CN116289238A - Carbon fiber hard felt surface coating and preparation process thereof - Google Patents
Carbon fiber hard felt surface coating and preparation process thereof Download PDFInfo
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- CN116289238A CN116289238A CN202310398370.4A CN202310398370A CN116289238A CN 116289238 A CN116289238 A CN 116289238A CN 202310398370 A CN202310398370 A CN 202310398370A CN 116289238 A CN116289238 A CN 116289238A
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- 239000010703 silicon Substances 0.000 abstract description 7
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- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
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- OEIMLTQPLAGXMX-UHFFFAOYSA-I tantalum(v) chloride Chemical compound Cl[Ta](Cl)(Cl)(Cl)Cl OEIMLTQPLAGXMX-UHFFFAOYSA-I 0.000 description 2
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
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- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
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- D—TEXTILES; PAPER
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- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0011—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using non-woven fabrics
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0059—Organic ingredients with special effects, e.g. oil- or water-repellent, antimicrobial, flame-resistant, magnetic, bactericidal, odour-influencing agents; perfumes
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0063—Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/007—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by mechanical or physical treatments
- D06N3/0077—Embossing; Pressing of the surface; Tumbling and crumbling; Cracking; Cooling; Heating, e.g. mirror finish
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0086—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique
- D06N3/0088—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique by directly applying the resin
- D06N3/009—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique by directly applying the resin by spraying components on the web
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
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- D06N2201/00—Chemical constitution of the fibres, threads or yarns
- D06N2201/08—Inorganic fibres
- D06N2201/087—Carbon fibres
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- D06N2209/00—Properties of the materials
- D06N2209/06—Properties of the materials having thermal properties
- D06N2209/067—Flame resistant, fire resistant
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- D06N2209/00—Properties of the materials
- D06N2209/10—Properties of the materials having mechanical properties
- D06N2209/103—Resistant to mechanical forces, e.g. shock, impact, puncture, flexion, shear, compression, tear
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- D06N2209/00—Properties of the materials
- D06N2209/14—Properties of the materials having chemical properties
- D06N2209/143—Inert, i.e. inert to chemical degradation, corrosion resistant
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- D06N2209/00—Properties of the materials
- D06N2209/16—Properties of the materials having other properties
- D06N2209/1685—Wear resistance
Abstract
The invention discloses a carbon fiber hard felt surface coating and a preparation process thereof. The carbon/carbon composite material can be uniformly coated with the resin, the graphite powder, the silicon carbide powder, the carbon fiber powder and the silicon dioxide powder serving as raw materials to form a good dispersion form, so that the binding force between the coating and a matrix is increased, and the coating is prevented from falling off in a high-temperature environment. The invention also provides a preparation method of the composite. Compared with the prior art, the carbon fiber hard felt surface coating prepared by the invention has the performances of high temperature resistance, oxidation resistance, silicon vapor corrosion resistance, corrosion resistance and the like.
Description
Technical Field
The invention relates to the technical field of carbon-based composite materials, in particular to a carbon fiber hard felt surface coating and a preparation process thereof.
Background
The carbon/carbon composite material is a high-performance and high-strength composite material and consists of carbon fibers and a carbon matrix material. They have high heat resistance, corrosion resistance, mechanical strength and abrasion resistance, and thus are widely used in the fields of aviation, aerospace, navigation, automobiles, sports equipment and the like in severe environments such as high temperature, high speed, high load and the like. The following are some advances in the area of carbon/carbon composite research:
(1) Development of new materials: researchers are developing new carbon fibers and matrix materials to improve the performance and reduce the cost of composite materials. Including novel matrix materials based on polymers and metals.
(2) And (3) structural optimization: researchers are developing new design methods and simulation techniques to optimize the structure and performance of composite materials. Including novel design methods based on multi-scale simulation and deep learning.
(3) The manufacturing technology comprises the following steps: researchers are developing new manufacturing techniques to improve the efficiency and quality of carbon/carbon composite manufacturing. Including novel manufacturing techniques based on automation and machine learning.
(4) Application expansion: researchers are expanding the application fields of carbon/carbon composite materials, including sports equipment, medical devices, building materials, and the like. Among them, the application of carbon/carbon composite materials in the field of medical devices is gaining increasing attention.
In general, research progress on carbon/carbon composites is continuously pushing improvement of properties and expansion of application fields thereof.
When the carbon/carbon composite material is at 800 ℃, the oxidation reaction of the active points is more severe, the interface of the carbon/carbon composite material is damaged, the fiber strength is reduced, the connection and load carrying capacity of the carbon matrix are continuously weakened, a large number of thermal damage cracks are formed on the surface and inside of the material, the cracks are expanded, and the material is damaged.
CN110498684a patent provides a method for preparing a silicon carbide coating, comprising the steps of: (1) selecting and manufacturing a blank material: machining to the dimensional accuracy to obtain a primary blank sample; (2) pretreatment of a preform sample: polishing, ultrasonic cleaning and drying for later use; and (3) performing priming pretreatment on the blank sample: uniformly brushing a primer on the surface, and then placing the surface in an oven for drying treatment; (4) coating the coating slurry: coating silicon carbide coating slurry, and drying; (5) sintering treatment: performing atmosphere sintering treatment on the dried primary blank sample; after sintering treatment, a compact silicon carbide coating is formed on the surface of the primary blank sample. The interface of the carbon/carbon composite material is damaged, the fiber strength is reduced, the connection and load carrying capacity of a carbon matrix are continuously weakened, the high-temperature oxidation resistance and the silicon vapor corrosion resistance are weak, and the performance of the carbon/material is further influenced.
Disclosure of Invention
In order to achieve the above purpose, the invention provides a carbon fiber hard felt surface coating, which is characterized in that: comprises resin, graphite powder, silicon carbide powder, carbon fiber powder, fumed silica powder, absolute ethyl alcohol and water.
Preferably, the carbon fiber hard felt surface coating comprises the following raw materials in percentage by weight: 5 to 7.1 weight percent of resin, 4 to 4.4 weight percent of graphite powder, 20 to 22 weight percent of silicon carbide powder, 1.5 to 1.7 weight percent of carbon fiber powder, 1 to 1.2 weight percent of silicon dioxide powder, 12.5 to 13.1 weight percent of absolute ethyl alcohol and the balance of water.
Preferably, the resin is a phenolic resin.
The silicon carbide is used as a main material of the coating, has the characteristics of high strength, excellent wear resistance, excellent corrosion resistance and the like, and has low thermal expansion coefficient, good physical and chemical compatibility with carbon materials and similar linear expansion coefficient, and the properties of high temperature resistance, oxidation resistance, silicon vapor corrosion resistance, corrosion resistance and the like can be improved when the silicon carbide is used in the coating. At the position ofA small amount of graphite is added into the original pure silicon carbide coating to replace a part of silicon carbide, so that the cracking risk of the coating is reduced, the cost is reduced, and the process is simplified. SiO generated by the current composite coating under high-temperature oxidation environment 2 The protective film can effectively prevent oxygen from penetrating, but along with the increase of the oxidation temperature and the extension of the oxidation time, the high-temperature oxidation resistance of the outer coating which is researched at present is not ideal.
Further preferably, the carbon fiber hard felt surface coating comprises the following raw materials in percentage by weight: 5 to 7.1 weight percent of resin, 4 to 4.4 weight percent of graphite powder, 20 to 22 weight percent of silicon carbide powder, 10 to 20 weight percent of triethanolamine borate, 1.5 to 1.7 weight percent of carbon fiber powder, 1 to 1.2 weight percent of silicon dioxide powder, 12.5 to 13.1 weight percent of absolute ethyl alcohol and the balance of water.
Further preferably, the carbon fiber hard felt surface coating comprises the following raw materials in percentage by weight: 5 to 7.1 weight percent of resin, 4 to 4.4 weight percent of graphite powder, 20 to 22 weight percent of silicon carbide powder, 10 to 20 weight percent of triethanolamine borate, 5 to 15 weight percent of additive, 1.5 to 1.7 weight percent of carbon fiber powder, 1 to 1.2 weight percent of silicon dioxide powder, 12.5 to 13.1 weight percent of absolute ethyl alcohol and the balance of water.
The additive is one or a mixture of more of yttrium silicate and aluminum tantalate. Preferably, the mass ratio of the yttrium silicate to the aluminum tantalate is 1:1-2;
yttrium silicate is a ceramic material with high melting point, high hardness and high strength, has an expansion coefficient very close to that of SiC, and has good physical and chemical compatibility. Aluminum tantalate is a high-melting-point substance and has excellent high-temperature oxidation resistance and corrosion resistance. Yttrium silicate, aluminum tantalate and triethanolamine borate are introduced, the dispersibility of inorganic materials and organic substances is effectively improved, the triethanolamine borate is heated to 1700-1800 ℃, yttrium silicate, aluminum tantalate, silicon carbide powder, graphite powder and triethanolamine borate interact and are mutually fused to generate yttrium aluminum garnet phases (YAG, yttrium Aluminum Garnet) or TaC, taB and boron oxide substances, the thermal expansion coefficient of the aluminum tantalate is reduced, the porosity of the coating is reduced, the permeation of oxygen is reduced, the high-temperature strength, the high-temperature oxidation resistance and the shock resistance of the coating are improved, and the compactness of the coating is improved; and simultaneously, carbon fiber powder is introduced, and the carbon fiber improves the bonding strength of the coating through mechanisms such as pulling out, bridging, crack deflection and the like, so that the strength and toughness of the coating are further improved, and the silicon vapor corrosion resistance of the coating at high temperature is improved.
The carbon/carbon composite material can be uniformly coated with resin, graphite powder, silicon carbide powder, carbon fiber powder, silicon dioxide powder, yttrium silicate, aluminum tantalate and triethanolamine borate serving as raw materials to form a good dispersion form, so that the binding force between a coating and a matrix is increased, and the coating is prevented from falling off in a high-temperature environment.
The invention also discloses a preparation process of the carbon fiber hard felt surface coating.
A preparation process of a carbon fiber hard felt surface coating comprises the following steps: adding graphite powder, silicon carbide powder, carbon fiber powder and silicon dioxide powder into water, uniformly mixing, adding resin and absolute ethyl alcohol, uniformly coating the mixture on a carbon fiber hard felt, baking, cooling to room temperature after baking, polishing by using sand paper, and finally calcining in a high-temperature furnace.
Preferably, the baking conditions are: the temperature is 160-180deg.C, and the time is 30-120min;
preferably, the calcination conditions are: the temperature is 1700-1800 ℃ and the calcination time is 1-2h;
preferably, the thickness of the coating is 80-100 μm;
preferably, the carbon fiber hard felt is at least one of PAN-based carbon fiber hard felt, asphalt-based carbon fiber hard felt and viscose-based hard felt.
The invention has the beneficial effects that:
1. the carbon/carbon composite material can be uniformly coated with the resin, the graphite powder, the silicon carbide powder, the carbon fiber powder and the silicon dioxide powder serving as raw materials to form a good dispersion form, so that the binding force between the coating and a matrix is increased, and the coating is prevented from falling off in a high-temperature environment.
2. Yttrium silicate, aluminum tantalate and triethanolamine borate are introduced, the dispersibility of inorganic materials and organic substances is effectively improved, the triethanolamine borate is heated to 1700-1800 ℃, yttrium silicate, aluminum tantalate, silicon carbide powder, graphite powder and triethanolamine borate interact and are mutually fused to generate yttrium aluminum garnet phases (YAG, yttrium Aluminum Garnet) or TaC, taB and boron oxide substances, the thermal expansion coefficient of the aluminum tantalate is reduced, the porosity of the coating is reduced, the permeation of oxygen is reduced, the high-temperature strength, the high-temperature oxidation resistance and the shock resistance of the coating are improved, and the compactness of the coating is improved; and simultaneously, carbon fiber powder is introduced, and the carbon fiber improves the bonding strength of the coating through mechanisms such as pulling out, bridging, crack deflection and the like, so that the strength and toughness of the coating are further improved, and the silicon vapor corrosion resistance of the coating at high temperature is improved.
Drawings
FIG. 1 is a photograph of a carbon fiber stiff felt of the present application;
FIG. 2 is a photograph of a carbon fiber hard felt surface coating of the present application after being dried;
fig. 3 is a photograph of the carbon fiber hard felt surface coating of the present application after calcination.
Detailed Description
Parameters of specific chemicals, sources:
the EXP0371 resin had a free phenol of 8.09%, a moisture of 5.14%, a solids content of 46.8%, a pH of 9.09 and a viscosity of 10.68 mPas at 25 ℃.
Graphite powder, 1.7 μm;
silicon carbide powder, 1.7 μm;
carbon fiber powder, wherein the diameter of a monofilament is 5-10 mu m, and the length-diameter ratio is 3:1-6:1;
fumed silica powder, 10-30nm;
preparation example 1
The preparation method of the aluminum tantalate comprises the step of weighing 0.05mol of TaCl 5 Adding water to obtain tantalum pentachloride solution with the mass concentration of 0.5 g/mL; then 0.05mol of Al (NO) was weighed 3 ) 3 Adding 65wt% ethanol water solution to prepare an aluminum nitrate solution with the mass concentration of 0.5 g/mL; and (3) uniformly mixing the tantalum pentachloride solution and the aluminum nitrate solution, heating to 40 ℃, adopting 9g/mL ammonia water to adjust the pH value to 6, then keeping the reaction for 5 hours, washing and drying after the reaction is finished, and finally heating to 1200 ℃ and preserving the heat for 5 hours to obtain the aluminum tantalate.
Preparation example 2
A preparation method of the PAN-based carbon fiber hard felt comprises the following steps: x1, cutting carbon fiber precursor (Pan base, model T700, zhongfu godet hawk) into chopped filaments with an average length of 6cm in a chopping machine;
x2, the carbon fiber is chopped, cut and carded into net tyres with uniform thickness and needled into soft felt, and the surface density of the soft felt is 90g/m 2 ；
X3 spraying the soft felt with a resin adhesive mixed solution, wherein the resin adhesive mixed solution comprises phenolic resin adhesive (model PF9501, solid content 82.4%, free phenol 14.46%, water 3.72%, viscosity (25 ℃) 5400 mPa.s, pH value 7.90) and absolute ethyl alcohol in a weight ratio of 1:4, placing the sprayed soft felt into a hot press, and carrying out hot press curing for 50min at 140 ℃ under the pressure of 25MPa to obtain a blank; then placing the mixture into a carbonization furnace for carbonization, wherein the carbonization temperature curve is as follows: raising the temperature to 450 ℃ at the heating rate of 0.75 ℃/min, introducing nitrogen for protection, raising the temperature to 850 ℃ at the heating rate of 2.5 ℃/min, preserving the heat for 3 hours, and naturally cooling; then placing the mixture in a high-temperature furnace for purification, wherein the high-temperature purification temperature curve is as follows: raising the temperature to 1000 ℃ at the heating rate of 2 ℃/min, raising the temperature to 1750 ℃ at the heating rate of 1.5 ℃/min, raising the temperature to 2200 ℃ at the heating rate of 1.5 ℃/min, preserving heat for 5h, and naturally cooling to obtain the PAN-based carbon fiber hard felt.
Example 1
A preparation process of a carbon fiber hard felt surface coating comprises the following steps: adding graphite powder, silicon carbide powder, carbon fiber powder and fumed silica powder into water, uniformly mixing, adding EXP0371 resin and absolute ethyl alcohol, uniformly mixing, uniformly coating on PAN-based carbon fiber hard felt, baking at 160 ℃ for 1h, cooling to medium room temperature after baking, polishing by using sand paper, and finally calcining at 1800 ℃ for 1h in a high-temperature furnace; wherein the thickness of the coating is 100 μm; wherein the raw materials comprise 7.1wt% of EXP0371 resin, 4.3wt% of graphite powder, 21.5wt% of silicon carbide powder, 1.6wt% of carbon fiber powder, 1.1wt% of fumed silica powder, 51.5wt% of water and 12.9wt% of absolute ethyl alcohol.
Example 2
A preparation process of a carbon fiber hard felt surface coating comprises the following steps: adding graphite powder, silicon carbide powder, carbon fiber powder and fumed silica powder into water, uniformly mixing, adding EXP0371 resin and absolute ethyl alcohol, uniformly mixing, uniformly coating on PAN-based carbon fiber hard felt, baking at 160 ℃ for 1h, cooling to medium room temperature after baking, polishing by using sand paper, and finally calcining at 1800 ℃ for 1h in a high-temperature furnace; wherein the thickness of the coating is 100 μm; wherein the raw materials comprise 5.5wt% of EXP0371 resin, 4.4wt% of graphite powder, 21.8wt% of silicon carbide powder, 1.6wt% of carbon fiber powder, 1.1wt% of fumed silica powder, 52.5wt% of water and 13.1wt% of absolute ethyl alcohol.
Example 3
A preparation process of a carbon fiber hard felt surface coating comprises the following steps: adding graphite powder, silicon carbide powder, carbon fiber powder, fumed silica powder and triethanolamine borate into water, uniformly mixing, adding EXP0371 resin and absolute ethyl alcohol, uniformly mixing, uniformly coating the mixture on PAN-based carbon fiber hard felt, baking at 160 ℃ for 1h, cooling to the middle room temperature after baking, polishing by using sand paper, and finally calcining at 1800 ℃ for 1h in a high-temperature furnace; wherein the thickness of the coating is 100 μm; wherein the raw materials comprise 5.5wt% of EXP0371 resin, 4.4wt% of graphite powder, 21.8wt% of silicon carbide powder, 1.6wt% of carbon fiber powder, 1.1wt% of fumed silica powder, 10wt% of triethanolamine borate, 42.5wt% of water and 13.1wt% of absolute ethyl alcohol.
Example 4
A preparation process of a carbon fiber hard felt surface coating comprises the following steps: adding graphite powder, silicon carbide powder, carbon fiber powder, fumed silica powder, yttrium silicate and triethanolamine borate into water, uniformly mixing, adding EXP0371 resin and absolute ethyl alcohol, uniformly mixing, uniformly coating the mixture on PAN-based carbon fiber hard felt, baking at 160 ℃ for 1h, cooling to room temperature after baking, polishing by using sand paper, and finally calcining at 1800 ℃ for 1h in a high-temperature furnace; wherein the thickness of the coating is 100 μm; the raw materials comprise 5.5wt% of EXP0371 resin, 4.4wt% of graphite powder, 21.8wt% of silicon carbide powder, 1.6wt% of carbon fiber powder, 1.1wt% of fumed silica powder, 10wt% of triethanolamine borate, 8wt% of yttrium silicate, 34.5wt% of water and 13.1wt% of absolute ethyl alcohol.
Example 5
A preparation process of a carbon fiber hard felt surface coating comprises the following steps: adding graphite powder, silicon carbide powder, carbon fiber powder, fumed silica powder, aluminum tantalate and triethanolamine borate into water, uniformly mixing, adding EXP0371 resin and absolute ethyl alcohol, uniformly mixing, uniformly coating the mixture on PAN-based carbon fiber hard felt, baking at 160 ℃ for 1h, cooling to room temperature after baking, polishing by using sand paper, and finally calcining at 1800 ℃ for 1h in a high-temperature furnace; wherein the thickness of the coating is 100 μm; the raw materials comprise 5.5wt% of EXP0371 resin, 4.4wt% of graphite powder, 21.8wt% of silicon carbide powder, 1.6wt% of carbon fiber powder, 1.1wt% of fumed silica powder, 10wt% of triethanolamine borate, 8wt% of aluminum tantalate, 34.5wt% of water and 13.1wt% of absolute ethyl alcohol.
Example 6
A preparation process of a carbon fiber hard felt surface coating comprises the following steps: adding graphite powder, silicon carbide powder, carbon fiber powder, fumed silica powder, an additive and triethanolamine borate into water, uniformly mixing, adding EXP0371 resin and absolute ethyl alcohol, uniformly mixing, uniformly coating the mixture on PAN-based carbon fiber hard felt, baking at 160 ℃ for 1h, cooling to room temperature after baking, polishing by using sand paper, and finally calcining at 1800 ℃ for 1h in a high-temperature furnace; wherein the thickness of the coating is 100 μm; wherein the raw materials comprise 5.5wt% EXP0371 resin, 4.4wt% graphite powder, 21.8wt% silicon carbide powder, 1.6wt% carbon fiber powder, 1.1wt% gas phase silicon dioxide powder, 10wt% triethanolamine borate, 8wt% additive, 34.5wt% water and 13.1wt% absolute ethyl alcohol; the additive is prepared from yttrium silicate and aluminum tantalate according to a mass ratio of 1:2.
Example 7
A preparation process of a carbon fiber hard felt surface coating comprises the following steps: adding graphite powder, silicon carbide powder, carbon fiber powder, fumed silica powder and aluminum tantalate into water, uniformly mixing, adding EXP0371 resin and absolute ethyl alcohol, uniformly mixing, uniformly coating the mixture on PAN-based carbon fiber hard felt, baking at 160 ℃ for 1h, cooling to the middle room temperature after baking, polishing by using sand paper, and finally calcining at 1800 ℃ for 1h in a high-temperature furnace; wherein the thickness of the coating is 100 μm; wherein the raw materials comprise 5.5wt% of EXP0371 resin, 4.4wt% of graphite powder, 21.8wt% of silicon carbide powder, 1.6wt% of carbon fiber powder, 1.1wt% of fumed silica powder, 8wt% of aluminum tantalate, 44.5wt% of water and 13.1wt% of absolute ethyl alcohol.
Example 8
A preparation process of a carbon fiber hard felt surface coating comprises the following steps: adding graphite powder, silicon carbide powder, carbon fiber powder, fumed silica powder and yttrium silicate into water, uniformly mixing, adding EXP0371 resin and absolute ethyl alcohol, uniformly mixing, uniformly coating the mixture on PAN-based carbon fiber hard felt, baking at 160 ℃ for 1h, cooling to room temperature after baking, polishing by using sand paper, and finally calcining at 1800 ℃ for 1h in a high-temperature furnace; wherein the thickness of the coating is 100 μm, and the raw materials are 5.5wt% EXP0371 resin, 4.4wt% graphite powder, 21.8wt% silicon carbide powder, 1.6wt% carbon fiber powder, 1.1wt% gas phase silicon dioxide powder, 8wt% yttrium silicate, 44.5wt% water and 13.1wt% absolute ethyl alcohol.
Comparative example 1
A preparation process of a carbon fiber hard felt surface coating comprises the following steps: adding silicon carbide powder, carbon fiber powder and fumed silica powder into water, uniformly mixing, adding resin and absolute ethyl alcohol, uniformly mixing, uniformly coating on PAN-based carbon fiber hard felt, baking for 1h at 160 ℃, cooling to the middle room temperature after baking, polishing by using sand paper, and finally calcining for 1h at 1800 ℃ in a high-temperature furnace; wherein the thickness of the coating is 100 μm; wherein the raw materials comprise 5.5wt% of EXP0371 resin, 26.2wt% of silicon carbide powder, 1.6wt% of carbon fiber powder, 1.1wt% of fumed silica powder, 52.5wt% of water and 13.1wt% of absolute ethyl alcohol.
Test example 1
The high-temperature oxidation resistance testing method comprises the following steps: the oxidation experiment of the coating was carried out in static air in a high temperature tube furnace, the carbon fiber hard felt sample containing the coating was placed in a corundum crucible, and then the crucible was placed in the tube furnace which had reached the set temperature. Taking out the crucible at intervals, weighing the sample after cooling, and then placing the crucible back into the tube furnace, and repeating the steps until the preset experiment time is reached. Weight loss = (original sample weight-sample weight after high temperature treatment)/original sample weight×100%, where both original sample weight and sample weight refer to surface coating weight.
TABLE 1 high temperature antioxidant test results
From the above table 1, it can be seen from the comparison of the comparative example 1 and the example 2 that the high temperature oxidation resistance of the example 2 is significantly better than that of the comparative example 1, and a small amount of graphite is added to replace a part of silicon carbide based on the example, so that the cracking risk of the coating is reduced, the cost is reduced, the process is simplified, and meanwhile, the bonding strength of the coating is improved by the carbon fiber through the mechanisms of pulling out, bridging, crack deflection and the like, so that the strength and toughness of the coating are further improved.
By comparing the examples 2-3, it is found that the oxidation resistance of the example 3 is improved compared with the example 2, and the triethanolamine borate is added on the basis of the example 2, so that the dispersion of graphite powder, silicon carbide powder, carbon fiber powder and fumed silica powder can be effectively improved, boron oxide can be generated by heating to 1700-1800 ℃, the porosity of the coating is further reduced, the permeation of oxygen is reduced, the high-temperature strength, the high-temperature oxidation resistance and the shock resistance of the coating are improved, and the compactness of the coating is improved.
Comparing examples 4-6, the oxidation resistance of example 6 is improved compared with examples 4-5, and yttrium silicate is a ceramic material with high melting point, high hardness and high strength, has an expansion coefficient very close to that of SiC, and has good physicochemical compatibility; aluminum tantalate is a high-melting-point substance and has excellent high-temperature oxidation resistance and corrosion resistance; yttrium silicate, aluminum tantalate and triethanolamine borate are introduced into the coating, the triethanolamine borate improves the dispersibility of inorganic materials and organic substances, the inorganic materials and the organic substances are heated to 1700-1800 ℃, the yttrium silicate, the aluminum tantalate, the silicon carbide powder, the graphite powder and the triethanolamine borate interact and fuse with each other to generate yttrium aluminum garnet phases (YAG, yttrium Aluminum Garnet) or TaC, taB and boron oxide substances, the thermal expansion coefficient of the aluminum tantalate is reduced, the porosity of the coating is reduced, the permeation of oxygen is reduced, the high-temperature strength, the high-temperature oxidation resistance and the shock resistance of the coating are improved, and the compactness of the coating is improved; and simultaneously, carbon fiber powder is introduced, and the carbon fiber improves the bonding strength of the coating through mechanisms such as pulling out, bridging, crack deflection and the like, so that the strength and toughness of the coating are further improved, and the silicon vapor corrosion resistance of the coating at high temperature is improved.
Test example 2
Treating the carbon fiber hard felt sample containing the coating at a high temperature of 1500 ℃ for 3 days under a certain silicon steam concentration, thus obtaining a complete process cycle; the second process cycle then continues. When cracks appear on the coating of the carbon fiber hard felt containing the coating and/or 10% of the coating with the area falls off, the carbon fiber hard felt containing the coating cannot be used any more. The time when the coating first appears in the situation is the service life of the coating.
Table 2 life test results
| Service life/month | |
| Example 1 | 9-10 |
| Example 2 | 9-10 |
| Example 3 | 12-14 |
| Example 4 | 17-19 |
| Example 5 | 17-19 |
| Example 6 | 20-22 |
| Example 7 | 15-18 |
| Example 8 | 15-18 |
| Comparative example 1 | 7-8 |
The carbon/carbon composite material can be uniformly coated with resin, graphite powder, silicon carbide powder, carbon fiber powder, fumed silica powder, yttrium silicate, aluminum tantalate and triethanolamine borate serving as raw materials, so that a good dispersion form is formed, the binding force of a coating and a matrix is increased, and the coating is prevented from falling off in a high-temperature environment.
Claims (9)
1. A preparation process of a carbon fiber hard felt surface coating is characterized by comprising the following steps: adding silicon carbide powder, carbon fiber powder and silicon dioxide powder into water, uniformly mixing, adding resin and absolute ethyl alcohol, uniformly coating the mixture on a carbon fiber hard felt, baking, cooling to room temperature after baking, polishing by using sand paper, and finally calcining in a high-temperature furnace.
2. The process for preparing the carbon fiber hard felt surface coating according to claim 1, wherein the process comprises the following steps: adding graphite powder, silicon carbide powder, carbon fiber powder and silicon dioxide powder into water, uniformly mixing, adding resin and absolute ethyl alcohol, uniformly coating the mixture on a carbon fiber hard felt, baking, cooling to room temperature after baking, polishing by using sand paper, and finally calcining in a high-temperature furnace.
3. The process for preparing the carbon fiber hard felt surface coating according to claim 2, wherein the process comprises the following steps: also included are triethanolamine borates.
4. The process for preparing the carbon fiber hard felt surface coating according to claim 2, wherein the process comprises the following steps: additives are also included.
5. The process for preparing the carbon fiber hard felt surface coating according to claim 2, wherein the process comprises the following steps: the baking conditions: the temperature is 160-180deg.C, and the time is 30-120min.
6. The process for preparing the carbon fiber hard felt surface coating according to claim 2, wherein the process comprises the following steps: the calcination conditions are as follows: the temperature is 1700-1800 ℃ and the calcination time is 1-2h.
7. The process for preparing the carbon fiber hard felt surface coating according to claim 2, wherein the process comprises the following steps: the carbon fiber hard felt is at least one of PAN-based carbon fiber hard felt, asphalt-based carbon fiber hard felt and viscose-based hard felt.
8. The carbon fiber hard felt surface coating is characterized in that: prepared by the preparation method of any one of claims 1 to 7.
9. The use of a carbon fiber hard felt surface coating according to claim 8, wherein: the method is applied to the fields of photovoltaics, semiconductors, vacuum heat treatment and the like.
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