In-situ ceramicized EPDM erosion-resistant thermal insulation material and preparation method thereof
By using hyperbranched polycarbosilane and high-temperature-resistant ceramicized precursors in the insulating layer of the solid rocket engine, a co-cured interface structure is formed, which solves the problem of loose and porous carbon layer ablation of the insulating layer, significantly improves the erosion resistance and ensures the safety of the engine.
Patent Information
- Application Number
- CN202411800733.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-09
- Publication Date
- 2025-04-04
AI Technical Summary
Under high temperature conditions, the ablated carbon layer of the ethylene propyl group insulating layer of solid rocket engines is loose and porous, which reduces the erosion resistance and has a safety risk of burning through and disintegrating.
Hyperbranched polycarbosilane is used to replace phenolic resin, and the three-dimensional carbon fiber braid is immersed by high-temperature ceramicization precursor, and the ceramic coating is formed by high-temperature heat treatment. The interface co-curing is achieved through carbon-carbon unsaturated bonding, enhancing the binding performance of carbon fiber and ethylene propylene matrix.
The formation of a solid and dense carbon layer structure significantly improves the erosion resistance of the insulation material and avoids the safety hazards of the engine thermal insulation layer burning through and disintegrating under long-term high overload conditions.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of thermal protection materials for solid engines, and in particular to an ethylene propylene diene monomer erosion-resistant thermal insulation material that can be in-situ ceramicized and a preparation method thereof. Background Art
[0002] Under the service condition of 3000℃ for solid rocket engines, the EPDM rubber insulation layer absorbs most of the heat through self-ablation, forming an ablated carbon layer to play an anti-insulation role and protect the integrity of the engine structure. For some high-overload solid engines, high-temperature gas and propellant combustion products, aluminum oxide condensed phase particles, will aggravate the ablation of the insulation layer, posing a safety risk of engine burnout and disintegration. Carbon fiber braided reinforced rubber-based composite materials have the advantages of high carbonization, ablation resistance, and adaptability to the molded patch process of the engine combustion chamber. They are often used as reinforcement layers for solid engine insulation layers to resist the erosion of high-temperature gas and condensed phase particles.
[0003] CN115895130A provides a three-dimensional carbon fiber braided body reinforced EPDM-phenolic erosion-resistant composite material and a preparation method thereof. The compatibility of the EPDM / phenolic composite resin matrix is improved by grafting modified phenolic resin. The prepared C3D / EPDM / PF erosion-resistant composite material can be co-vulcanized with the EPDM insulation layer to improve the interfacial bonding strength of the solid engine insulation layer. However, the problem that the phenolic resin is cured to form a fluffy and porous carbon layer that reduces the erosion resistance has not yet been solved.
[0004] Ceramics can promote the formation of high-temperature dense ablation carbon layers in composite materials. CN105925001A discloses an alumina fiber-reinforced hybrid resin-based composite material, which uses Si, B, C, and N hybrid resins as the matrix and alumina fibers as the reinforcement. The RTM process is used to prepare the thermal structural material, which has good high-temperature mechanical properties and can be used in the end / leading edge, aerodynamic shell, rudder / wing, combustion chamber and other parts of the aircraft. During service, the hybrid resin matrix is in-situ ceramicized to improve the thermal oxidation resistance of the composite material. However, Si, B, C, and N hybrid resins are relatively rigid, and the composite materials prepared as resin matrices have poor flexibility and are less compatible with the molding and patching processes of the insulation layer of solid rocket engines. CN118754696A provides a method for preparing a carbon / carbon composite material, using polyolefin as a matrix resin and cyclized organic fiber as a reinforcement to prepare a carbon / carbon composite material precursor, further impregnating the surface with carbon-based or silicon-based materials such as tetramethylsilane and polycarbosilane, pyrolyzing and densifying to obtain a carbon / carbon-silicon carbide ceramic composite material, thereby improving the oxidation resistance of the carbon / carbon composite material. Using polyolefin thermoplastic resin as a matrix resin, the carbonization performance of polyolefin is improved by chemically grafting polar groups, effectively solving the problems of long curing cycle and complicated molding process of traditional matrix resins such as phenolic resin, but the interface performance between the polyolefin matrix and the silicon base is not solved, which will reduce the material mechanics and aging life. Summary of the invention
[0005] The invention provides an EPDM erosion-resistant thermal insulation material that can be in-situ ceramicized and a preparation method thereof, which can solve the problem that a high-temperature carbon layer of an EPDM composite material reinforced with a carbon fiber braid is loose and the erosion resistance is reduced.
[0006] An EPDM erosion-resistant thermal insulation material capable of in-situ ceramicization comprises the following raw materials in parts by mass: 10-30 parts of EPDM rubber, 60-70 parts of carbon fiber braid, 1.2-3 parts of vulcanizer, 0.5-2 parts of vulcanization accelerator, 2-5 parts of high temperature resistant ceramic precursor, and 4-15 parts of hyperbranched polycarbosilane.
[0007] Optionally, the hyperbranched polycarbosilane is a vinyl terminated hyperbranched polycarbosilane or an ethynyl terminated hyperbranched polycarbosilane. Optionally, the high temperature resistant ceramic precursor is any one or more of polyhafnium carbosilane, polyzirconium carbosilane, polytitanium silane and polyborosilazane.
[0008] Optionally, the raw material satisfies at least one of the following conditions: The vulcanizing agent is sulfur and dicumyl peroxide; The vulcanization accelerator is any one or more of triallyl isocyanurate (TAIC), terpene compounds, trimethylolpropane triacrylate (TMPTA), trimethylolpropane trimethacrylate (TMPTMA), pentaerythritol triacrylate (PET3A), and polybutadiene.
[0009] Optionally, the fiber volume content of the carbon fiber braid is 40-60%, and the braid thickness is 4-8 mm.
[0010] The present invention also relates to a method for preparing the thermal insulation material, comprising the following steps: S1. The carbon fiber braid is subjected to surface etching treatment in an air atmosphere at 200°C to improve the surface roughness; S2, using a solvent to dissolve a high temperature resistant ceramic precursor to obtain an impregnation solution 1, placing the carbon fiber braid obtained in S1 into the impregnation solution 1 for immersion, and then drying and heat treating to obtain a three-dimensional carbon fiber braid coated with a ceramic coating; S3, kneading EPDM, a vulcanizing agent and a vulcanization accelerator to form a film, dissolving the film with a solvent to obtain an impregnation solution 2, impregnating a three-dimensional carbon fiber braid coated with a ceramic coating in the impregnation solution 2, and then drying to obtain a ceramicized carbon fiber braid reinforced EPDM prepreg; S4. The ceramicizable carbon fiber braid is reinforced with ethylene propylene diene monomer prepreg and is molded and cured to obtain an in-situ ceramicizable ethylene propylene diene monomer erosion-resistant thermal insulation material.
[0011] Optionally, the solvent in S2 is any one or more of toluene, dichloromethane, and chloroform; and the heat treatment temperature is 1500°C.
[0012] Optionally, S3 satisfies at least one of the following conditions: The solvent in S3 is any one or more of toluene, xylene, cyclohexane, heptane, and solvent gasoline; The immersion temperature is 40~80℃, the immersion pressure is 1~3MPa, and the immersion time is 0.5~2h; When the film is dissolved with a solvent, hyperbranched polycarbosilane is also added to dissolve to obtain an impregnation solution 2; The drying temperature is 80°C.
[0013] Optionally, in S4, the curing temperature is 150° C., the curing pressure is 2 MPa, and the curing time is the positive vulcanization point+10 min.
[0014] The thermal insulation material of the present invention is characterized in that a high-temperature resistant ceramic precursor is impregnated on the surface of a carbon fiber braid, high-temperature treatment is performed to ceramicize it in situ to obtain a carbon fiber braid coated with a ceramic coating, and hyperbranched polycarbosilane and an ethylene propylene diene monomer are impregnated for the second time, and the interface co-curing of the polycarbosilane precursor and the ethylene propylene diene monomer is achieved through the action of carbon-carbon unsaturated bonds, thereby improving the interface bonding performance between the ethylene propylene diene monomer and the carbon fiber. Meanwhile, the polycarbosilane precursor can be ceramicized in situ during the high-temperature service process of the engine, thereby delaying the high-temperature sublimation and gasification of the carbon fiber, increasing the degree of graphitization of the carbon fiber, forming a solid and dense carbon layer structure, and improving the erosion resistance.
[0015] The present invention has the following beneficial effects: (1) The ceramicizable EPDM erosion-resistant thermal insulation material of the present invention uses hyperbranched polycarbosilane to replace phenolic resin, retains a certain flexibility under 150°C curing conditions to meet the requirements of the thermal insulation layer molding process, and in-situ ceramicizes the hyperbranched polycarbosilane and adheres to the surface of the carbon fiber braid under high-temperature service conditions to form a solid carbon layer structure, thereby solving the problem of loose and porous carbon layer caused by ablation of phenolic resin in the preparation of EPDM erosion-resistant thermal insulation material, and avoiding safety hazards such as burn-through and disintegration of the engine thermal insulation layer under long-duration and high-overload conditions.
[0016] (2) The present invention uses a high-temperature resistant ceramic precursor to impregnate a three-dimensional carbon fiber braid, and obtains a carbon fiber braid covered with a high-temperature resistant ceramic coating through high-temperature heat treatment. The carbon fiber braid can delay the decomposition and sublimation of the carbon fiber under high-temperature conditions, promote the graphitization process of the carbon fiber, and improve the erosion resistance of the high-temperature ablated carbon layer, thereby avoiding the safety hazard caused by structural failure of the prepared erosion-resistant layer under high overload conditions. Compared with preparing ceramic fibers through melt spinning, infusible treatment and high-temperature pyrolysis of high-temperature resistant ceramic precursors, the present invention uses ceramic fibers with higher brittleness and poorer weavability mixed with carbon fibers as the reinforcing phase, which has the advantage of simple operation process.
[0017] (3) The present invention uses a high-temperature resistant ceramic precursor with good interface bonding performance with the carbon fiber to impregnate the carbon fiber. The high-temperature resistant ceramic fiber synthesized in situ on the surface of the carbon fiber after high-temperature heat treatment can be used as a transition layer, and has good interface bonding with the hyperbranched polycarbosilane precursor with similar structural components. Under the action of the sulfur and diisopropylbenzene peroxide vulcanization system, the hyperbranched polycarbosilane precursor forms an interpenetrating cross-linked network with the ethylene propylene diene monomer matrix through carbon-carbon unsaturated bonds, which solves the problem of poor interface bonding between the ethylene propylene diene monomer matrix and the carbon fiber, and avoids the quality risk of the erosion-resistant insulation layer caused by micro-interface separation of the composite material. DETAILED DESCRIPTION
[0018] The present invention is described in detail below in conjunction with specific embodiments. This embodiment is implemented based on the technical solution of the present invention, and provides a detailed implementation method and a specific operation process, but the protection scope of the present invention is not limited to the following embodiments.
[0019] The experimental methods in the following examples are conventional methods unless otherwise specified. The raw materials, reagents, etc. used in the following examples are commercially available products unless otherwise specified.
[0020] Comparative Example 1: An EPDM erosion-resistant thermal insulation material has the following formula: 25 parts of EPDM rubber, 1 part of sulfur, 2 parts of dicumyl peroxide, 2 parts of trimethylolpropane triacrylate and 70 parts of carbon fiber braid.
[0021] Preparation method: (1) A three-dimensional carbon fiber braid with a fiber volume content of 45% and a 6 mm diameter was prepared by braiding carbon fibers. The surface of the carbon fiber braid was etched in an air atmosphere at 200°C to remove the sizing agent on the surface of the carbon fiber and increase the surface roughness of the carbon fiber. (2) EPDM, sulfur, diisopropylbenzene peroxide and trimethylolpropane triacrylate are mixed in an internal mixer to prepare an EPDM film, cyclohexane is used to dissolve the EPDM film to prepare an impregnation solution, a surface-etched three-dimensional carbon fiber braid is placed in the impregnation solution, and the three-dimensional carbon fiber braid is pressurized at 50°C, 2MPa, for 1h and dried at 80°C to obtain a carbon fiber braid reinforced EPDM prepreg; (3) The carbon fiber braided body is reinforced with ethylene propylene diene monomer prepreg and molded and cured at 150°C and 2 MPa to obtain an ethylene propylene diene monomer erosion-resistant thermal insulation material.
[0022] Comparative Example 2: An EPDM erosion-resistant thermal insulation material that can be in-situ ceramicized has a formula of: 25 parts of EPDM rubber, 1 part of sulfur, 2 parts of dicumyl peroxide, 2 parts of trimethylolpropane triacrylate, 5 parts of polyhafnium carbosilane and 65 parts of carbon fiber braid.
[0023] Preparation method: (1) A three-dimensional carbon fiber braid with a fiber volume content of 45% and a 6 mm diameter was prepared by braiding carbon fibers. The surface of the carbon fiber braid was etched in an air atmosphere at 200°C to remove the sizing agent on the surface of the carbon fiber and increase the surface roughness of the carbon fiber. (2) using chloroform to dissolve polyhafnium carbosilane to prepare an impregnation solution 1, placing the etched three-dimensional carbon fiber braid in the impregnation solution 1, pressurizing and impregnating, drying, and performing a heat treatment at 1500° C. to obtain a three-dimensional carbon fiber braid coated with a ceramic coating; (3) EPDM, sulfur, diisopropylbenzene peroxide and trimethylolpropane triacrylate are mixed in an internal mixer to prepare an EPDM film, cyclohexane is used to dissolve the EPDM film to prepare an impregnation solution 2, a three-dimensional carbon fiber braid coated with a ceramic coating is placed in the impregnation solution 2, and the mixture is impregnated under pressure at 50°C, 2MPa, for 1h and dried at 80°C to obtain a ceramicized carbon fiber braid reinforced EPDM prepreg; (4) The ceramicizable carbon fiber braid reinforced ethylene propylene diene monomer prepreg is compression-cured at 150°C and 2 MPa to obtain an in-situ ceramicizable ethylene propylene diene monomer erosion-resistant thermal insulation material.
[0024] Embodiment 1: An EPDM erosion-resistant thermal insulation material that can be in-situ ceramicized has a formula of: 10 parts of EPDM rubber, 1 part of sulfur, 2 parts of dicumyl peroxide, 2 parts of trimethylolpropane triacrylate, 5 parts of polyhafnium carbosilane, 15 parts of vinyl-terminated hyperbranched polycarbosilane, and 65 parts of carbon fiber braid.
[0025] Preparation method: (1) A three-dimensional carbon fiber braid with a fiber volume content of 45% and a 6 mm diameter was prepared by braiding carbon fibers. The surface of the carbon fiber braid was etched in an air atmosphere at 200°C to remove the sizing agent on the surface of the carbon fiber and increase the surface roughness of the carbon fiber. (2) using chloroform to dissolve polyhafnium carbosilane to prepare an impregnation solution 1, placing the etched three-dimensional carbon fiber braid in the impregnation solution 1, pressurizing and impregnating, drying, and performing a heat treatment at 1500° C. to obtain a three-dimensional carbon fiber braid coated with a ceramic coating; (3) EPDM, sulfur, diisopropylbenzene peroxide and trimethylolpropane triacrylate are mixed in an internal mixer to prepare an EPDM film, cyclohexane is used to dissolve the EPDM film and vinyl-terminated hyperbranched polycarbosilane to prepare an impregnation solution 2, a three-dimensional carbon fiber braid coated with a ceramic coating is placed in the impregnation solution 2, and the mixture is impregnated at 50°C, 2MPa, for 1h under pressure and dried at 80°C to obtain a ceramicized carbon fiber braid reinforced EPDM prepreg; (4) The ceramicizable carbon fiber braid reinforced ethylene propylene diene monomer prepreg is compression-cured at 150°C and 2 MPa to obtain an in-situ ceramicizable ethylene propylene diene monomer erosion-resistant thermal insulation material.
[0026] Embodiment 2: An EPDM erosion-resistant thermal insulation material that can be in-situ ceramicized, the formula of which is: 30 parts of EPDM rubber, 0.8 parts of sulfur, 1.0 parts of dicumyl peroxide, 1.2 parts of triallyl isocyanurate, 3 parts of polytitanium silane, 4 parts of ethynyl-terminated hyperbranched polycarbosilane, and 60 parts of carbon fiber braid; Preparation method: (1) The carbon fibers were woven to prepare a three-dimensional carbon fiber braid with a fiber volume content of 60% and the surface of the carbon fiber braid was etched in an air atmosphere at 200°C to remove the sizing agent on the surface of the carbon fiber and increase the surface roughness of the carbon fiber; (2) using toluene to dissolve polytitanium silane to prepare an impregnation solution 1, placing the etched three-dimensional carbon fiber braid in the impregnation solution 1, pressurizing and impregnating, drying, and performing a heat treatment at 1500° C. to obtain a three-dimensional carbon fiber braid coated with a ceramic coating; (3) EPDM, sulfur, diisopropylbenzene peroxide and triallyl isocyanurate are mixed in an internal mixer to prepare an EPDM film, cyclohexane is used to dissolve the EPDM film and acetylene-terminated hyperbranched polycarbosilane to prepare an impregnation solution 2, a three-dimensional carbon fiber braid coated with a ceramic coating is placed in the impregnation solution 2, and the mixture is impregnated at 80°C, 3MPa, and pressured for 2h at 80°C and dried at 80°C to obtain a ceramicized carbon fiber braid reinforced EPDM prepreg; (4) The ceramicizable carbon fiber braid reinforced ethylene propylene diene monomer prepreg is compression-cured at 150°C and 2 MPa to obtain an in-situ ceramicizable ethylene propylene diene monomer erosion-resistant thermal insulation material.
[0027] Embodiment 3: An EPDM erosion-resistant thermal insulation material that can be in-situ ceramicized, the formula of which is: 20 parts of EPDM rubber, 0.2 parts of sulfur, 1.0 parts of dicumyl peroxide, 0.8 parts of trimethylolpropane trimethacrylate, 4 parts of polyborosilazane, 12 parts of ethynyl-terminated hyperbranched polycarbosilane, and 62 parts of carbon fiber braid; Preparation method: (1) The carbon fibers were woven to prepare a three-dimensional carbon fiber braid with a fiber volume content of 40% and the surface of the carbon fiber braid was etched in an air atmosphere at 200°C to remove the sizing agent on the surface of the carbon fiber and increase the surface roughness of the carbon fiber; (2) using toluene to dissolve polyborosilazane to prepare an impregnation solution 1, placing the etched three-dimensional carbon fiber braid in the impregnation solution 1, pressurizing and impregnating, drying, and performing a heat treatment at 1500° C. to obtain a three-dimensional carbon fiber braid coated with a ceramic coating; (3) EPDM, sulfur, diisopropylbenzene peroxide and trimethylolpropane triacrylate are mixed in an internal mixer to prepare an EPDM film, cyclohexane is used to dissolve the EPDM film and acetylene-terminated hyperbranched polycarbosilane to prepare an impregnation solution 2, a three-dimensional carbon fiber braid coated with a ceramic coating is placed in the impregnation solution 2, and the mixture is impregnated under pressure at 40°C, 1MPa, for 1.5h and dried at 80°C to obtain a ceramicized carbon fiber braid reinforced EPDM prepreg; (4) The ceramicizable carbon fiber braid reinforced ethylene propylene diene monomer prepreg is compression-cured at 150°C and 2 MPa to obtain an in-situ ceramicizable ethylene propylene diene monomer erosion-resistant thermal insulation material.
[0028] Embodiment 4: An EPDM erosion-resistant thermal insulation material that can be in-situ ceramicized, the formula of which is: 15 parts of EPDM rubber, 0.3 parts of sulfur, 1.2 parts of dicumyl peroxide, 0.5 parts of pentaerythritol triacrylate, 2 parts of polyzirconium carbosilane, 15 parts of vinyl-terminated hyperbranched polycarbosilane, and 66 parts of carbon fiber braid; Preparation method: (1) Weaving carbon fibers to prepare a three-dimensional carbon fiber braid with a fiber volume content of 50% of 5 mm, and performing surface etching treatment on the carbon fiber braid in an air atmosphere at 200°C to remove the sizing agent on the carbon fiber surface and increase the surface roughness of the carbon fiber; (2) using dichloromethane to dissolve polyzirconium carbosilane to prepare an impregnation solution 1, placing the etched three-dimensional carbon fiber braid in the impregnation solution 1, pressurizing and impregnating, drying, and performing a heat treatment at 1500° C. to obtain a three-dimensional carbon fiber braid coated with a ceramic coating; (3) EPDM, sulfur, diisopropylbenzene peroxide and pentaerythritol triacrylate are mixed in an internal mixer to prepare EPDM film, cyclohexane is used to dissolve the EPDM film and vinyl-terminated hyperbranched polycarbosilane to prepare impregnation solution 2, a three-dimensional carbon fiber braid coated with a ceramic coating is placed in the impregnation solution 2, and the mixture is impregnated at 60°C, 2.5 MPa, and pressured for 0.5 h at 80°C and dried to obtain a ceramicized carbon fiber braid reinforced EPDM prepreg; (4) The ceramicizable carbon fiber braid reinforced ethylene propylene diene monomer prepreg is compression-cured at 150°C and 2 MPa to obtain an in-situ ceramicizable ethylene propylene diene monomer erosion-resistant thermal insulation material.
[0029] The high temperature resistant ceramic precursor used in the above comparative examples and embodiments has a ceramic yield of 40-60% at 1500°C; after the hyperbranched polycarbosilane terminated with unsaturated carbon-carbon bonds is cured at 150°C, the high temperature ceramic yield is 60-80%.
[0030] Comparative Example 2 is a comparative case of using a high temperature resistant ceramic precursor to treat carbon fiber for ceramic coating in Comparative Example 1, Example 1 is a comparative case of using a hyperbranched polycarbosilane and EPDM rubber composite as the resin matrix of the erosion resistant material in Comparative Example 2, and Examples 1 to 4 are cases of different material formulations, impregnation processes and curing processes. The carbon fiber braid reinforced EPDM / phenolic erosion resistant composite material was used as a blank group, and the thermal insulation materials prepared in Comparative Examples 1 and 2 and Examples 1 to 4 were tested for oxygen-acetylene wire ablation rate, and the results are shown in Table 1.
[0031] Table 1 Oxygen-acetylene line ablation rate of erosion-resistant insulation materials
[0032] Note: Ablation time is 60s.
[0033] The above embodiments describe the preferred implementation of the present invention, but the present invention is not limited thereto. Within the technical concept of the present invention, the technical solution of the present invention can be subjected to a variety of simple modifications, including the combination of various technical features in any other manner, and these simple modifications and combinations should also be regarded as the contents disclosed by the present invention and belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.
Claims
1. An EPDM erosion-resistant thermal insulation material that can be in-situ ceramicized, characterized in that: Including the following raw materials by mass: 10-30 parts of EPDM rubber, 60-70 parts of carbon fiber braid, 1.2-3 parts of vulcanizer, 0.5-2 parts of vulcanization accelerator, 2-5 parts of high temperature resistant ceramic precursor, and 4-15 parts of hyperbranched polycarbosilane.
2. The thermal insulation material according to claim 1, characterized in that: The fiber volume content of the carbon fiber braid is 40-60%, and the braid thickness is 4-8 mm.
3. The thermal insulation material according to claim 1, characterized in that: The vulcanizing agent is sulfur and dicumyl peroxide.
4. The thermal insulation material according to claim 1, characterized in that: The vulcanization accelerator is any one or more of triallyl isocyanurate (TAIC), terpene compounds, trimethylolpropane triacrylate (TMPTA), trimethylolpropane trimethacrylate (TMPTMA), pentaerythritol triacrylate (PET3A), and polybutadiene.
5. The thermal insulation material according to claim 1, characterized in that: The high temperature resistant ceramic precursor is any one of polyhafnium carbosilane, polyzirconium carbosilane, polytitanium silane and polyborosilazane.
6. The thermal insulation material according to claim 1, characterized in that: The hyperbranched polycarbosilane is a vinyl-terminated hyperbranched polycarbosilane or an ethynyl-terminated hyperbranched polycarbosilane.
7. The method for preparing the thermal insulation material according to any one of claims 1 to 6, characterized in that: The following steps are involved: S1. The carbon fiber braid is subjected to surface etching treatment in an air atmosphere at 200-300°C to improve the surface roughness; S2, using a solvent to dissolve a high temperature resistant ceramic precursor to obtain an impregnation solution 1, placing the carbon fiber braid obtained in S1 into the impregnation solution 1 for immersion, and then drying and heat treating to obtain a three-dimensional carbon fiber braid coated with a ceramic coating; S3, kneading EPDM, a vulcanizing agent and a vulcanization accelerator to form a film, dissolving the film with a solvent to obtain an impregnation solution 2, impregnating a three-dimensional carbon fiber braid coated with a ceramic coating in the impregnation solution 2, and then drying to obtain a ceramicized carbon fiber braid reinforced EPDM prepreg; S4. The ceramicizable carbon fiber braid is reinforced with ethylene propylene diene monomer prepreg and is molded and cured to obtain an in-situ ceramicizable ethylene propylene diene monomer erosion-resistant thermal insulation material.
8. The preparation method according to claim 7, characterized in that: The solvent in S2 is any one or more of toluene, dichloromethane, and chloroform; the heat treatment temperature is 1500°C.
9. The preparation method according to claim 7, characterized in that: S3 meets at least one of the following conditions: The solvent in S3 is any one or more of toluene, xylene, cyclohexane, heptane, and solvent gasoline; The immersion temperature is 40~80℃, the immersion pressure is 1~3MPa, and the immersion time is 0.5~2h; When the film is dissolved in a solvent, hyperbranched polycarbosilane is added to dissolve to obtain an impregnation solution 2; The drying temperature is 80°C.
10. The preparation method according to claim 7, characterized in that: In S4, the curing temperature is 150°C, the curing pressure is 2MPa, and the curing time is positive vulcanization point + 10min.
Citation Information
Patent Citations
Alumina fiber reinforced hybrid resin-based composite material and preparation method thereof
CN105925001A
Carbon / carbon composite material and preparation method and application thereof
CN118754696A