CN115976880A - High-temperature-resistant antioxidant electromagnetic film and preparation method thereof - Google Patents

High-temperature-resistant antioxidant electromagnetic film and preparation method thereof Download PDF

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Publication number
CN115976880A
CN115976880A CN202211664943.5A CN202211664943A CN115976880A CN 115976880 A CN115976880 A CN 115976880A CN 202211664943 A CN202211664943 A CN 202211664943A CN 115976880 A CN115976880 A CN 115976880A
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chopped
temperature
fibers
carbon fibers
resistant
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林海燕
刘大伟
赵宏杰
吕通
刘甲
李旻
刘冉
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Aerospace Research Institute of Materials and Processing Technology
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Aerospace Research Institute of Materials and Processing Technology
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Abstract

The invention discloses a high-temperature-resistant antioxidant electromagnetic film and a preparation method thereof, and belongs to the technical field of functional materials. The high-temperature-resistant antioxidant electromagnetic film takes the chopped carbon fibers coated by the high-temperature-resistant coating and the low-dielectric chopped fibers as raw materials, the two raw materials are uniformly mixed by adopting a wet papermaking technology, and the mixture is dried to form the film. In the preparation process, the high-temperature resistant electromagnetic film with different dielectric properties can be obtained by adjusting the proportion of the chopped carbon fibers and the low-dielectric chopped fibers. The invention effectively improves the oxidation resistance of the electromagnetic film of the carbon fiber as the electrical loss absorbent, and greatly improves the high temperature resistance of the carbon fiber conductive absorbent.

Description

High-temperature-resistant antioxidant electromagnetic film and preparation method thereof
Technical Field
The invention discloses a high-temperature-resistant antioxidant electromagnetic film and a preparation method thereof, and belongs to the technical field of functional materials.
Background
The high-temperature wave-absorbing material has high temperature resistance and electromagnetic wave absorption functions, so that the high-temperature wave-absorbing material has important application value in the field of new generation military equipment, and is widely concerned. The traditional high-temperature wave-absorbing material is prepared by selecting a high-temperature-resistant absorbent and a ceramic or glass matrix through a certain composite process. The current research mainly focuses on adjusting physical and chemical properties such as electromagnetic parameters, mixing performance and the like of the high-temperature absorbent through doping, modification, shape regulation and control of the high-temperature absorbent and distribution state in a matrix so as to achieve the purposes of adjusting equivalent electromagnetic matching performance, mechanical property, high-temperature resistance and the like of the high-temperature absorbing material. The electromagnetic film is a technical approach for adjusting the electromagnetic parameters of the absorbent by dispersing the absorbent in the matrix and then adjusting the distribution state of the absorbent in the matrix. The carbon fiber has high strength, high modulus and good conductive property, is a key fiber with both reinforcing property and electromagnetic loss property commonly used in structural wave-absorbing materials, and plays an important role in structural stealth materials. The chopped carbon fiber wave-absorbing electromagnetic film obtained by mixing the chopped carbon fibers and the low-dielectric chopped fibers plays an important role in the preparation of the structural wave-absorbing material.
With the development of the new generation of high-speed aircraft, equipment also puts higher requirements on the temperature resistance of materials. For example, in the flying process of the supersonic cruise aircraft, the thermal equilibrium temperature of the outer surface of the structure reaches over 600 ℃ due to pneumatic heating. Test data show that the oxidation rate of the carbon fiber is obviously increased at about 500 ℃, the oxidation resistance is sharply reduced, the weight loss rate is as high as more than 50 percent, and the application of materials and components is seriously influenced. Thereby also causing the short carbon fiber wave-absorbing electromagnetic film obtained by doping the low-dielectric short carbon fibers with the short carbon fibers to lose the effect. Therefore, the oxidation resistance of the chopped carbon fiber doped low-dielectric chopped fiber wave-absorbing electromagnetic film must be improved, and a technical support is provided for the development of high-temperature wave-absorbing structural materials.
In the prior art for preparing hybrid chopped carbon fiber electromagnetic films, patent document CN102206371A provides a technical scheme that chopped carbon fibers are mixed with reclaimed rubber, and then the mixture is uniformly mixed on an open mill and an internal mixer and pressed into sheets to obtain the product. Because low-dielectric chopped fibers are not added in the technology, and only chopped carbon fibers with strong conductivity are added, the prepared rubber-based high-reflection electromagnetic shielding film has the main function of serving as a reflection layer of a structural wave-absorbing material, has large thickness (0.5-15 mm) and temperature resistance of less than 300 ℃, and cannot meet the requirement of more than 600 ℃ required by the technical background.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant and oxidation-resistant electromagnetic film and a preparation method thereof, and the prepared product effectively improves the oxidation resistance of the wave-absorbing film and realizes the high-temperature strong absorption function of the material while keeping the good performance of the wave-absorbing electromagnetic film obtained by mixing short carbon fibers with low-dielectric short fibers as an absorbent. In the technical scheme, the high-temperature oxidation-resistant coating is coated with the modified chopped carbon fibers and the low-dielectric chopped fibers as raw materials, and the wave-absorbing electromagnetic film obtained by mixing the high-temperature-resistant chopped carbon fibers with the low-dielectric chopped fibers is prepared by adopting a papermaking process.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a high-temperature-resistant antioxidant electromagnetic film comprises the following steps:
1) Selecting chopped carbon fibers coated by a high-temperature-resistant coating, wherein the high-temperature-resistant coating comprises one or more of a silicon carbide coating, a silicon dioxide coating and a zirconium oxide coating; selecting low-dielectric chopped fibers, wherein the low-dielectric chopped fibers comprise one or more of glass chopped fibers, quartz chopped fibers and alumina chopped fibers;
2) Mixing the chopped carbon fiber coated by the high-temperature-resistant coating and the low-dielectric chopped fiber selected in the step 1), adding water and a dispersing agent, and uniformly mixing;
3) Manufacturing the mixed fiber obtained in the step 2) into a fiber web by adopting a papermaking process;
4) Gluing the fiber web obtained in the step 3);
5) Placing the fiber net film coated with the glue solution obtained in the step 4) on a press for pressurizing, and pressing out redundant glue solution;
6) And taking the fiber net film out of the press, and drying the glue solution to obtain the high-temperature-resistant antioxidant electromagnetic film.
Furthermore, the chopped carbon fibers are one or more of chopped T300 carbon fibers, chopped T700 carbon fibers, chopped T800 carbon fibers, chopped T1000 carbon fibers, chopped M300J carbon fibers and chopped M550J carbon fibers.
Further, when the two fibers are mixed in the step 2), the mass ratio of the chopped carbon fibers coated by the high-temperature resistant coating is 0.05% -15%.
Furthermore, the mass of the water in the step 2) is 15-35 times of that of the mixture of the two fibers, and the dispersing agent is 0.018-0.06% of the mass of the water.
Further, the glue coated in the step 4) is one of epoxy resin glue, bismaleimide resin glue, polyimide glue and polyvinyl alcohol.
Further, the drying temperature in the step 6) is 105 +/-5 ℃, and the drying time is 5-10 minutes.
A high temperature resistant antioxidant electromagnetic film is prepared by the preparation method.
The invention provides a high-temperature-resistant antioxidant electromagnetic film, which is prepared by adopting high-temperature-resistant coating-coated chopped carbon fibers and low-dielectric chopped fibers as raw materials and adopting a wet papermaking technology. Because the chopped carbon fibers are mixed with the chopped fibers with low dielectric constant, the electrical conductivity of the composite material film is reduced, the composite material film becomes a dielectric film, and the main function of the product is changed into a loss layer serving as a structural wave-absorbing material. Then, a series of electromagnetic films with different dielectric properties are obtained by adjusting the proportion of the two materials, and the possibility is provided for the broadband design of the wave-absorbing material. The prepared product has the advantages of thin thickness (0.1-0.3 mm), adjustable dielectric property, good oxidation resistance and the like. The material can effectively improve the oxidation resistance of the carbon fiber while keeping the good dielectric property of the carbon fiber as an absorbent. The temperature resistance is higher than 600 ℃, and the requirement of more than 600 ℃ required by the background of the technology is met. Provides powerful technical support for the technical development of the high-temperature wave-absorbing material, and the material has wide application prospect in the fields of national defense industry, aviation, aerospace and the like.
Drawings
FIG. 1 is a schematic structural diagram of a high temperature resistant and oxidation resistant electromagnetic film according to the present invention.
FIG. 2 is a photograph of a sample of the high temperature and oxidation resistant electromagnetic film prepared in example 1.
Detailed Description
In order to make the aforementioned and other features and advantages of the invention more comprehensible, embodiments accompanied with figures are described in detail below.
Example 1
Step 1: weighing 0.03g of silicon carbide-coated chopped T300 carbon fibers and 59.9g of glass fibers;
step 2: adding 1kg of water and 0.18g of dispersant methyl acrylate into the mixture of the two fibers, and uniformly mixing;
and step 3: filtering the liquid of the mixed slurry, and forming a net by using the mixed fibers by adopting a papermaking process;
and 4, step 4: weighing 18g of adhesive PVA, and uniformly coating the adhesive PVA on the obtained mixed fiber forming net;
and 5: putting the obtained film coated with the glue solution on a press, pressurizing, and pressing out redundant glue solution;
step 6: and (3) heating the flat press to 110 ℃, preserving the heat for 5 minutes, and drying the glue solution to obtain the high-temperature-resistant antioxidant electromagnetic film.
And (3) product performance testing: the oxidation temperature of the prepared high-temperature-resistant oxidation-resistant electromagnetic film is increased from original 480 ℃ to 570 ℃ through testing as shown in figure 2.
Example 2
Step 1: the silicon carbide-coated chopped T300 carbon fibers (14.05 g) and the glass fibers (79.6 g) were weighed.
Step 2: 2kg of water and 0.8g of dispersant methyl acrylate are added into the mixture of the two fibers and evenly mixed.
And step 3: filtering the liquid of the mixed slurry, and forming a net by using the mixed fibers by adopting a papermaking process;
and 4, step 4: weighing 3.2g of adhesive PVA, and uniformly coating the adhesive PVA on the obtained mixed fiber web;
and 5: putting the obtained film coated with the glue solution on a press, pressurizing, and pressing out redundant glue solution;
step 6: and (3) raising the temperature of the flat press to 105 ℃, preserving the heat for 8 minutes, and drying the glue solution to obtain the high-temperature-resistant antioxidant electromagnetic film.
And (3) product performance testing: the oxidation temperature of the prepared high-temperature-resistant and oxidation-resistant electromagnetic film is increased from 480 ℃ to 575 ℃.
Example 3
Step 1: silicon carbide-coated chopped T300 carbon fibers (0.9 g) and glass fibers (149.1 g) were weighed.
Step 2: 5kg of water and 3g of dispersant methyl acrylate are added into the mixture of the two fibers and evenly mixed.
And step 3: filtering the liquid of the mixed slurry, and forming a net by using the mixed fibers by adopting a papermaking process;
and 4, step 4: weighing 4.5g of adhesive PVA, and uniformly coating the adhesive PVA on the obtained mixed fiber web;
and 5: putting the obtained film coated with the glue solution on a press, pressurizing, and pressing out redundant glue solution;
step 6: and (3) heating the flat press to 100 ℃, preserving the heat for 10 minutes, and drying the glue solution to obtain the high-temperature-resistant antioxidant electromagnetic film.
And (3) product performance testing: the oxidation temperature of the prepared high-temperature-resistant and antioxidant electromagnetic film is increased to 580 ℃ from the original 480 ℃.
Although the present invention has been described with reference to the above embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (7)

1. The preparation method of the high-temperature-resistant antioxidant electromagnetic film is characterized by comprising the following steps of:
1) Selecting chopped carbon fibers coated by a high-temperature-resistant coating, wherein the high-temperature-resistant coating comprises one or more of a silicon carbide coating, a silicon dioxide coating and a zirconium oxide coating; selecting low-dielectric chopped fibers, wherein the low-dielectric chopped fibers comprise one or more of glass chopped fibers, quartz chopped fibers and alumina chopped fibers;
2) Mixing the chopped carbon fiber coated by the high-temperature-resistant coating and the low-dielectric chopped fiber selected in the step 1), adding water and a dispersing agent, and uniformly mixing;
3) Manufacturing the mixed fiber obtained in the step 2) into a fiber web by adopting a papermaking process;
4) Gluing the fiber web obtained in the step 3);
5) Placing the fiber net film coated with the glue solution obtained in the step 4) on a press for pressurizing, and pressing out redundant glue solution;
6) And taking the fiber net film out of the press, and drying the glue solution to obtain the high-temperature-resistant antioxidant electromagnetic film.
2. The preparation method according to claim 1, wherein the chopped carbon fibers are one or more of chopped T300 carbon fibers, chopped T700 carbon fibers, chopped T800 carbon fibers, chopped T1000 carbon fibers, chopped M300J carbon fibers and chopped M550J carbon fibers.
3. The preparation method according to claim 1, wherein the chopped carbon fibers coated with the high-temperature-resistant coating are 0.05 to 15% by mass when the two fibers are mixed in the step 2).
4. The production method according to claim 1, wherein the mass of the water in the step 2) is 15 to 35 times that of the two fiber mixture, and the dispersant is 0.018 to 0.06% of the mass of the water.
5. The method of claim 1, wherein the adhesive applied in step 4) is one of epoxy adhesive, bismaleimide adhesive, polyimide adhesive, and polyvinyl alcohol.
6. The method of claim 1, wherein the drying temperature in the step 6) is 105 ± 5 ℃ and the drying time is 5 to 10 minutes.
7. A high-temperature-resistant antioxidant electromagnetic film, which is prepared by the preparation method of any one of claims 1 to 6.
CN202211664943.5A 2022-12-23 2022-12-23 High-temperature-resistant antioxidant electromagnetic film and preparation method thereof Pending CN115976880A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105951301A (en) * 2016-07-04 2016-09-21 朗铂新材料科技(上海)有限公司 Preparation method of antioxidant carbon fiber heat insulation felt
CN106567246A (en) * 2016-10-31 2017-04-19 航天材料及工艺研究所 Method used for preparing SiC reinforced low-density porous carbon fiber thermal insulation composite material via chemical vapor infiltration
CN113511914A (en) * 2021-06-29 2021-10-19 冠立科技扬州有限公司 In-situ solidification colloidal forming method of high-performance aluminum oxide-based composite ceramic
CN114055866A (en) * 2021-11-23 2022-02-18 航天特种材料及工艺技术研究所 High-temperature resin-based structural wave-absorbing composite material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105951301A (en) * 2016-07-04 2016-09-21 朗铂新材料科技(上海)有限公司 Preparation method of antioxidant carbon fiber heat insulation felt
CN106567246A (en) * 2016-10-31 2017-04-19 航天材料及工艺研究所 Method used for preparing SiC reinforced low-density porous carbon fiber thermal insulation composite material via chemical vapor infiltration
CN113511914A (en) * 2021-06-29 2021-10-19 冠立科技扬州有限公司 In-situ solidification colloidal forming method of high-performance aluminum oxide-based composite ceramic
CN114055866A (en) * 2021-11-23 2022-02-18 航天特种材料及工艺技术研究所 High-temperature resin-based structural wave-absorbing composite material and preparation method thereof

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