CN112830762A - Preparation method of silicon carbide aerogel heat-insulating material - Google Patents
Preparation method of silicon carbide aerogel heat-insulating material Download PDFInfo
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- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/32—Carbides; Nitrides; Borides ; Silicides
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- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
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Abstract
The invention relates to a preparation method of a silicon carbide aerogel heat-insulating material, belonging to the technical field of heat-insulating materials. The preparation method of the silicon carbide aerogel heat-insulating material comprises the preparation of a silicon carbide aerogel reinforced fiber material and the integral compounding process of the material. Soaking the carbon fiber material in silica sol dissolved with silicon carbide, gelling, aging and drying to obtain the silicon carbide aerogel reinforced fiber material, and then compounding and molding the reinforced material to obtain the aerogel thermal insulation material. The silicon carbide aerogel is applied to the carbon fiber heat-insulating material, so that the carbon fiber heat-insulating material has the advantages of large specific surface area, low heat conductivity coefficient, small density and the like, and the preparation method is simple and is easy for industrial mass production.
Description
Technical Field
The invention belongs to the technical field of heat preservation and insulation materials, and particularly relates to a preparation method of a silicon carbide aerogel heat preservation and insulation material.
Technical Field
The aerogel is a solid material with a nano-porous network structure formed by mutually aggregating nano particles, and has excellent performances of ultralow density, ultrahigh specific surface area, ultrahigh porosity, low thermal conductivity coefficient and the like. The porosity of aerogel materials is more than 90%, and the mesoporous structure in the aerogel materials can enable the aerogel to have excellent heat-insulating performance, so that the aerogel can be widely applied to the fields of battery energy, industrial high-temperature furnaces, aerospace and the like. Aerogel is one of the most potential heat insulation materials at present, but the strength, the brittleness and the mechanical property of the aerogel are poor due to low density and high porosity.
At present, the temperature resistance of the most researched silicon dioxide aerogel is poor, when the temperature is higher than 800 ℃, silicon dioxide aerogel particles shrink and agglomerate, the particles grow up, and the pore structure collapses, so that the specific surface area and the porosity are obviously reduced, and the heat preservation and heat insulation performance of the silicon dioxide aerogel is influenced, therefore, the improvement of the temperature resistance and the mechanical property of the aerogel becomes the main research direction of researchers at present. Relevant data show that the maximum use temperature of the carbon aerogel material can reach 2000 ℃ in an inert atmosphere or a vacuum environment, the temperature resistance of the graphitized carbon aerogel can be further improved, the maximum temperature can reach 3000 ℃, and the carbon aerogel material is expected to become a 'black horse' in the field of heat insulation materials.
The traditional carbon fiber heat-insulating material has the advantages of light weight, low thermal conductivity, good mechanical property and the like, but the defect of over-quick increase of the thermal conductivity at high temperature is overcome, and the application of the heat-insulating material in the scene of 1000 ℃ and higher temperature is limited.
Disclosure of Invention
The invention aims to overcome the problems and defects of the prior art and provides a preparation method of a silicon carbide aerogel thermal insulation material.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a silicon carbide aerogel thermal insulation material comprises the following steps:
1) firstly adding 100-mesh 2000-mesh graphite powder and 100-mesh 1000-mesh silicon carbide powder into 10-30% of silica sol, wherein the mass part ratio of the graphite powder to the silicon carbide powder is 0.5-2: 0.6-5: 8-50, uniformly mixing to obtain sol solution, then pouring the sol solution into a mold filled with carbon fiber materials, just immersing the sol solution in the carbon fiber materials, and standing for gelation for 10-30 minutes; adding a certain amount of ethanol solvent as aging solution to replace the excessive water in the gel, wherein the aging temperature is 35-80 ℃, and the aging standing time is 12-72 hours, so as to obtain alcohol gel; supercritical drying at 7-30MPa and 60-100 deg.C to obtain silicon carbide aerogel reinforced fiber material;
2) compounding the silicon carbide aerogel reinforced fiber material in the step 1) in a multilayer manner, wherein carbon fiber cloth with the thickness of 0.5-1.0mm and carbon paper with the thickness of 0.3-1.5mm are adhered on the layered surface of the silicon carbide aerogel reinforced fiber material, and the adopted adhesive is formed by mixing one, two or more of epoxy resin, phenolic resin, polyurethane resin, furan resin or/and urea resin in any proportion; then the silicon carbide aerogel thermal insulation material is obtained by high temperature treatment at 1400 ℃ to 2200 ℃.
The optimized mass part ratio of the graphite powder, the silicon carbide powder and the silica sol is 0.8-2: 0.6-1.8: 30-45.
The graphite powder is optimized and then 800-1000-mesh graphite powder is selected.
The silicon carbide powder disclosed by the invention is optimized and then selected from 600-1000-mesh silicon carbide powder.
The content of the silica sol is 20 to 25 percent after optimization.
The carbon fiber material provided by the invention is polyacrylonitrile-based carbon fiber, asphalt-based carbon fiber or viscose-based carbon fiber.
The silicon carbide aerogel heat-insulation material comprises a heat-insulation plate material and a heat-insulation barrel material.
The supercritical drying method has the optimized pressure of 10-25MPa and the optimized temperature of 80-100 ℃.
Silica sol: compared with other silicon sources (organic silicon: tetraethoxysilane), the silicon source has low price and simple and easily-controlled production process; SiO 22The content of the polymer affects the strength of the gel, and the content of the polymer is too low, insufficient in strength and too high, and aging is easily caused. Of silicon carbide aerogelsAnd (3) aging process: the structure and properties of the gel will change during aging. The aging conditions selected in the invention enable the gelling process to be more thorough, and the silicon carbide aerogel has small shrinkage in the drying process, so that the performance of the final product is more stable. Supercritical drying treatment process: the supercritical drying process conditions selected in the invention obviously improve the defects of material structure damage, unstable performance and the like caused by large surface tension in the micro-pores in the drying process of the silicon carbide aerogel.
Compared with the prior art, the heat-insulating material is prepared by preparing a silicon carbide aerogel reinforced fiber material and integrally compounding the material, is innovative in method, and has low density (0.1 g/m)3) The composite material has the advantages of good heat preservation and insulation effects, low heat conductivity coefficient (0.021W/m x k), high strength, excellent temperature resistance (the highest temperature can reach 2000 ℃) and the like, and has important significance for promoting the development of the fields of aerospace, industrial pressure furnaces, building industry and the like.
Drawings
FIG. 1 is a schematic diagram of a cross-sectional structure of the present invention;
fig. 2 is a sectional view of the heat insulating structure of the heat insulating cylinder of the present invention.
The main figure numbers in the figures illustrate: 1 is a carbon paper layer, 2 is a carbon fiber cloth layer, 3 is a silicon carbide reinforced fiber material layer, and 4 is an adhesive layer.
In order to more clearly illustrate the embodiments of the present invention, the drawings needed for the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained by those skilled in the art without inventive efforts.
The specific implementation mode is as follows:
example 1
Adding 1000-mesh graphite powder and 800-mesh silicon carbide powder into 20-25% silica sol, wherein the mass part ratio of the graphite powder to the silicon carbide powder is 1.0: 3.0: 40, uniformly mixing to obtain sol solution, pouring the sol solution into a mold filled with a polyacrylonitrile-based carbon fiber material, enabling the sol solution surface to be just immersed in the polyacrylonitrile-based carbon fiber material, and standing until gelation lasts for 10-30 minutes; adding a certain amount of ethanol solvent as aging solution to replace the excessive water in the gel, wherein the aging temperature is 35-80 ℃, and the aging standing time is 12-72 hours, so as to obtain alcohol gel; supercritical drying at 10-25MPa and 80-100 deg.C to obtain silicon carbide aerogel reinforced fiber material;
2) as shown in fig. 1 or fig. 2, the silicon carbide aerogel reinforced fiber material layer 3 in the step 1) is compounded by four layers, carbon fiber cloth 2 with the thickness of 0.5-1.0mm and carbon paper 1 with the thickness of 0.3-1.5mm are adhered on the laminated surface of the silicon carbide aerogel reinforced fiber material, and the adopted adhesive is an adhesive layer 4 formed by mixing epoxy resin, phenolic resin and polyurethane resin in a ratio of 1.0: 1.0: 1.0; then the silicon carbide aerogel thermal insulation material is obtained by high temperature treatment at 1800 ℃ to 2000 ℃.
Example 2
Graphite powder, silicon carbide powder and silica sol are mixed according to the mass fraction ratio of 0.5: 0.6: 20, uniformly mixing, pouring into a mold filled with the polyacrylonitrile-based carbon fiber felt, just immersing the carbon fiber felt in the sol liquid level, standing for 20 minutes to obtain a gel material, replacing excessive water in the gel with an ethanol solvent as an aging liquid, aging at 55 ℃ for 14 hours after sealing to obtain alcohol gel, and performing supercritical drying at 18MPa and 85 ℃ to obtain the silicon carbide aerogel reinforced polyacrylonitrile-based fiber material. As shown in FIG. 1, the silicon carbide aerogel reinforcing fiber 3 is multi-layered and compounded, and a carbon paper 1 having a thickness of 1.0mm and a carbon cloth 2 having a thickness of 0.5mm are bonded to both surfaces of the composite, and the composite is sequentially bonded to each other with an epoxy resin adhesive layer 4 and subjected to a high temperature treatment at 1800 ℃ to obtain a silicon carbide aerogel insulation board heat insulating material.
Example 3
Graphite powder, silicon carbide powder and silica sol are mixed according to the mass fraction ratio of 0.8: 1.2: 35, uniformly mixing, pouring into a mold filled with the viscose-based carbon fiber felt, just immersing the carbon fiber felt in the sol liquid surface, standing for 25 minutes to obtain a gel material, replacing excessive water in the gel with an ethanol solvent as an aging solution, aging at 35 ℃ for 48 hours after sealing to obtain alcogel, and performing supercritical drying at 20MPa and 65 ℃ to obtain the silicon carbide aerogel reinforced viscose-based fiber material. As shown in figure 1, the silicon carbide aerogel reinforced fiber 3 is compounded in a multi-layer way, carbon paper 1 with the thickness of 0.8mm and carbon fiber cloth 2 with the thickness of 1.0mm are adhered to the two surfaces of the silicon carbide aerogel reinforced fiber, and are sequentially adhered together by a phenolic resin adhesive 4, and the silicon carbide aerogel insulation board thermal insulation material is obtained after high-temperature treatment at 1600 ℃.
Example 4
Graphite powder, silicon carbide powder and silica sol are mixed according to the mass fraction ratio of 1.5: 0.8: 42, uniformly mixing, pouring into a mold filled with the pitch-based carbon fiber felt, just immersing the carbon fiber felt on the surface of the sol, standing for 25 minutes to obtain a gel material, replacing excessive water in the gel with an ethanol solvent as an aging solution, aging at 60 ℃ for 60 hours after sealing to obtain alcogel, and performing supercritical drying at 10MPa and 90 ℃ to obtain the silicon carbide aerogel reinforced pitch-based fiber material. As shown in figure 2, the silicon carbide aerogel reinforced fiber 3 is compounded in a multi-layer way, carbon paper 1 with the thickness of 0.5mm and carbon fiber cloth 2 with the thickness of 0.5mm are adhered to the two surfaces of the silicon carbide aerogel reinforced fiber, and are sequentially adhered together by a polyurethane resin adhesive 4, and after winding and forming, the silicon carbide aerogel insulation barrel heat insulation material is obtained after 2200 ℃ high-temperature treatment.
Example 5
Graphite powder, silicon carbide powder and silica sol are mixed according to the mass fraction ratio of 2.0: 3.5: 48, uniformly mixing, pouring into a mold filled with the polyacrylonitrile-based carbon fiber felt, just immersing the carbon fiber felt in the sol liquid level, standing for 30 minutes to obtain a gel material, replacing excessive water in the gel with an ethanol solvent as an aging liquid, aging at 70 ℃ for 36 hours after sealing to obtain alcohol gel, and performing supercritical drying at 7MPa and 100 ℃ to obtain the silicon carbide aerogel reinforced polyacrylonitrile-based fiber material. As shown in figure 1, the silicon carbide aerogel reinforced fiber 3 is compounded in a multi-layer way, carbon paper 1 with the thickness of 0.7mm and carbon fiber cloth 2 with the thickness of 0.5mm are adhered to the two surfaces of the silicon carbide aerogel reinforced fiber, an adhesive layer 4 formed by mixing epoxy resin and phenolic resin according to the proportion of 0.7:0.3 is adopted for adhesion, and the silicon carbide aerogel insulation board is obtained after high-temperature treatment at 2000 ℃.
Example 6
Graphite powder, silicon carbide powder and silica sol are mixed according to the mass fraction ratio of 1.0: 2.4: 40, uniformly mixing, pouring into a mold filled with the pitch-based carbon fiber felt, just immersing the carbon fiber felt on the surface of the sol, standing for 28 minutes to obtain a gel material, replacing excessive water in the gel with an ethanol solvent as an aging solution, aging at 80 ℃ for 24 hours after sealing to obtain alcogel, and performing supercritical drying at 25MPa and 60 ℃ to obtain the silicon carbide aerogel reinforced pitch-based fiber material. As shown in figure 1, the silicon carbide aerogel reinforced fiber 3 is compounded in a multi-layer way, carbon paper 1 with the thickness of 1.2mm and carbon fiber cloth 2 with the thickness of 0.5mm are adhered on the two surfaces, an adhesive layer 4 formed by mixing epoxy resin, polyurethane resin and furan resin according to the proportion of 0.5:0.2:0.3 is adhered together, and the silicon carbide aerogel insulation board heat insulation material is obtained after high-temperature treatment at 2100 ℃.
Claims (9)
1. A preparation method of a silicon carbide aerogel thermal insulation material comprises the following steps:
1) firstly adding 100-mesh 2000-mesh graphite powder and 100-mesh 1000-mesh silicon carbide powder into 10-30% of silica sol, wherein the mass part ratio of the graphite powder to the silicon carbide powder is 0.5-2: 0.6-5: 8-50, uniformly mixing to obtain sol solution, then pouring the sol solution into a mold filled with carbon fiber materials, just immersing the sol solution in the carbon fiber materials, and standing for gelation for 10-30 minutes; adding a certain amount of ethanol solvent as aging solution to replace the excessive water in the gel, wherein the aging temperature is 35-80 ℃, and the aging standing time is 12-72 hours, so as to obtain alcohol gel; supercritical drying at 7-30MPa and 60-100 deg.C to obtain silicon carbide aerogel reinforced fiber material;
2) compounding the silicon carbide aerogel reinforced fiber material in the step 1) in a multilayer manner, wherein carbon fiber cloth with the thickness of 0.5-1.0mm and carbon paper with the thickness of 0.3-1.5mm are adhered on the layered surface of the silicon carbide aerogel reinforced fiber material, and the adopted adhesive is formed by mixing one, two or more of epoxy resin, phenolic resin, polyurethane resin, furan resin or/and urea resin in any proportion; then the silicon carbide aerogel thermal insulation material is obtained by high temperature treatment at 1400 ℃ to 2200 ℃.
2. The method of claim 1, wherein: the mass part ratio of the graphite powder, the silicon carbide powder and the silica sol is 0.8-2: 0.6-1.8: 30-45.
3. The method of claim 1, wherein: the graphite powder is 800-1000 mesh graphite powder.
4. The method of claim 1, wherein: the silicon carbide powder is 600-1000-mesh silicon carbide powder.
5. The method of claim 1, wherein: the silica sol is 20-25% of silica sol.
6. The method of claim 1, wherein: the carbon fiber material is polyacrylonitrile-based carbon fiber, asphalt-based carbon fiber or viscose-based carbon fiber.
7. The method of claim 1, wherein: the silicon carbide aerogel heat-insulating material comprises a heat-insulating plate material and a heat-insulating barrel material.
8. The method of claim 1, wherein: the supercritical drying is carried out at the pressure of 10-25MPa and the temperature of 80-100 ℃.
9. The method of claim 1, wherein: the temperature of the high-temperature treatment is 1800-2000 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114716229A (en) * | 2022-04-14 | 2022-07-08 | 中国科学技术大学先进技术研究院 | Silicon carbide aerogel and preparation method thereof |
| CN114907145A (en) * | 2022-06-10 | 2022-08-16 | 辽宁奥亿达新材料有限公司 | Silicon carbide coating adhesive on surface of carbon fiber composite material and preparation and use method thereof |
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| CN114907145A (en) * | 2022-06-10 | 2022-08-16 | 辽宁奥亿达新材料有限公司 | Silicon carbide coating adhesive on surface of carbon fiber composite material and preparation and use method thereof |
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Application publication date: 20210525 |