CN118125861A - Preparation method of carbon aerogel composite material antioxidation coating - Google Patents
Preparation method of carbon aerogel composite material antioxidation coating Download PDFInfo
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- CN118125861A CN118125861A CN202410264569.2A CN202410264569A CN118125861A CN 118125861 A CN118125861 A CN 118125861A CN 202410264569 A CN202410264569 A CN 202410264569A CN 118125861 A CN118125861 A CN 118125861A
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- carbon aerogel
- composite material
- aerogel composite
- polycarbosilane
- carbon
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- 239000004966 Carbon aerogel Substances 0.000 title claims abstract description 100
- 239000002131 composite material Substances 0.000 title claims abstract description 89
- 239000011248 coating agent Substances 0.000 title claims abstract description 32
- 238000000576 coating method Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 230000003064 anti-oxidating effect Effects 0.000 title claims description 16
- 229920003257 polycarbosilane Polymers 0.000 claims abstract description 56
- 238000001035 drying Methods 0.000 claims abstract description 20
- 238000000197 pyrolysis Methods 0.000 claims abstract description 12
- 230000032683 aging Effects 0.000 claims abstract description 11
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 8
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 7
- 239000004917 carbon fiber Substances 0.000 claims abstract description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 18
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 230000003647 oxidation Effects 0.000 claims description 16
- 238000007254 oxidation reaction Methods 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- 238000005470 impregnation Methods 0.000 claims description 11
- 239000000835 fiber Substances 0.000 claims description 8
- 238000005336 cracking Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 19
- 239000011159 matrix material Substances 0.000 abstract description 7
- 239000012466 permeate Substances 0.000 abstract description 7
- 238000005524 ceramic coating Methods 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract description 2
- 150000003384 small molecules Chemical class 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000004964 aerogel Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011852 carbon nanoparticle Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
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Abstract
The invention discloses a preparation method of an antioxidant coating of a carbon aerogel composite material, which comprises the steps of preparing Polycarbosilane (PCS) sol, impregnating the PCS sol into the carbon aerogel composite material in vacuum, enabling PCS sol small molecules to permeate into nano holes of the material, then performing gel aging, normal pressure drying and high temperature pyrolysis, repeating the steps to volatilize a solvent and a catalyst in the carbon aerogel, and enabling a polycarbosilane high temperature pyrolysis product (SiC) to generate a thin and compact antioxidant coating on the surface of carbon particles to obtain the carbon aerogel composite material with the SiC ceramic coating inside and outside. The material can maintain its shape and performance in an aerobic environment at 1600 ℃. The PCS sol has good wettability to the carbon aerogel composite material, not only can permeate into gaps between the carbon aerogel and fibers, but also can permeate into nano holes of a carbon aerogel matrix, and is adhered to carbon aerogel particles, and after high-temperature pyrolysis, an antioxidant SiC ceramic coating is generated inside and outside the carbon aerogel composite material.
Description
Technical Field
The invention belongs to the field of preparation of carbon aerogel materials, relates to a method for improving oxidation resistance of a composite material, and particularly relates to a preparation method of an oxidation-resistant coating of a carbon aerogel composite material.
Background
The carbon aerogel composite material is a composite material compounded by taking carbon aerogel as a matrix and taking fibers, foam and the like as reinforcements. The carbon aerogel is a nano porous amorphous solid material with a three-dimensional network structure, which is composed of carbon nano particles, has the characteristics of high specific surface area, high porosity and adjustable pore structure, has intrinsic characteristics of the carbon material, is currently known to be the aerogel material with the highest temperature resistance (the temperature can reach more than 2000 ℃ under inert or vacuum atmosphere), has the characteristic of low heat conductivity due to the unique nano pore structure and nano particles, and is a very promising ultra-high temperature heat insulation material. Has wide application prospect in the fields of high-temperature heat insulation, catalyst carriers, battery cathode materials, wastewater treatment, adsorption and the like.
Because the carbon aerogel is easily oxidized in a high-temperature aerobic atmosphere, the carbon aerogel composite material also has the problem of being easily oxidized in the high-temperature aerobic atmosphere, so that the composite material is collapsed in structure, weight loss, heat insulation and mechanical property are greatly reduced, and the carbon aerogel composite material is a bottleneck for limiting the application of the carbon aerogel composite material in the field of high-temperature heat insulation. Aiming at the problem that carbon aerogel and a composite material thereof are easy to oxidize under a high-temperature aerobic atmosphere, an important solution to the problem is to prepare a high-temperature-resistant and oxidation-resistant coating on the surface of the carbon aerogel composite material, for example, an oxidation-resistant ceramic composite shell layer is coated on the surface of the carbon aerogel composite material by Ultramet company in the United states so as to achieve the aim of resisting oxidation of the surface of the carbon aerogel composite material. However, carbon aerogel is a developed porous open-cell structure, and only a coating is prepared on the surface of a material, so that the gas such as air is difficult to block from entering the interior of the material through the nano holes of the matrix and the slit holes of the matrix and the fibers, and the oxidation failure in the interior of the material is caused. The other solution is to chemically modify the carbon aerogel matrix, and adopt precursors of Si, al and Zr to react with the carbon aerogel matrix in a contact way, and generate antioxidant components such as SiC, mullite and ZrCO on the surface of the material through high-temperature pyrolysis.
The method for preparing the antioxidation coating on the surface of the material and performing chemical modification cannot solve the problem of easy oxidation inside the material, and the antioxidation degree is limited. Therefore, in order to realize that the carbon aerogel composite material can be used in an aerobic environment, the problem of oxidation resistance inside and outside the material must be solved simultaneously.
Disclosure of Invention
In view of the above-mentioned shortcomings, it is an object of the present invention to provide a method for improving the oxidation resistance of carbon aerogel composites both external and internal, i.e., bulk.
In order to achieve the above purpose, the PCS sol is used for vacuum impregnation of the carbon aerogel composite material, so that small molecules of the PCS sol are permeated into nano holes of the material, then the steps are repeated for a plurality of times through gel aging, normal pressure drying and high temperature pyrolysis, the solvent and the catalyst in the carbon aerogel volatilize, and a thin and compact antioxidation coating is generated on the surface of carbon particles by a high temperature pyrolysis product (SiC) of the PCS, so that the carbon aerogel composite material with the SiC ceramic coating inside and outside is obtained. The SiC ceramic is a high-temperature resistant and light ceramic material generated by high-temperature pyrolysis of Polycarbosilane (PCS), and can keep the shape and the performance of the SiC ceramic in an aerobic environment at 1600 ℃. The PCS sol is a flowable liquid, has good wettability to the carbon aerogel composite material, can permeate into gaps between the carbon aerogel and fibers, can permeate into nano holes of a carbon aerogel matrix, is adhered to carbon aerogel particles, and generates an antioxidant SiC ceramic coating inside and outside the carbon aerogel composite material after high-temperature pyrolysis.
The invention is realized by the following technical means:
the preparation method of the carbon aerogel composite material antioxidation coating comprises the following steps:
(1) Preparing Polycarbosilane (PCS) sol:
Mixing and stirring polycarbosilane and ethanol for 20-60 min to fully dissolve the polycarbosilane and obtain polycarbosilane sol for later use;
(2) Vacuum impregnation:
Placing a container filled with the carbon aerogel composite material on a bracket of a vacuum impregnation tank, screwing a valve on the tank, and vacuumizing the impregnation tank under the pressure of 0.001-0.03 MPa; then pouring the polycarbosilane sol into a liquid storage tank above an impregnation tank, slowly opening a valve at the joint of the impregnation tank and the liquid storage tank, dripping the polycarbosilane sol into a container filled with a carbon aerogel composite material, and keeping the pressure state for 0.5-3 h;
(3) Gel aging
Sealing the container filled with the carbon aerogel composite material and the polycarbosilane sol in the step (2), and placing the container in a water bath or a drying oven at 30-70 ℃ for gel aging for 10-30 hours to enable the polycarbosilane sol to form polycarbosilane gel on the surface and inside of the carbon aerogel composite material, so as to obtain the carbon aerogel composite material containing the polycarbosilane gel;
(4) Drying under normal pressure
Placing the carbon aerogel composite material containing the polycarbosilane gel in a drying oven for normal pressure gradient drying to obtain the carbon aerogel composite material containing the polycarbosilane coating;
(5) Pyrolysis at high temperature
Placing the carbon aerogel composite material containing the polycarbosilane coating in a cracking furnace, vacuumizing, introducing inert gas nitrogen or argon, continuously heating up, stopping heating after the highest temperature is kept for 0.5-6 h, and naturally cooling to below 100 ℃ under the protection of the mobile inert gas nitrogen or argon to obtain the carbon aerogel composite material containing the SiC coating;
(6) Repeating
And (3) repeating the steps (1) to (5), namely preparing polycarbosilane sol, vacuum impregnating, gel aging, normal-pressure drying and high-temperature cracking, and obtaining the carbon aerogel composite material antioxidation coating.
Further, the mass ratio of polycarbosilane to ethanol in the step (1) is 1:0.8 to 1.5.
Further, the mass ratio of polycarbosilane to ethanol is 1:1.5.
Further, the carbon aerogel composite of step (2) is selected from the group consisting of: any one of carbon fiber reinforced carbon aerogel composite material, carbon foam reinforced carbon aerogel composite material, silicon carbide fiber reinforced carbon aerogel composite material and alumina fiber reinforced carbon aerogel composite material.
Further, the density of the carbon aerogel composite is 0.15-0.8 g/cm 3.
Further, the normal pressure gradient drying of step (4) includes: raising the temperature to 30-50 ℃ at normal temperature for 4-6h, continuously raising the temperature to 50-80 ℃ for 4-6h, and continuously raising the temperature to 80-120 ℃ for 4-6h.
Further, the continuous temperature rise heating in the step (5) is as follows: heating to 900-1200 deg.c at 1-10 deg.c/min.
Further, the repetition number of the step (6) is 1 to 3.
The invention also discloses an anti-oxidation coating of the carbon aerogel composite material prepared by any one of the preparation methods.
The invention has the beneficial effects that:
1. according to the invention, the antioxidation SiC coating is formed on the surface and inside the nano holes of the carbon aerogel composite material by adopting the modes of vacuum impregnation of polycarbosilane sol, gel aging, normal pressure drying and high temperature pyrolysis, so that the antioxidation of the carbon aerogel composite material is effectively improved, and the surface and inside of the carbon aerogel composite material are both antioxidative.
2. The oxidation resistance of the carbon aerogel composite material is obviously improved. After the carbon aerogel composite material containing the SiC coating prepared by the method disclosed by the invention is subjected to oxidation resistance examination in a muffle furnace at 1200 ℃ for 15min, the appearance is intact, the size is not obviously changed, and the mass loss rate is as low as below 10%. There are three main reasons: ① The surface and the interior of the carbon aerogel composite material prepared by the method contain the antioxidation SiC coating, and the antioxidation SiC coating and the carbon aerogel composite material jointly resist the erosion and damage of oxygen to the material, so that the antioxidation performance of the carbon aerogel composite material is improved as a whole. ② Silicon carbide can generate a silicon dioxide glass layer with oxygen in an aerobic high-temperature environment, and the silicon dioxide has extremely low oxygen permeability at high temperature, so that the diffusion of oxygen on the surface and inside of a material can be prevented. ③ And (6) repeating the step (6) to bridge the micro-cracks generated in the last cracking process, so that the coating is more compact and thicker, the time and distance for oxygen to permeate into the material are increased, and the oxidation resistance of the material is improved.
3. The density of the carbon aerogel composite material prepared by the method is increased by about 0.2-0.5 g/cm 3, the thermal conductivity is 0.048-0.139W/m K, and the density and the thermal conductivity are not obviously increased, so that the carbon aerogel composite material can be applied to a thermal protection system of an aerospace craft.
4. The method has the advantages of simple process, low production cost, less influence on environment and easy realization of industrial production.
Drawings
FIG. 1 is a process flow diagram of the method of the present invention.
Detailed Description
The present invention will be further described with reference to examples, but the scope of the present invention is not limited to these examples.
Example 1 as shown in fig. 1, the present invention comprises the steps of:
(1) Preparing Polycarbosilane (PCS) sol:
and mixing and stirring polycarbosilane and ethanol according to the mass ratio of 1:0.8 for 20min to fully dissolve the polycarbosilane. (2) vacuum impregnation:
Placing a container filled with the carbon aerogel composite material on a bracket of a vacuum impregnation tank, screwing a valve on the tank, and vacuumizing the impregnation tank to a pressure of 0.02MPa; and then pouring the polycarbosilane sol prepared in the first step into a liquid storage tank above the dipping tank, slowly opening a valve at the joint of the dipping tank and the liquid storage tank, dripping the polycarbosilane sol into a container filled with the carbon aerogel composite material, and keeping the pressure state for 1h.
The carbon aerogel composite material can be carbon fiber reinforced carbon aerogel composite material, carbon foam reinforced carbon aerogel composite material, silicon carbide fiber reinforced carbon aerogel composite material, alumina fiber reinforced carbon aerogel composite material and the like.
The density range of the carbon aerogel composite material is 0.15-0.7 g/cm 3.
(3) Gel aging
Sealing the container filled with the carbon aerogel composite material and the polycarbosilane sol in the step (2), placing the container in a water bath or a drying oven at 30 ℃, and aging the gel for 10 hours to enable the polycarbosilane sol to form the polycarbosilane gel on the surface and inside of the carbon aerogel composite material, so as to obtain the carbon aerogel composite material containing the polycarbosilane gel.
(4) Drying under normal pressure
Placing the carbon aerogel composite material containing the polycarbosilane gel obtained in the step (3) in a drying box for normal pressure gradient drying, wherein the gradient drying method comprises the following steps of: and (3) heating to 50 ℃ at normal temperature for 5 hours, continuously heating to 80 ℃ for 5 hours, continuously heating to 100 ℃ for 5 hours, and obtaining the carbon aerogel composite material containing the polycarbosilane coating.
(5) Pyrolysis at high temperature
Placing the carbon aerogel composite material containing the polycarbosilane coating obtained in the step (4) in a cracking furnace, vacuumizing, introducing inert gas nitrogen or argon, heating to 1000 ℃ at a speed of 5 ℃/min, preserving heat for 1h at the highest temperature, stopping heating, and naturally cooling to below 100 ℃ under the protection of mobile inert gas nitrogen or argon to obtain the carbon aerogel composite material containing the SiC coating.
(6) Repeating
Repeating the steps (1) to (5), namely preparing polycarbosilane sol, vacuum dipping, gel aging, normal-pressure drying and high-temperature cracking, and repeating for 1 time. Obtaining the carbon aerogel composite material containing the SiC coating.
The antioxidant carbon aerogel composite material prepared in the example 1 has the density of 0.26g/cm 3, the thermal conductivity at room temperature of 0.052W/mK and the mass loss rate of 8.8%.
Examples 2 to 45
The process parameters used in examples 2 to 45 are as shown in Table 1, except for the listed parameters, the process parameters not listed are the same as in example 1. Since the process parameters affecting the oxidation resistance of the carbon aerogel composite are mainly the ratio of raw materials for preparing the polycarbosilane sol, the type of the carbon aerogel composite, and the number of repetitions of step (6), examples 2 to 45 are mainly modified to further explain the present invention.
Table 1 examples 2 to 45 parameter variations
As shown in table 1, with the increase of the repetition number of the step (6), the mass loss rate of the material after the oxidation resistance check is smaller and smaller, and the minimum mass loss rate can reach 6.5% as shown in example 45, because with the increase of the repetition number of the step (6), the micro cracks generated in the last cracking process are closed, the coating is more compact and thicker, the time and distance for oxygen to permeate into the material are increased, and the oxidation resistance of the material is improved. Therefore, the carbon aerogel composite material antioxidation coating prepared by the invention has excellent antioxidation capability in an aerobic high-temperature environment at 1200 ℃.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of one of ordinary skill in the art without departing from the spirit of the present invention. Furthermore, embodiments of the invention and features of the embodiments may be combined with each other without conflict.
Claims (9)
1. A preparation method of an antioxidant coating of a carbon aerogel composite material comprises the following steps:
(1) Preparing polycarbosilane sol:
Mixing and stirring polycarbosilane and ethanol for 20-60 min to fully dissolve the polycarbosilane and obtain polycarbosilane sol for later use;
(2) Vacuum impregnation:
Dropping polycarbosilane sol into a container filled with carbon aerogel composite material, and maintaining the container under vacuum of 0.001-0.03 MPa for 0.5-3 h;
(3) Gel aging
Sealing the container in the step (2), and aging gel in a water bath kettle or a drying oven at the temperature of 30-70 ℃ for 10-30 hours to obtain a carbon aerogel composite material containing polycarbosilane gel;
(4) Drying under normal pressure
Placing the carbon aerogel composite material containing the polycarbosilane gel in a drying oven for normal pressure gradient drying to obtain the carbon aerogel composite material containing the polycarbosilane coating;
(5) Pyrolysis at high temperature
Placing the carbon aerogel composite material containing the polycarbosilane coating in a cracking furnace, vacuumizing, introducing inert gas, continuously heating, stopping heating after the highest temperature is kept for 0.5-6 h, and naturally cooling to below 100 ℃ under the protection of the mobile inert gas to obtain the carbon aerogel composite material containing the SiC coating;
(6) Repeating
And (5) repeating the steps (1) to (5) to obtain the carbon aerogel composite material antioxidation coating.
2. The method of manufacturing according to claim 1, wherein:
the mass ratio of polycarbosilane to ethanol in the step (1) is 1: (0.8-1.5).
3. The preparation method according to claim 2, wherein:
the mass ratio of polycarbosilane to ethanol is 1:1.5.
4. The method of manufacturing according to claim 1, wherein:
The carbon aerogel composite of step (2) is selected from the group consisting of: any one of carbon fiber reinforced carbon aerogel composite material, carbon foam reinforced carbon aerogel composite material, silicon carbide fiber reinforced carbon aerogel composite material and alumina fiber reinforced carbon aerogel composite material.
5. The method of manufacturing according to claim 4, wherein:
The density of the carbon aerogel composite material is 0.15-0.8 g/cm 3.
6. The method of manufacturing according to claim 1, wherein:
The normal pressure gradient drying in the step (4) comprises the following steps: raising the temperature to 30-50 ℃ at normal temperature for 4-6 h, continuously raising the temperature to 50-80 ℃ for 4-6 h, and continuously raising the temperature to 80-120 ℃ for 4-6 h.
7. The method of manufacturing according to claim 1, wherein:
the continuous temperature rise heating in the step (5) is as follows: heating to 900-1200 deg.c at 1-10 deg.c/min.
8. The method of manufacturing according to claim 1, wherein:
The repetition number of the step (6) is 1-3.
9. A carbon aerogel composite oxidation-resistant coating made according to the method of any one of claims 1 to 8.
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