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CN103862033A - Iron powder surface coating processing method - Google Patents

Iron powder surface coating processing method Download PDF

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Publication number
CN103862033A
CN103862033A CN201410100487.0A CN201410100487A CN103862033A CN 103862033 A CN103862033 A CN 103862033A CN 201410100487 A CN201410100487 A CN 201410100487A CN 103862033 A CN103862033 A CN 103862033A
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iron powder
powder
concentration
silane
temperature
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CN201410100487.0A
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李发长
李�一
柳学全
李楠
丁存光
李金普
李立鑫
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Central Iron and Steel Research Institute
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Central Iron and Steel Research Institute
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Abstract

The invention relates to an iron powder surface coating processing method and belongs to the technical field of functional material and powder metallurgy. The process comprises the following steps of: placing iron powder in phosphorizing liquid, stirring for 15 to 60min at a temperature of 20 to 50 DEG C, and filtering, washing and drying; then placing the obtained product in silane treating fluid, stirring for 30 to 120min at a temperature of 20 to 70 DEG C, filtering and washing; and finally, drying at a temperature of 50 to 120 DEG C to obtain coated powder of which the surface is simultaneously provided with a phosphate layer and a siloxane layer. The method adopts the simple preparation process, has high efficiency, is complete to coat, is easy to form the industrial scale; the phosphate coating layer on the surface has high resistivity and can effectively reduce magnetic loss of an iron powder core; and the siloxane coating layer can improve brittleness of the phosphate layer and can improve heat resistance of the coated iron powder.

Description

The coated processing method in a kind of iron powder surface
Technical field
The invention belongs to functional material and powder metallurgical technology, particularly the coated processing method in a kind of iron powder surface.
Background technology
Soft magnetic-powder core adopts PM technique manufacture, the iron-based powder particle by surface with clad forms, can a step be pressed into the parts with complicated shape, and there is good Three-Dimensional Isotropic magnetic property and 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 and be used as core material at some, when obtaining extensive use, can bring revolutionary variation to electrical convertors and generators design.Along with the development of 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 ferrocart core with special performance will produce huge economic benefit in the application in these fields.
Cladding iron powder is the important source material of preparing ferrocart core, directly has influence on serviceability and the structural strength of magnetic core.In recent years, external leading company has successively developed cladded type iron powder, as Sweden kIPMG270H of the ATOMET EM-1 of the SomaloyTM series of AB company, Canadian QMP company and Japanese JFE company etc., and applied for Patents in China.Patent (application number: 03811970.6, publication number: CN1656575A) and the Sweden of the Robert Bosch Co., Ltd (Robert Bosch GmbH) of Germany
Figure BDA0000478234370000012
in the patent (application number: 97192452.X, publication number: CN1211943A) of AB company (application number: 200480025248.8, publication number: CN1845805A) technology, all adopt phosphating process to obtain cladding iron powder; In the patent of JFE company of Japan (application number: 200480025248.8, publication number: CN1518011A) technology, adopt the coated soft magnetic powder of phosphalugel to make high-performance coated composite powder.TDK Corp. of Japan (application number: 97102244.5, publication number: CN1167990A) successfully make by add silica, silicone resin and organic titanic compound in iron powder the coated composite powder being formed by iron powder and silicon titanyl rete.In addition, domestic also have similar patented technology to occur, as the patented technology of Tianyi Superfine Metal Powders Co., Ltd., Jiangsu (application number: 200610040493.7, publication number: CN1895820A) provides a kind of with adopting physical method to prepare the method for nano silicon coating carbonyl iron powder after coupling agent, ammoniacal liquor modified carbonyl iron powder or silica surface; University of Science & Technology, Beijing (application number: 200910093052.7, publication number: CN101658932A) adopt Phosphating Solution and zinc stearate saponification liquor processing iron powder to prepare a kind of self-lubricating insulated iron powder for motor magnetic core; 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; Iron and Steel Research Geueral Inst (application number: 201210018920.7, publication number: CN102528024A) adopt fluotitanic acid covering liquid processing iron powder to develop a kind of preparation method of insulated iron powder used by soft magnetic composite materials.
Above method is prepared cladded type iron powder and is all more or less had some problems, as low in the coated easy embrittlement of rete, coated inhomogeneous, complicated process of preparation, efficiency etc.Up to the present, such application of studying in industry at home does not also make substantial progress, and further seeks that technique is simple, the cladding iron powder preparation method of excellent performance is very important.
Summary of the invention
The object of the present invention is to provide the coated processing method in a kind of iron powder surface, have the advantages that technique is simple, coated evenly, efficiency is high, be applicable to industrialization.Prepared phosphate/siloxanes cladding iron powder, has taken into account organic and inorganic coated advantage, has the feature of covered effect and suppression performance excellence simultaneously.Phosphate inorganic layer has high resistivity, plays insulating effect, can significantly reduce the magnetic loss of ferrocart core; Silane insulating barrier improves clad resistivity on the one hand, can improve on the other hand the fragility of phosphate inorganic clad, and in addition, due to the good resistance to elevated temperatures of siloxanes, it can also improve the resistance to elevated temperatures that is coated rete.
Main processes of the present invention: soft magnetic powder → phosphatization processing → filtration → washing → oven dry → silane treatment → filtration → washing → dry → compound coating iron powder.For solving the problems of the technologies described above the technical scheme adopting be: raw meal is placed in to Phosphating Solution, at 20~50 ℃ of temperature, stir 15~60min, wash after filtration, and be dried, be placed in again silane treatment liquid, at 20~70 ℃ of temperature, stir 30~120min, filtration washing, is finally dried and obtains the surperficial cladding iron powder that simultaneously has phosphate layer and siloxane layer in 50~120 ℃.Concrete processing step has:
(1) preparation Phosphating Solution, phosphoric acid is solute, and absolute ethyl alcohol or acetone are solvent, and controlled concentration is 0.002~0.02g/ml;
(2) soft magnetic powder is joined in Phosphating Solution, control iron powder concentration is 0.1~2g/ml simultaneously, and controlling treatment fluid temperature is 20~50 ℃, mechanical agitation reaction 15~60min;
(3) filtration washing the dry phosphatizing powder that obtains;
(4) preparation silane treatment fluid, organosilan (containing the alkoxyls such as methoxy or ethoxy) is solute, and the mixture of ethanol or ethylene glycol and deionized water is solvent, and control silane concentration is 0.01~0.2g/ml;
(5) phosphatizing powder is joined in silane treatment liquid, control iron powder concentration is 0.1~2g/ml simultaneously, and treatment fluid temperature is 20~70 ℃, and mechanical agitation is processed 30~120min;
(6) filtration washing, and be placed in 50~120 ℃ of fully dry superpacket whitings that obtain.
As preferably, the solvent in above-mentioned steps (1) can be absolute ethyl alcohol or acetone, and is preferably acetone; Solute concentration is preferably 0.005~0.01g/ml.
As preferably, soft magnetic powder in above-mentioned steps (2) can be one or more in reduced iron powder, atomized iron powder, electrolytic iron powder, carbonyl iron dust and various fe-based alloy powder, and be preferably water-atomized iron powder or reduced iron powder, its purity is high and suppression performance good, and concentration is preferably 0.2~1g/ml; Reaction time is preferably no more than 30min.
As preferably, the organosilan in above-mentioned steps (4) can be the silane that contains the alkoxyls such as methoxy or ethoxy, and is preferably the amino silane that molecular weight is larger.
As preferably, the treatment temperature in above-mentioned steps (5) is preferably 20~50 ℃, and the stir process time is preferably 60~120min.
The invention has the advantages that: the prepared coated composite powder of the present invention has phosphate and siloxane layer double-coating structure, taken into account organic and advantage inorganic coating, and made magnetic core resistivity is high, magnetic loss is very low; The siloxanes insulating barrier on iron powder surface has improved the fragility of inorganic coating layer, has improved resistance to elevated temperatures simultaneously; Technique is simple, and efficiency is high, and cost is low, 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
Raw material iron powder adopts high-purity atomized iron powder, controlling its concentration is 0.2g/ml, getting a certain amount of phosphoric acid joins and in acetone, is made into Phosphating Solution, control phosphoric acid concentration is 0.008g/ml, iron powder is joined to room temperature in Phosphating Solution (20 ℃) mechanical agitation reaction 30min, be placed on 50 ℃ for 3 times with acetone filtration washing and be fully dried.Get again in the mixed solution that a certain amount of 3-aminopropyl triethoxysilane joins absolute ethyl alcohol and 5% deionized water and be made into silane treatment liquid after hydrolysis, control silane concentration is 0.01g/ml, above-mentioned phosphatization iron powder is joined to room temperature in treatment fluid (20 ℃) mechanical agitation reaction 120min, be placed on 80 ℃ with absolute ethyl alcohol filtration washing and be fully dried, make phosphate layer and siloxane layer double-coating structure atomized iron powder.The coated magnetic property of processing the made ring-shaped magnetic core of front and back iron powder same process of contrast is found, the maximum relative permeability of magnetic powder core becomes 350 from 385, have to a certain degree and decline, saturation induction density becomes 1.48T from 1.49T, almost do not change, but magnetic loss significantly reduces, magnetic loss in the time of magnetic strength 1T frequency 400Hz drops to 62W/kg by 246W/kg, reduced by 75%, and magnetic loss in the time of magnetic strength 1T frequency 1000Hz drops to 178W/kg by 982W/kg, has reduced by 82%.
Embodiment 2
Raw material iron powder adopts iron-6.5 silicon alloy powder, controlling its concentration is 2g/ml, getting a certain amount of phosphoric acid joins and in acetone, is made into Phosphating Solution, control phosphoric acid concentration is 0.01g/ml, iron powder is joined to 30 ℃ of mechanical agitation reaction 60min in Phosphating Solution, be placed on 50 ℃ for 3 times with acetone filtration washing and be fully dried.Get again in the mixed solution that a certain amount of 3-aminopropyl trimethoxysilane joins absolute ethyl alcohol and 5% deionized water and be made into silane treatment liquid after hydrolysis, control silane concentration is 0.1g/ml, above-mentioned phosphatization iron powder is joined to 50 ℃ of mechanical agitation reaction 60min in treatment fluid, be placed on 120 ℃ with absolute ethyl alcohol filtration washing and be fully dried, make the double-deck cladded type ferro-silicium of phosphate layer and siloxane layer powder.
Embodiment 3
Raw material iron powder adopts carbonyl iron dust, controlling its concentration is 0.1g/ml, gets a certain amount of phosphoric acid and joins in acetone and be made into Phosphating Solution, and control phosphoric acid concentration is 0.002g/ml, iron powder is joined to 50 ℃ of mechanical agitation reaction 15min in Phosphating Solution, be placed on 50 ℃ for 3 times with acetone filtration washing and be fully dried.Get again in the mixed solution that a certain amount of 3-aminopropyl triethoxysilane joins absolute ethyl alcohol and 5% deionized water and be made into silane treatment liquid after hydrolysis, control silane concentration is 0.2g/ml, above-mentioned phosphatization iron powder is joined to 70 ℃ of mechanical agitation reaction 30min in treatment fluid, be placed on 100 ℃ with absolute ethyl alcohol filtration washing and be fully dried, make the double-deck cladded type carbonyl iron dust of phosphate layer and siloxane layer.
Embodiment 4
Raw material iron powder adopts reduced iron powder, controlling its concentration is 1g/ml, gets a certain amount of phosphoric acid and joins in acetone and be made into Phosphating Solution, and control phosphoric acid concentration is 0.02g/ml, iron powder is joined to room temperature mechanical stirring reaction 30min in Phosphating Solution, be placed on 50 ℃ for 3 times with acetone filtration washing and be fully dried.Get again in the mixed solution that a certain amount of 3-aminopropyl trimethoxysilane joins absolute ethyl alcohol and 5% deionized water and be made into silane treatment liquid after hydrolysis, control silane concentration is 0.01g/ml, above-mentioned phosphatization iron powder is joined to 40 ℃ of mechanical agitation reaction 90min in treatment fluid, be placed on 80 ℃ with absolute ethyl alcohol filtration washing and be fully dried, make phosphate layer and siloxane layer double-decker cladded type reduced iron powder.

Claims (5)

1. the coated processing method in iron powder surface, is characterized in that, processing step is as follows:
(1) preparation Phosphating Solution, phosphoric acid is solute, and absolute ethyl alcohol or acetone are solvent, and control solute concentration is 0.002~0.02g/ml;
(2) soft magnetic powder is joined in Phosphating Solution, control iron powder concentration is 0.1~2g/ml simultaneously, and controlling treatment fluid temperature is 20~50 ℃, mechanical agitation reaction 15~60min;
(3) filtration washing the dry phosphatizing powder that obtains;
(4) preparation silane treatment fluid, organosilan is solute, and the mixture of ethanol or ethylene glycol and deionized water is solvent, and control silane concentration is 0.01~0.2g/ml;
(5) phosphatizing powder is joined in silane treatment liquid, control iron powder concentration is 0.1~2g/ml simultaneously, and treatment fluid temperature is 20~70 ℃, and mechanical agitation is processed 30~120min;
(6) filtration washing, and be placed in 50~120 ℃ of fully dry superpacket whitings that obtain.
2. method according to claim 1, is characterized in that: in step (1), solute concentration is 0.005~0.01g/ml.
3. method according to claim 1, is characterized in that: the soft magnetic powder in step (2) is one or more in reduced iron powder, atomized iron powder, electrolytic iron powder, carbonyl iron dust or fe-based alloy powder; Iron powder concentration is 0.2~1g/ml.
4. method according to claim 1, is characterized in that: the organosilan in step (4) is the silane that contains methoxy or ethoxy alkoxyl.
The concentration of described raw material iron powder in Phosphating Solution and silane treatment liquid is 0.1~2g/ml.
5. method according to claim 1, is characterized in that: the treatment temperature in step (5) is 20~50 ℃, stir process 60~120min.
CN201410100487.0A 2014-03-18 2014-03-18 Iron powder surface coating processing method Pending CN103862033A (en)

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Cited By (11)

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Publication number Priority date Publication date Assignee Title
CN105161239A (en) * 2015-09-16 2015-12-16 广州齐达材料科技有限公司 Composite half-hard magnetic material and preparation method thereof
CN105400060A (en) * 2015-12-22 2016-03-16 深圳和畅电磁材料有限公司 Process for preparing flexible absorbing material
CN105502517A (en) * 2015-12-21 2016-04-20 中国科学院长春应用化学研究所 Modification method for electromagnetic parameters of carbonyl iron powder
CN105798291A (en) * 2016-05-30 2016-07-27 济南大学 Iron powder not easy to oxidize and oxidation resistant treatment method of iron powder
CN110014143A (en) * 2018-12-27 2019-07-16 江苏博迁新材料股份有限公司 The preparation method of copper phosphorus coated composite powder
DE112018001808T5 (en) 2017-11-29 2019-12-19 Grirem Advanced Materials Co., Ltd. Rare earth-bonded magnetic powder and manufacturing process therefor and bonded magnet
CN111354527A (en) * 2020-04-07 2020-06-30 浙江工业大学 High-strength glass phase-added silane-coated metal soft magnetic composite material and preparation method thereof
CN111354528A (en) * 2020-04-07 2020-06-30 浙江工业大学 Phosphoric acid-silane co-coated metal soft magnetic composite material and preparation method thereof
CN111377486A (en) * 2018-12-29 2020-07-07 洛阳尖端技术研究院 Preparation method of carbonyl powder
CN112475288A (en) * 2020-09-30 2021-03-12 东睦新材料集团股份有限公司 Preparation method of soft magnetic composite material for stator
CN113470916A (en) * 2021-07-05 2021-10-01 中国科学院宁波材料技术与工程研究所 Fe-Si-Al soft magnetic powder core and preparation method thereof

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105161239A (en) * 2015-09-16 2015-12-16 广州齐达材料科技有限公司 Composite half-hard magnetic material and preparation method thereof
CN105161239B (en) * 2015-09-16 2018-08-24 广州齐达材料科技有限公司 A kind of compound half-hard magnetic material and preparation method thereof
CN105502517A (en) * 2015-12-21 2016-04-20 中国科学院长春应用化学研究所 Modification method for electromagnetic parameters of carbonyl iron powder
CN105400060A (en) * 2015-12-22 2016-03-16 深圳和畅电磁材料有限公司 Process for preparing flexible absorbing material
CN105798291A (en) * 2016-05-30 2016-07-27 济南大学 Iron powder not easy to oxidize and oxidation resistant treatment method of iron powder
DE112018001808T5 (en) 2017-11-29 2019-12-19 Grirem Advanced Materials Co., Ltd. Rare earth-bonded magnetic powder and manufacturing process therefor and bonded magnet
CN110014143A (en) * 2018-12-27 2019-07-16 江苏博迁新材料股份有限公司 The preparation method of copper phosphorus coated composite powder
CN111377486A (en) * 2018-12-29 2020-07-07 洛阳尖端技术研究院 Preparation method of carbonyl powder
CN111354527A (en) * 2020-04-07 2020-06-30 浙江工业大学 High-strength glass phase-added silane-coated metal soft magnetic composite material and preparation method thereof
CN111354528A (en) * 2020-04-07 2020-06-30 浙江工业大学 Phosphoric acid-silane co-coated metal soft magnetic composite material and preparation method thereof
CN112475288A (en) * 2020-09-30 2021-03-12 东睦新材料集团股份有限公司 Preparation method of soft magnetic composite material for stator
CN112475288B (en) * 2020-09-30 2023-04-18 东睦新材料集团股份有限公司 Preparation method of soft magnetic composite material for stator
CN113470916A (en) * 2021-07-05 2021-10-01 中国科学院宁波材料技术与工程研究所 Fe-Si-Al soft magnetic powder core and preparation method thereof

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Application publication date: 20140618