CN110819971A - Based on SiO2Preparation method of coated carbonyl iron powder composite wave-absorbing material - Google Patents
Based on SiO2Preparation method of coated carbonyl iron powder composite wave-absorbing material Download PDFInfo
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- CN110819971A CN110819971A CN201911124691.5A CN201911124691A CN110819971A CN 110819971 A CN110819971 A CN 110819971A CN 201911124691 A CN201911124691 A CN 201911124691A CN 110819971 A CN110819971 A CN 110819971A
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- iron powder
- carbonyl iron
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1212—Zeolites, glasses
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
Abstract
The invention provides a SiO-based material2The preparation method of the coated carbonyl iron powder composite wave-absorbing material comprises the steps of S1, adding carbonyl iron powder into deionized water to form a mixture, wherein the mass percent of the carbonyl iron powder is 1-5%, and performing ultrasonic treatment on the mixture for 1-2 min to obtain a system A; s2, adding tetraethoxysilane and a silane coupling agent into absolute ethyl alcohol to form a mixture, wherein the mass percentage of tetraethoxysilane and silane coupling agent is 0.5% -2%, and obtaining a system B; s3, mixing the two systems, adding a catalyst for promoting hydrolysis of ethyl orthosilicate to form a mixed solution, wherein the mass percentage of the catalyst is 0.2% -1%, heating the mixed solution in a constant-temperature water bath for 2-4 hours under stirring of a magnetic stirrer, and the temperature of the water bath is 40-60 ℃; s4, pouring out supernatant in the mixed solution, washing the lower precipitate with deionized water for many times, and continuously using magnetismMagnetically enriching carbonyl iron powder by using a sexual stirring bar; s5, drying the product obtained in the step S4 in vacuum at the temperature of 50-70 ℃ for 18-24 hours, and grinding for 4-6 min. The wave-absorbing material prepared by the method has excellent wave-absorbing performance.
Description
Technical Field
The invention relates to the technical field of wave-absorbing material preparation, in particular to a microwave absorbing material based on SiO2A preparation method of a coated carbonyl iron powder composite wave-absorbing material.
Background
With the continuous progress of science and technology, the application technology of electromagnetic waves is continuously developed, but the technology brings about a lot of convenience and brings about a lot of electromagnetic wave pollution, which brings about a lot of adverse effects to the life and work of people, for example, some precision equipment may operate abnormally. Therefore, research and development and application of the wave-absorbing material become the focus of attention of people (especially scientific research personnel).
The carbonyl iron powder has the characteristics of good temperature stability, high magnetic conductivity and low production cost, has wide application prospect in the wave-absorbing material, and is the magnetic electromagnetic wave absorbent which is most deeply researched, most widely applied and excellent in wave-absorbing performance at home and abroad. However, the application of carbonyl iron powder is limited by the self defects of magnetic particles such as high surface density, poor chemical stability, easy agglomeration and the like. Therefore, the modification or compounding of the carbonyl iron powder is very important, and becomes one of the research hotspots at home and abroad.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a SiO-based material2The preparation method of the coated carbonyl iron powder composite wave-absorbing material is convenient for ensuring that the carbonyl iron powder has better impedance matching and corrosion resistance on the premise of ensuring the original wave-absorbing performance.
In order to achieve the purpose, the invention provides a SiO-based material2The preparation method of the coated carbonyl iron powder composite wave-absorbing material comprises the following steps:
step 1, adding carbonyl iron powder into deionized water to form a mixture, wherein the mass percent of the carbonyl iron powder in the mixture is 1% -5%, and carrying out ultrasonic treatment on the mixture for 1-2 min to obtain a system A;
step 3, mixing the system A and the system B, adding a catalyst for promoting hydrolysis of ethyl orthosilicate to form a mixed solution, wherein the mass percentage of the catalyst in the mixed solution is 0.2-1%, and heating the mixed solution in a constant-temperature water bath for 2-4 h under the condition of stirring by a magnetic stirrer, wherein the temperature of the water bath is 40-60 ℃;
step 5, drying the product obtained in the step 4 in vacuum for 18-24 h at the temperature of 50-70 ℃, and then grinding for 4-6 min to obtain the product based on SiO2The coated carbonyl iron powder composite wave-absorbing material.
Preferably, in the step 2, kh550 is used as the silane coupling agent.
Preferably, in the step 3, L-lysine is used as the catalyst.
Preferably, in the step 3, the water bath heating is a constant temperature water bath kettle.
Preferably, in the step 5, an oven is used for drying, and a mortar is used for grinding.
The scheme of the invention has the beneficial effect that the SiO-based material is prepared by the method2Carbonyl iron powder surface prepared by preparation method of coated carbonyl iron powder composite wave-absorbing material has a layer of SiO2Thus, the impedance matching of the carbonyl iron powder is improved, and the wave absorbing performance and the corrosion resistance of the carbonyl iron powder are enhanced. The invention adopts a sol-gel method to make SiO2The preparation method is formed on the surface of carbonyl iron powder, the preparation process is simple, the operability is strong, and the potential of large-scale mass production is realized.
Drawings
FIG. 1 shows SiO2XRD patterns of carbonyl iron powder before and after coating, wherein Sample A is SiO2XRD pattern of coated original carbonyl iron powder, Sample C is SiO2XRD pattern of the coated carbonyl iron powder composite wave-absorbing material.
FIG. 2 shows a SiO coated glass2Scanning electron microscope atlas of the coated original carbonyl iron powder, wherein (a) is low power picture and (b) is high power picture.
FIG. 3 shows SiO2Scanning electron microscope atlas of the coated carbonyl iron powder composite wave-absorbing material, wherein (a) is a low-power image and (b) is a high-power image.
FIG. 4 is SiO coated2The transmission spectrum of the coated carbonyl iron powder composite wave-absorbing material, wherein (a) is SiO on the surface of the carbonyl iron powder2A selected area electron diffraction pattern of the layer (b) is SiO2And (3) a selected area electron diffraction pattern of the coated carbonyl iron powder composite wave-absorbing material.
FIG. 5 is SiO coated2An EDX atlas is used for elemental analysis of the coated carbonyl iron powder composite wave-absorbing material, wherein a scanning path is a straight line in the atlas.
FIG. 6 is a SiO coated glass2The impedance of the coated original carbonyl iron powder is matched and the reflection and absorption rate of the coated original carbonyl iron powder at different thicknesses, wherein (a) is an impedance matching curve diagram, and (b) is a reflection and absorption rate curve diagram at different thicknesses.
FIG. 7 is a SiO coating2The impedance of the coated carbonyl iron powder composite wave-absorbing material is matched and the reflection and absorption rate of the coated carbonyl iron powder composite wave-absorbing material in different thicknesses are matched, wherein (a) is an impedance matching curve diagram, and (b) is a reflection and absorption rate curve diagram in different thicknesses.
Detailed Description
The following further describes embodiments of the present invention with reference to the drawings.
The invention relates to a SiO-based2The preparation method of the coated carbonyl iron powder composite wave-absorbing material comprises the following steps:
step 1, adding carbonyl iron powder into deionized water to form a mixture, wherein the mass percent of the carbonyl iron powder in the mixture is 1% -5%, and carrying out ultrasonic treatment on the mixture for 1-2 min to obtain a system A.
The surfaces of metals and metal oxides are distributed throughout hydroxyl groups in water due to the action of water molecules, so that carbonyl iron powder is put into deionized water for treatment for a period of time, and stirring and ultrasound are both used for accelerating the process.
And 2, respectively adding tetraethoxysilane and a silane coupling agent into absolute ethyl alcohol to form a mixture, wherein the mass percent of tetraethoxysilane in the mixture is 0.5-2%, and the mass percent of the silane coupling agent is 0.5-2%, so as to obtain a system B. In this embodiment, kh550 is selected as the silane coupling agent.
The ethyl orthosilicate contains rich silicon-oxygen bonds, and can generate SiO by hydrolysis2Sufficient silicon source can be provided for the subsequent coating process. One end of the silane coupling agent kh550 can be adsorbed on the surface of carbonyl iron powder through coulomb force due to molecular polarity, and the other end is of a siloxane structure similar to tetraethoxysilane and can be connected with tetraethoxysilane
And 3, mixing the system A and the system B, adding a catalyst for promoting hydrolysis of the tetraethoxysilane to form a mixed solution, wherein the mass percent of the catalyst in the mixed solution is 0.2-1%, and heating the mixed solution in a constant-temperature water bath for 2-4 h under the condition of stirring by a magnetic stirrer, wherein the water bath temperature is 40-60 ℃. In this embodiment, the catalyst is L-lysine, and the L-lysine can not only maintain the catalytic action of promoting the hydrolysis of silicon-oxygen bonds, but also avoid the corrosion of ammonia water to metals, and even influence SiO2In an ordered arrangement. The water bath heating adopts a constant temperature water bath kettle.
And 4, pouring out supernatant in the mixed solution, washing the lower precipitate for multiple times by using deionized water, and continuously utilizing the magnetism of the magnetic stirrer to enrich carbonyl iron powder.
The magnetic stirrer can play a role in stirring in the previous water bath heating process and can also play a role in enriching in the water washing process, and most of carbonyl iron powder can be adsorbed on the surface of the carbonyl iron powder, so that the water washing process is greatly simplified.
Step 5, drying the product obtained in the step 4 in vacuum for 18 h-2 h at the temperature of 50-70 DEG CGrinding for 4-6 min for 4h to obtain the product based on SiO2The coated carbonyl iron powder composite wave-absorbing material. Wherein the drying adopts an oven, and the grinding adopts a mortar.
Based on SiO that the invention relates to2SiO obtained by preparation method of coated carbonyl iron powder composite wave-absorbing material2The coated carbonyl iron powder composite wave-absorbing material is flocculent SiO2The (silicon dioxide) is uniformly distributed on the surface of the carbonyl iron powder and SiO2When the thickness of the coated carbonyl iron powder composite wave-absorbing material is 2.55mm, the reflection attenuation value of the coated carbonyl iron powder composite wave-absorbing material is-49.39 dB, which is close to-50 dB, the maximum absorption bandwidth reaches 7.12GHz, the electromagnetic wave absorption rate reaches 99.99%, and the wave-absorbing performance is excellent.
By the above-mentioned SiO-based2Carbonyl iron powder surface prepared by preparation method of coated carbonyl iron powder composite wave-absorbing material has a layer of SiO2Thus, the impedance matching of the carbonyl iron powder is improved, and the wave absorbing performance and the corrosion resistance of the carbonyl iron powder are enhanced. The invention adopts a sol-gel method to make SiO2The preparation method is formed on the surface of carbonyl iron powder, the preparation process is simple, the operability is strong, and the potential of large-scale mass production is realized.
Claims (5)
1. Based on SiO2The preparation method of the coated carbonyl iron powder composite wave-absorbing material is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding carbonyl iron powder into deionized water to form a mixture, wherein the mass percent of the carbonyl iron powder in the mixture is 1% -5%, and carrying out ultrasonic treatment on the mixture for 1-2 min to obtain a system A;
step 2, respectively adding tetraethoxysilane and a silane coupling agent into absolute ethyl alcohol to form a mixture, wherein the mass percent of tetraethoxysilane in the mixture is 0.5-2%, and the mass percent of the silane coupling agent is 0.5-2%, so as to obtain a system B;
step 3, mixing the system A and the system B, adding a catalyst for promoting hydrolysis of ethyl orthosilicate to form a mixed solution, wherein the mass percentage of the catalyst in the mixed solution is 0.2-1%, and heating the mixed solution in a constant-temperature water bath for 2-4 h under the condition of stirring by a magnetic stirrer, wherein the temperature of the water bath is 40-60 ℃;
step 4, pouring out supernatant liquor in the mixed liquor, washing the lower-layer precipitate for multiple times by using deionized water, and continuously utilizing the magnetism of the magnetic stirrer to enrich carbonyl iron powder;
step 5, drying the product obtained in the step 4 in vacuum for 18-24 h at the temperature of 50-70 ℃, and then grinding for 4-6 min to obtain the product based on SiO2The coated carbonyl iron powder composite wave-absorbing material.
2. SiO-based according to claim 12The preparation method of the coated carbonyl iron powder composite wave-absorbing material is characterized by comprising the following steps: in the step 2, kh550 is adopted as the silane coupling agent.
3. SiO-based according to claim 1 or 22The preparation method of the coated carbonyl iron powder composite wave-absorbing material is characterized by comprising the following steps: in the step 3, L-lysine is used as the catalyst.
4. SiO-based according to claim 32The preparation method of the coated carbonyl iron powder composite wave-absorbing material is characterized by comprising the following steps: in the step 3, the water bath heating adopts a constant-temperature water bath kettle.
5. SiO-based according to claim 12The preparation method of the coated carbonyl iron powder composite wave-absorbing material is characterized by comprising the following steps: in the step 5, an oven is used for drying, and a mortar is used for grinding.
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Cited By (11)
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| CN112029480A (en) * | 2020-08-24 | 2020-12-04 | 电子科技大学 | Organic-inorganic composite coated metal wave-absorbing filler and preparation method thereof |
| CN112374547A (en) * | 2020-11-13 | 2021-02-19 | 航天特种材料及工艺技术研究所 | Carbonyl iron powder composite wave-absorbing material and preparation method thereof |
| CN113352706A (en) * | 2021-06-15 | 2021-09-07 | 武汉中科先进技术研究院有限公司 | Basalt fiber structural wave-absorbing composite material and preparation method thereof |
| CN113402920A (en) * | 2021-06-16 | 2021-09-17 | 电子科技大学 | Preparation method of FeSiAl-based organic-inorganic double-layer core-shell structure |
| CN113416504A (en) * | 2021-08-13 | 2021-09-21 | 广州市方佳崇医疗科技有限公司 | Medical hot-melt adhesive and preparation method thereof |
| CN114082943A (en) * | 2021-11-23 | 2022-02-25 | 成都佳驰电子科技股份有限公司 | Method for coating carbonyl iron powder with silicon dioxide in ethanol-free system |
| CN114350156A (en) * | 2022-01-13 | 2022-04-15 | 傲川科技(河源)有限公司 | High-temperature-resistant heat-conducting wave-absorbing composite material and preparation method thereof |
| CN114644795A (en) * | 2020-12-17 | 2022-06-21 | 洛阳尖端技术研究院 | Wave-absorbing material and preparation method and application thereof |
| CN114771045A (en) * | 2022-05-18 | 2022-07-22 | 成都三洪高科科技有限公司 | Wave-absorbing composite carbon fiber plate |
| CN114932734A (en) * | 2022-06-06 | 2022-08-23 | 广东国科电磁防护科技有限公司 | Electromagnetic shielding multilayer composite film and processing technology thereof |
| CN116200120A (en) * | 2023-03-14 | 2023-06-02 | 东莞市雷兹盾电子材料有限公司 | Composite wave-absorbing sizing material and preparation method thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112029480B (en) * | 2020-08-24 | 2021-09-24 | 电子科技大学 | Organic-inorganic composite coated metal wave-absorbing filler and preparation method thereof |
| CN112029480A (en) * | 2020-08-24 | 2020-12-04 | 电子科技大学 | Organic-inorganic composite coated metal wave-absorbing filler and preparation method thereof |
| CN112374547A (en) * | 2020-11-13 | 2021-02-19 | 航天特种材料及工艺技术研究所 | Carbonyl iron powder composite wave-absorbing material and preparation method thereof |
| CN114644795A (en) * | 2020-12-17 | 2022-06-21 | 洛阳尖端技术研究院 | Wave-absorbing material and preparation method and application thereof |
| CN113352706A (en) * | 2021-06-15 | 2021-09-07 | 武汉中科先进技术研究院有限公司 | Basalt fiber structural wave-absorbing composite material and preparation method thereof |
| CN113402920A (en) * | 2021-06-16 | 2021-09-17 | 电子科技大学 | Preparation method of FeSiAl-based organic-inorganic double-layer core-shell structure |
| CN113402920B (en) * | 2021-06-16 | 2022-05-03 | 电子科技大学 | Preparation method of FeSiAl-based organic-inorganic double-layer core-shell structure |
| CN113416504A (en) * | 2021-08-13 | 2021-09-21 | 广州市方佳崇医疗科技有限公司 | Medical hot-melt adhesive and preparation method thereof |
| CN114082943A (en) * | 2021-11-23 | 2022-02-25 | 成都佳驰电子科技股份有限公司 | Method for coating carbonyl iron powder with silicon dioxide in ethanol-free system |
| CN114082943B (en) * | 2021-11-23 | 2024-01-05 | 成都佳驰电子科技股份有限公司 | Method for coating carbonyl iron powder with silicon dioxide in ethanol-free system |
| CN114350156A (en) * | 2022-01-13 | 2022-04-15 | 傲川科技(河源)有限公司 | High-temperature-resistant heat-conducting wave-absorbing composite material and preparation method thereof |
| CN114771045A (en) * | 2022-05-18 | 2022-07-22 | 成都三洪高科科技有限公司 | Wave-absorbing composite carbon fiber plate |
| CN114932734A (en) * | 2022-06-06 | 2022-08-23 | 广东国科电磁防护科技有限公司 | Electromagnetic shielding multilayer composite film and processing technology thereof |
| CN114932734B (en) * | 2022-06-06 | 2022-11-18 | 广东国科电磁防护科技有限公司 | Electromagnetic shielding multilayer composite film and processing technology thereof |
| CN116200120A (en) * | 2023-03-14 | 2023-06-02 | 东莞市雷兹盾电子材料有限公司 | Composite wave-absorbing sizing material and preparation method thereof |
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