2) can be atomized iron powder, reduced iron powder, electrolytic iron powder and carbonyl iron dust, and is preferably water-atomized iron powder, and its purity is high and suppression performance good, and concentration is preferably 0.1～2g/ml; The treatment fluid temperature is preferably 30～60 ℃; Reaction time is preferably 20～30min.
The raw material iron powder provides basic magnetic property for the SMC magnetic core, and the concentration for the treatment of fluid, reaction temperature and time can directly affect quality and the thickness of dielectric film, and further have influence on the final performance of magnetic core.In certain limit, insulating film layer thickness increases, and the magnetic loss of magnetic core significantly reduces, but magnetic conductivity also can be lost; Surpass the certain thickness scope, its magnetic property will worsen rapidly, and magnetic conductivity significantly reduces, and magnetic loss increases.Control suitable treatment process and condition, can make the insulated iron powder of actual required magnetic property excellence.
The invention has the advantages that:
1, the insulating barrier on iron powder surface has good resistance to elevated temperatures, has improved insulated iron powder to be subject to insulating barrier and the too low problem of heat treatment temperature all the time;
2, the prepared SMC magnetic core of the present invention has good comprehensive magnetic energy, and can adjust according to actual needs;
3, technique is simple, and efficient is high, is suitable for industrial applications.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention, but embodiment does not limit the present invention, and do not address part and be applicable to prior art in invention.
Embodiment 1
Getting a certain amount of hexafluoro metatitanic acid solution joins and is made into reactant liquor in absolute ethyl alcohol, controlling hexafluoro metatitanic acid concentration is 0.005g/ml, heating in water bath for reaction liquid temp to 30 ℃, be that high-purity atomized iron powder (controlling its concentration is 0.2g/ml) of 99.5% joins mechanical agitation reaction 30min in reactant liquor with purity, use absolute ethanol washing 3 times after centrifugal filtration, be placed in 50 ℃ of fully dryings, make insulated iron powder.Iron powder is processed the rear surface through insulating and is become Paint Gloss, and glossiness is also better, and clad is evenly complete.Before and after contrast coats and processes, the magnetic property of the made magnetic core of iron powder is found, the maximum relative permeability of insulated iron powder magnetic core becomes 291 by 328, magnetic loss when magnetic strength 1T frequency 50Hz drops to 6.8W/kg by 9.1W/kg, and the magnetic loss when magnetic strength 1T frequency 400Hz drops to 85.2W/kg by 212W/kg, and magnetic loss has reduced by 60%.
Embodiment 2
What the raw material iron powder adopted atomized iron powder and reduced iron powder mass ratio 1: 1 mixes iron powder, purity 99.3%.Getting a certain amount of hexafluoro zirconate solution joins and is made into reactant liquor in anhydrous propanone, controlling hexafluoro zirconate concentration is 0.05g/ml, heating in water bath for reaction liquid temp to 60 ℃, the mixing iron powder of preparation is joined in reactant liquor, controlling iron powder concentration is 5g/ml, and mechanical agitation reaction 60min washs 3 times with anhydrous propanone after centrifugal filtration, be placed in 120 ℃ of fully dryings, make insulated iron powder.Before and after contrast coats and processes, the magnetic property of the made magnetic core of iron powder is found, the maximum relative permeability of insulated iron powder magnetic core becomes 263 by 318, and the magnetic loss when magnetic strength 1T frequency 400Hz drops to 63.5W/kg by 201W/kg.
Embodiment 3
What the raw material iron powder adopted atomized iron powder and carbonyl iron dust mass ratio 1: 1 mixes iron powder, purity 99.4%.Getting a certain amount of hexafluoro metatitanic acid solution joins and is made into reactant liquor in absolute ethyl alcohol, controlling hexafluoro metatitanic acid concentration is 0.02g/ml, heating in water bath for reaction liquid temp to 50 ℃, the mixing iron powder of preparation is joined in reactant liquor, controlling iron powder concentration is 2g/ml, and mechanical agitation reaction 5min uses absolute ethanol washing 3 times after centrifugal filtration, be placed in 80 ℃ of fully dryings, make insulated iron powder.Before and after contrast coats and processes, the maximum relative permeability of the prepared magnetic core of iron powder becomes 225 by 302, and the magnetic loss when magnetic strength 1T frequency 400Hz drops to 92W/kg by 196W/kg.
Embodiment 4
The raw material iron powder adopts reduced iron powder, purity 99.4%.Getting a certain amount of hexafluoro zirconate solution joins and is made into reactant liquor in absolute ethyl alcohol, controlling hexafluoro zirconate concentration is 0.002g/ml, heating in water bath for reaction liquid temp to 70 ℃, iron powder is joined in reactant liquor, controlling its concentration is 0.5g/ml, and mechanical agitation reaction 20min uses absolute ethanol washing 3 times after centrifugal filtration, be placed in 80 ℃ of fully dryings, make insulated iron powder.The maximum relative permeability of the magnetic core that makes is 268, and the magnetic loss when magnetic strength 1T frequency 400Hz is 106W/kg.
Embodiment 5
The raw material iron powder adopts electrolytic iron powder, purity 99.2%.Getting a certain amount of hexafluoro zirconate solution joins and is made into reactant liquor in absolute ethyl alcohol, controlling hexafluoro zirconate concentration is 0.01g/ml, heating in water bath for reaction liquid temp to 40 ℃, iron powder is joined in reactant liquor, controlling its concentration is 1g/ml, and mechanical agitation reaction 30min uses absolute ethanol washing 3 times after centrifugal filtration, be placed in 80 ℃ of fully dryings, make insulated iron powder.The maximum relative permeability of the magnetic core that makes is 239, and the magnetic loss when magnetic strength 1T frequency 400Hz is 96W/kg.
Embodiment 6
The raw material iron powder adopts carbonyl iron dust, purity 99.0%.Getting a certain amount of hexafluoro metatitanic acid solution joins and is made into reactant liquor in anhydrous propanone, controlling hexafluoro metatitanic acid concentration is 0.01g/ml, heating in water bath for reaction liquid temp to 50 ℃, iron powder is joined in reactant liquor, controlling its concentration is 2g/ml, and mechanical agitation reaction 20min washs 3 times with anhydrous propanone after centrifugal filtration, be placed in 70 ℃ of fully dryings, make insulated iron powder.The maximum relative permeability of the magnetic core that makes is 187, and the magnetic loss when magnetic strength 1T frequency 400Hz is 90.6W/kg.
Claims (3)
1. the preparation method of an insulated iron powder used by soft magnetic composite materials, it is characterized in that: processing step is as follows:
(1) preparation coats treatment fluid: hexafluoro metatitanic acid or hexafluoro zirconate are solute, and absolute ethyl alcohol or acetone are solvent, and the control solute concentration is 0.002～0.05g/ml;
(2) high-purity iron powder is joined in the coating treatment fluid, controlling simultaneously high-purity iron powder concentration is 0.1～5g/ml, and controlling the treatment fluid temperature is 20～70 ℃, mechanical agitation reaction 5～60min;
(3) filtration washing, and obtain insulated iron powder in 50～120 ℃ of dryings;
Described high-purity iron powder is one or more the composition in the above atomized iron powder of purity 99%, reduced iron powder, electrolytic iron powder or carbonyl iron dust.
2. the preparation method of insulated iron powder used by soft magnetic composite materials according to claim 1, it is characterized in that: the solvent in step (1) is absolute ethyl alcohol; The concentration of hexafluoro metatitanic acid or hexafluoro zirconate is 0.005～0.01g/ml.
3. the preparation method of insulated iron powder used by soft magnetic composite materials according to claim 1, it is characterized in that: the high-purity iron powder concentration in step (2) is 0.1～2g/ml, and reaction temperature is 30～60 ℃, and the reaction time is 20～30min.
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| CN104028750B (en) * | 2014-06-05 | 2016-04-27 | 浙江大学 | A kind of high bond strength insulating wrapped processing method of soft magnetic metal composite |
| CN104157389B (en) * | 2014-08-06 | 2017-01-18 | 江西磁姆新材料科技有限公司 | Preparing method of high-performance soft magnetism composite materials |
| CN108329021A (en) * | 2017-12-25 | 2018-07-27 | 日照亿鑫电子材料有限公司 | Low-frequency current sensor core material and preparation method thereof |
| CN109216006B (en) * | 2018-08-29 | 2020-06-23 | 深圳顺络电子股份有限公司 | Soft magnetic alloy powder core and preparation method thereof |
| CN111128537B (en) * | 2019-12-27 | 2022-01-25 | 浙江工业大学 | Preparation method of soft magnetic composite material based on fluorozirconic acid hydrolysis |
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| CA2452234A1 (en) * | 2002-12-26 | 2004-06-26 | Jfe Steel Corporation | Metal powder and powder magnetic core using the same |
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