CN105513739A - Method for preparing soft-magnetic composite material with core-shell structure by means of surfactant - Google Patents
Method for preparing soft-magnetic composite material with core-shell structure by means of surfactant Download PDFInfo
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- CN105513739A CN105513739A CN201510854721.3A CN201510854721A CN105513739A CN 105513739 A CN105513739 A CN 105513739A CN 201510854721 A CN201510854721 A CN 201510854721A CN 105513739 A CN105513739 A CN 105513739A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/36—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
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- Soft Magnetic Materials (AREA)
Abstract
The invention discloses a method for preparing a soft-magnetic composite material with a core-shell structure by means of a surfactant. Firstly, each 0.6 g of a soft-magnetic material body is dissolved in 100 mL of ethanol, then is stirred and cleaned, magnetic separation is carried out, black powder is obtained, then the black powder is added into 50 mL of distilled water, then 50 mL of ethanol and 0.5 mL of the surfactant are added into the distilled water and are stirred, and magnetic separation is carried out to the reaction product; each 0.6 g of the reaction product is added into 80 mL of alcoholic solution and is fully dispersed, then 15 mL of distilled water, 1 mL of ammonia water and 1 mL of tetraethyl orthosilicate are added, after the stirring process, the reaction product is cleaned sequentially through distilled water and ethanol, magnetic separation is carried out, then a black soft-magnetic composite material is obtained. According to the invention, soft-magnetic material body particles are completely coated, uniform insulating layers are formed, the electrical resistivity of the soft-magnetic composite material is improved, eddy-current loss is reduced, and therefore the high-frequency soft-magnetic performance is improved, and the preparation method is simple and moderate, and is low in energy consumption.
Description
Technical field
The invention relates to soft magnetic material, be specifically related to a kind ofly use the preparation of different surfaces activating agent to have excellent high frequency soft-magnetic composite material and preparation method thereof.
Background technology
Soft magnetic material (softmagneticmaterial) is a kind of magnetic material with low-coercivity and high magnetic permeability.Be widely used at electronic information communication, space flight and aviation, biomedicine field, be often made into absorbing material, inductance coil, drug targeting release and fluorescence detection material, catalyst etc.Along with the development of industry, under high frequency condition, the material of job applications more and more can not meet people's method demand.Wherein, soft magnetic metal simple substance and alloy thereof are because having the excellent soft magnetic characteristics such as higher magnetic permeability, higher saturation magnetization, less coercive force, studied person's extensive concern.But under high frequency condition, its conductivity causes too greatly huge eddy current loss, and these eddy current make magnetic core generate heat, while causing unnecessary energy dissipation, unnecessary security incident can be caused again.
At present, for the soft magnetic material of micron order Large stone, the industrial electric plating method of most employing, it is equivalent to carry out coated insulation layer to whole material block, and completely not coated for the single domain structure in soft magnetic material, and this method consumes mass energy, under high frequency condition, this still can make material produce huge eddy current loss, causes huge energy dissipation.Also studied by a large amount of researcher in the method for soft magnetic granules Surface coating one layer insulating, but due to micron-sized soft magnetic granules specific area little, be in the solution difficult to adsorption activity functional group, cause Surface coating Rotating fields uneven; And micron order soft magnetic granules density ratio is comparatively large, in the solution, this causes very large problem at particle surface coated insulation layer in very difficult suspension.
Summary of the invention
Object of the present invention, be to overcome that prior art energy resource consumption is excessive or coating layer structure is uneven or micron order soft magnetic granules is difficult to the defect that suspends in the solution, a kind of surfactant that utilizes is provided to prepare the method with nucleocapsid structure soft-magnetic composite material, it can carry out completely coated to particle, uniform coating layer is formed on its surface, thus improve high-frequency soft magnetic performance, and preparation method is simple, gentle, energy consumption is lower.
The invention provides one utilizes surfactant preparation to have nucleocapsid structure soft-magnetic composite material, by soft magnetic material body, and be coated on the insulating barrier composition of soft magnetic material body outer surface, its feature can be, this insulation layer structure is even, forms complete nucleocapsid structure;
Present invention also offers a kind of surfactant that utilizes and prepare the method with nucleocapsid structure soft-magnetic composite material, there are following steps:
(1) every 0.6g soft magnetic material body is dissolved in 100mL ethanol, stirring and washing, Magneto separate, the black powder obtained;
(2) black powder that step (1) obtains is joined in 50mL distilled water, then add 50mL ethanol, 0.5mL surfactant, stir 2 hours, by reacted product Magneto separate;
(3) take step (2) gained product, according to every 0.6g product, in following ratio, join in 80mL alcoholic solution and fully disperse, then add 15mL distilled water, 1mL ammoniacal liquor, 1mL tetraethyl orthosilicate, stir 6 hours; Cleaned with distilled water, ethanol successively by reacted product, pH value of solution=7 to distillation washing, Magneto separate, obtains black soft-magnetic composite material again.
Described soft magnetic material body is Ferrious material simple substance or Ferrious material alloy or soft magnetic ferrite.
The particle size of described soft magnetic material body is at 0.1 ~ 10 μm, and the thickness of described integument is at 2 ~ 50nm;
Surfactant in described step (2) be polyethylene glycol, oleic acid, natrium citricum, softex kw, dodecyl sodium sulfate, silane coupler one or more.
Alcoholic solution in described step (3) is methyl alcohol, ethanol, isopropyl alcohol, one or more and they of ethylene glycol and the mixed solution of distilled water arbitrary volume ratio.
Provided by the invention utilize surfactant prepare there is nucleocapsid structure soft-magnetic composite material, insulating barrier can carry out completely coated to particle, uniform coating layer is formed on its surface, form nucleocapsid structure, improve the resistivity of soft-magnetic composite material, reduce eddy current loss, thus improve high-frequency soft magnetic performance, and preparation method is simple, gentle, energy consumption is lower.
Accompanying drawing explanation
Fig. 1 is the TEM image with the soft-magnetic composite material of nucleocapsid structure that embodiment 1 obtains;
Fig. 2 is the TEM image with the soft-magnetic composite material of nucleocapsid structure that embodiment 4 obtains;
Fig. 3 is the infrared spectrogram of soft magnetism bulk product after the activation that in embodiment 1, step (2) obtains.
Embodiment
The invention provides a kind of method utilizing surfactant to prepare soft-magnetic composite material, soft magnetic material body is Ferrious material simple substance (embodiment 1), Ferrious material alloy (embodiment 4) or soft magnetic ferrite (embodiment 5).The grain size of soft magnetic material body can be micron order, also can be nanoscale, and its particle size, also can between 100nm ~ 200nm (Fig. 2) between 1 μm ~ 10 μm (Fig. 1).Thickness of insulating layer is between 2nm ~ 50nm.The surfactant used comprises silane coupler (KH550) (embodiment 1), oleic acid (embodiment 2) etc., for silane coupler (KH550), under the effect of this surfactant, can activate (as shown in Figure 3) the surface of soft magnetic material body, thus wrap up the uniform silicon oxide layer of one deck at soft magnetism body surface under TEOS hydrolytic polycondensation.For different alcoholic solutions, comprise absolute ethyl alcohol (embodiment 1), ethylene glycol (embodiment 3) etc., it can the growth rate of controlled oxidization silicon integument and uniformity.
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
(1) iron powder taking the about 1 μm of particle diameter of 0.6g is dissolved in the ethanol of 100mL, stirring and washing 2 times, Magneto separate;
(2) black powder that step (1) obtains is joined in 50mL distilled water, then add 50mL absolute ethyl alcohol, 0.5mL silane coupler (KH550), stir 2 hours, by reacted product Magneto separate;
(3) by 0.6g black powder that step (2) obtains, join in 80mL absolute ethyl alcohol, add 15mL distilled water, 1mL ammoniacal liquor, the tetraethyl orthosilicate (TEOS) of 1mL is dropwise added, mechanical agitation 6h, by reacted product successively with pH value of solution=7 after distilled water, ethanol purge to distillation washing in whipping process, Magneto separate, obtains black soft-magnetic composite material.
Embodiment 2
(1) iron powder taking the about 1 μm of particle diameter of 0.6g is dissolved in the ethanol of 100mL, stirring and washing 2 times, Magneto separate;
(2) black powder that step (1) obtains is joined in 50mL distilled water, then add 50mL absolute ethyl alcohol, the liquid oleic acid of 0.5mL, stir 2 hours, by reacted product Magneto separate;
(3) by 0.6g black powder that step (2) obtains, join in 80mL absolute ethyl alcohol, add 15mL distilled water again, 1mL ammoniacal liquor, the tetraethyl orthosilicate (TEOS) of 1mL is dropwise added, mechanical agitation 6h, by reacted product successively with pH value of solution=7 after distilled water, ethanol purge to distillation washing in whipping process, Magneto separate, obtains black soft-magnetic composite material.
Embodiment 3
(1) iron powder taking the about 1 μm of particle diameter of 0.6g is dissolved in the ethanol of 100mL, stirring and washing 2 times, Magneto separate;
(2) black powder that step (1) obtains is joined in 50mL distilled water, then add 50mL absolute ethyl alcohol, 0.5mL silane coupler (KH550), stir 2 hours, by reacted product Magneto separate;
(3) by 0.6g black powder that step (2) obtains, join in 80mL ethylene glycol, add 15mL distilled water, 1mL ammoniacal liquor, the tetraethyl orthosilicate (TEOS) of 1mL is dropwise added, mechanical agitation 6h, by reacted product successively with pH value of solution=7 after distilled water, ethanol purge to distillation washing in whipping process, Magneto separate, obtains black soft magnetism composite sample.
Embodiment 4
(1) iron-nickel alloy taking the about 100nm particle diameter of 0.6g is dissolved in the ethanol of 100mL, stirring and washing 2 times, Magneto separate;
(2) black powder that step (1) obtains is joined in 50mL distilled water, then add 50mL absolute ethyl alcohol, 0.5mL silane coupler (KH550), stir 2 hours, by reacted product Magneto separate;
(3) by 0.6g black powder that step (2) obtains, join in 80mL absolute ethyl alcohol, add 15mL distilled water, 1mL ammoniacal liquor, the tetraethyl orthosilicate (TEOS) of 1mL is dropwise added, mechanical agitation 6h, by reacted product successively with pH value of solution=7 after distilled water, ethanol purge to distillation washing in whipping process, Magneto separate, obtains black soft-magnetic composite material.
Embodiment 5
(1) ferrite taking the about 100nm particle diameter of 0.6g is dissolved in the ethanol of 100mL, stirring and washing 2 times, Magneto separate;
(2) black powder that step (1) obtains is joined in 50mL distilled water, then add 50mL absolute ethyl alcohol, 0.5mL silane coupler (KH550), stir 2 hours, by reacted product Magneto separate;
(3) by 0.6g black powder that step (2) obtains, join in 80mL absolute ethyl alcohol, add 15mL distilled water, 1mL ammoniacal liquor, the tetraethyl orthosilicate (TEOS) of 1mL is dropwise added, mechanical agitation 6h, by reacted product successively with pH value of solution=7 after distilled water, ethanol purge to distillation washing in whipping process, Magneto separate, obtains black soft-magnetic composite material.
All methods disclosed by the invention and technology of preparing, those skilled in the art are by using for reference present disclosure, the links such as appropriate change raw material and process route realize, although the present invention proposes various embodiments, but the alcoholic solution kind used in course of reaction and concentration proportioning can not limits, and the surfactant used can not enumerate.Person skilled in the art easily makes various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore of particular note, all similar replacements and change are all deemed to be included in spirit of the present invention, scope and content.
Claims (5)
1. utilize surfactant to prepare a soft-magnetic composite material with nucleocapsid structure, by soft magnetic material body, and be coated on the insulating barrier composition of soft magnetic material body outer surface, its feature can be, this insulation layer structure is even, forms complete nucleocapsid structure.
The preparation method of the soft-magnetic composite material of above-mentioned nucleocapsid structure, has following steps:
(1) every 0.6g soft magnetic material body is dissolved in 100mL ethanol, stirring and washing, Magneto separate, the black powder obtained;
(2) black powder that step (1) obtains is joined in 50mL distilled water, then add 50mL ethanol, 0.5mL surfactant, stir 2 hours, by product Magneto separate;
(3) take step (2) gained product, according to every 0.6g product, in following ratio, join in 80mL alcoholic solution and fully disperse, then add 15mL distilled water, 1mL ammoniacal liquor, 1mL tetraethyl orthosilicate, stir 6 hours; Product cleaned with distilled water, ethanol successively, pH value of solution=7 to distillation washing, Magneto separate, obtains black soft-magnetic composite material again.
2. one according to claim 1 utilizes surfactant to prepare to have nucleocapsid structure soft-magnetic composite material, it is characterized in that, described soft magnetic material body is Ferrious material simple substance or Ferrious material alloy or soft magnetic ferrite.
3. one according to claim 1 utilizes surfactant preparation to have nucleocapsid structure soft-magnetic composite material, and it is characterized in that, the particle size of described soft magnetic material body is at 0.1 ~ 10 μm, and the thickness of described integument is at 2 ~ 50nm.
4. one according to claim 1 utilizes surfactant preparation to have nucleocapsid structure soft-magnetic composite material, it is characterized in that, the surfactant in described step (2) be polyethylene glycol, oleic acid, natrium citricum, softex kw, dodecyl sodium sulfate, silane coupler one or more.
5. one according to claim 1 utilizes surfactant preparation to have nucleocapsid structure soft-magnetic composite material, it is characterized in that, the alcoholic solution in described step (3) is methyl alcohol, ethanol, isopropyl alcohol, one or more and they of ethylene glycol and the mixed solution of distilled water arbitrary volume ratio.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106024259A (en) * | 2016-05-31 | 2016-10-12 | 广州新莱福磁电有限公司 | Iron-based metal waterborne antirust magnetic paint and preparation method thereof |
| CN106835712A (en) * | 2017-02-28 | 2017-06-13 | 东华大学 | A kind of preparation method of ferrite/polyaniline Electromagnetically shielding fabrics |
| CN107578873A (en) * | 2017-09-12 | 2018-01-12 | 横店集团东磁股份有限公司 | A kind of preparation method of the iron nickel molybdenum powder core of magnetic permeability μ=400 |
| CN108597711A (en) * | 2018-04-17 | 2018-09-28 | 浙江工业大学 | A kind of method of soft magnetic metal powder surface in-stiu coating alundum (Al2O3) insulating layer |
| CN109216006A (en) * | 2018-08-29 | 2019-01-15 | 深圳顺络电子股份有限公司 | soft magnetic alloy powder core and preparation method thereof |
| CN110610788A (en) * | 2018-06-15 | 2019-12-24 | 山东精创磁电产业技术研究院有限公司 | Method for preparing soft magnetic composite material with core-shell structure |
| CN111883328A (en) * | 2020-06-09 | 2020-11-03 | 山东精创磁电产业技术研究院有限公司 | Modified binder and method for preparing soft magnetic composite material by using same |
| CN113488330A (en) * | 2021-07-15 | 2021-10-08 | 无锡蓝沛新材料科技股份有限公司 | Preparation method of functional magnetic slurry and magnetic device |
| CN116666101A (en) * | 2023-07-24 | 2023-08-29 | 通友微电(四川)有限公司 | Preparation method of organic coated soft magnetic powder |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106024259A (en) * | 2016-05-31 | 2016-10-12 | 广州新莱福磁电有限公司 | Iron-based metal waterborne antirust magnetic paint and preparation method thereof |
| CN106835712A (en) * | 2017-02-28 | 2017-06-13 | 东华大学 | A kind of preparation method of ferrite/polyaniline Electromagnetically shielding fabrics |
| CN107578873B (en) * | 2017-09-12 | 2019-03-08 | 横店集团东磁股份有限公司 | A kind of preparation method of the iron nickel molybdenum powder core of magnetic permeability μ=400 |
| CN107578873A (en) * | 2017-09-12 | 2018-01-12 | 横店集团东磁股份有限公司 | A kind of preparation method of the iron nickel molybdenum powder core of magnetic permeability μ=400 |
| CN108597711B (en) * | 2018-04-17 | 2019-11-19 | 浙江工业大学 | A kind of method of soft magnetic metal powder surface in-stiu coating aluminum oxide insulating layer |
| CN108597711A (en) * | 2018-04-17 | 2018-09-28 | 浙江工业大学 | A kind of method of soft magnetic metal powder surface in-stiu coating alundum (Al2O3) insulating layer |
| CN110610788A (en) * | 2018-06-15 | 2019-12-24 | 山东精创磁电产业技术研究院有限公司 | Method for preparing soft magnetic composite material with core-shell structure |
| CN110610788B (en) * | 2018-06-15 | 2021-09-28 | 山东精创磁电产业技术研究院有限公司 | Method for preparing soft magnetic composite material with core-shell structure |
| CN109216006A (en) * | 2018-08-29 | 2019-01-15 | 深圳顺络电子股份有限公司 | soft magnetic alloy powder core 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 |
| CN111883328A (en) * | 2020-06-09 | 2020-11-03 | 山东精创磁电产业技术研究院有限公司 | Modified binder and method for preparing soft magnetic composite material by using same |
| CN111883328B (en) * | 2020-06-09 | 2021-06-18 | 山东精创磁电产业技术研究院有限公司 | Modified binder and method for preparing soft magnetic composite material by using same |
| CN113488330A (en) * | 2021-07-15 | 2021-10-08 | 无锡蓝沛新材料科技股份有限公司 | Preparation method of functional magnetic slurry and magnetic device |
| CN116666101A (en) * | 2023-07-24 | 2023-08-29 | 通友微电(四川)有限公司 | Preparation method of organic coated soft magnetic powder |
| CN116666101B (en) * | 2023-07-24 | 2024-03-08 | 通友微电(四川)有限公司 | Preparation method of organic coated soft magnetic powder |
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Application publication date: 20160420 |