High-temperature-resistant semi-flexible thermal protection component and preparation method thereof
By designing a composite structure of silicon-based coating and thin-walled metal radiation layer, the problems of brittleness and easy deformation of traditional thermal protection components in extremely high temperature environments are solved, and efficient heat insulation and stable thermal protection effects are achieved to adapt to complex environmental conditions.
Patent Information
- Application Number
- CN202511011035.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-22
- Publication Date
- 2025-10-17
AI Technical Summary
Traditional thermal protection components have problems such as high brittleness, poor mechanical properties, easy deformation and functional failure in extremely high temperature environments. In addition, existing flexible insulation felts are easy to peel off during long-term use, making it difficult to meet the efficient insulation requirements of hot-end components such as engines.
A high-temperature resistant semi-flexible thermal protection component consisting of a silicon-based coating, a thin-walled metal radiation layer and a high-temperature resistant insulation layer is used. The thin-walled metal radiation layer is treated by plasma etching and anodizing, and combined with the dynamic cross-linking design of the silicon-based coating, a composite structure of multi-layer aerogel insulation material and fiber cloth material is formed to ensure the stability and flexibility of the component in high-temperature environments.
It achieves efficient thermal insulation in extreme environments, avoids cracks and falling off of components, ensures the overall bonding strength and interface compatibility of components, adapts to complex environmental conditions, and provides good thermal stability and long-term stability.
Smart Images
Figure CN120792286A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of heat protection, in particular to a high-temperature-resistant semi-flexible heat protection component and a preparation method thereof. BACKGROUND
[0002] The heat protection component is a key structure applied to an extremely high-temperature environment, which realizes heat blocking transmission through material design and composite process, and thus realizes heat protection of equipment, system, personnel, etc. The heat protection component is required for the heat end components such as engines to realize efficient heat insulation under the condition of limited space weight, and to have good environmental adaptability such as high-temperature resistance, moisture resistance, corrosion resistance, etc. The traditional heat protection component includes rigid ceramic heat insulation tiles and flexible heat insulation felt. The ceramic heat insulation tiles have problems such as large brittleness and poor mechanical properties, which seriously restrict the application of the ceramic heat insulation tiles in the field of heat protection components. The heat insulation felt has more excellent thermal matching, and the manufacturing and installation process is relatively simple, but the heat insulation felt will have problems such as deformation and peeling during long-term use, and thus is prone to functional failure. SUMMARY
[0003] In view of the problems existing in the prior art, the purpose of the present application is to provide a high-temperature-resistant semi-flexible heat protection component, which has the characteristics of high heat resistance, high corrosion resistance, and conformability, and has the advantages of rigid and flexible heat protection components. The heat protection component has strong heat shock resistance and environmental adaptability, and can effectively adapt to the complex environmental conditions such as high-temperature airflow scouring, rain or moisture of the heat end of the engine.
[0004] Another purpose of the present application is to provide a preparation method of the high-temperature-resistant semi-flexible heat protection component.
[0005] The purpose of the present application is achieved by the following technical solutions. A high-temperature-resistant semi-flexible heat protection component includes a silicon-based coating layer, a thin-wall metal radiation layer, and a high-temperature-resistant heat insulation layer from top to bottom. The high-temperature-resistant heat insulation layer is made of a plurality of layers of aerogel heat insulation materials, which are laid and wrapped by a fiber cloth material, and finally stitched by high-temperature-resistant fiber suture. The front surface of the thin-wall metal radiation layer corresponds to the high-temperature-resistant heat insulation layer, and the outer circle of the thin-wall metal radiation layer is bent to wrap the side edges of the high-temperature-resistant heat insulation layer. The thickness of the bent edge of the thin-wall metal radiation layer is higher than the thickness of the high-temperature-resistant heat insulation layer, and an air layer is formed between the thin-wall metal radiation layer and the high-temperature-resistant heat insulation layer. The silicon-based coating layer is uniformly sprayed on the side surface of the thin-wall metal radiation layer away from the high-temperature-resistant heat insulation layer.
[0006] Based on further optimization of the above scheme, the silicon-based coating includes a silicone rubber matrix, phenyltrimethoxysilane, KH560 (γ-glycidyloxypropyltrimethoxysilane), bismaleimide and nano-SiO2 particles. The silicone rubber matrix adopts methylphenyl silicone rubber with a phenyl content of 15%. The particle size of the nano-SiO2 particles is 20 to 50 nm; the thickness of the silicone-based coating is 30 to 70 μm.
[0007] Based on further optimization of the above solution, the thin-walled metal radiation layer adopts Ti foil, and is sequentially subjected to plasma etching, anodization and immersion in 3-isocyanatepropyltrimethoxysilane; the thickness of the thin-walled metal radiation layer is 0.05-0.15 mm.
[0008] Based on further optimization of the above solution, the thickness of the air interlayer is 0.5-1 mm; the outer circle of the thin-walled metal radiation layer is bent and wrapped around the side of the high-temperature insulation layer, and the width protruding on the back of the high-temperature insulation layer is 50-100 mm.
[0009] Based on further optimization of the above scheme, the fiber cloth material adopts one of basalt fiber cloth or glass fiber cloth, and the aerogel insulation material adopts at least one of glass fiber reinforced aerogel material, basalt fiber reinforced aerogel material, and alumina fiber reinforced aerogel material; the thickness of the fiber cloth material is 0.1~0.2mm, and the thickness of the single-layer aerogel material is 0.5~2mm.
[0010] A method for preparing a high-temperature resistant semi-flexible heat protection component, comprising: Step S1, pre-treatment of the thin-walled metal radiation layer: first, the thin-walled metal radiation layer is cleaned and vacuum-dried to remove oil stains on the surface of the thin-walled metal radiation layer; then, the treated thin-walled metal radiation layer is plasma-etched and anodized in sequence; Step S2, preparation of silicon-based coating base liquid: first, disperse nano-SiO2 particles in anhydrous toluene, and add terminal hydroxyl polymethylphenylsiloxane (molecular weight 5000-10000), and conduct reflux reaction under nitrogen protection. After centrifugal drying, add the coated nano-SiO2 particles and KH560 into an autoclave, and inject the silicone rubber matrix. After sealing, introduce CO2 to a critical state, stir evenly, and release the pressure to obtain a uniformly dispersed nano-SiO2 / silicone rubber matrix. Step S3, thin-walled metal radiation layer treatment: immerse the thin-walled metal radiation layer pretreated in step S1 in 3-isocyanatepropyltrimethoxysilane, let it stand for a period of time at room temperature, take it out and then dry it; Step S4, spraying a silicon-based coating: first, dissolving KH560 and phenyltrimethoxysilane in deionized water containing acetic acid, stirring at low temperature to form a hydrolyzed silane mixture; taking the nano-SiO2 / silicone rubber matrix, the hydrolyzed silane mixture and bismaleimide (BMI) in step S2, uniformly stirring, spraying them on the surface of the thin-walled metal radiation layer in step S3, and pre-curing to form a bottom layer; adjusting the phenyltrimethoxysilane content of the hydrolyzed silane mixture in the spraying liquid, and the remaining components are the same as those in the bottom layer, spraying them on the surface of the bottom layer, and pre-curing to form a middle layer; adjusting the phenyltrimethoxysilane and bismaleimide contents of the hydrolyzed silane mixture in the spraying liquid, spraying them on the surface of the middle layer, and pre-curing to form a surface layer; finally, performing gradient temperature curing and annealing to obtain a thin-walled metal radiation layer sprayed with a silicon-based coating; Step S5, preparing a high-temperature resistant thermal insulation layer: first, arranging multiple layers of aerogel thermal insulation material from top to bottom, then wrapping the arranged multiple layers of aerogel thermal insulation material with fiber cloth material, and finally connecting the wrapped materials with high-temperature fiber sutures in a V-shaped suture pattern to obtain a high-temperature resistant thermal insulation layer; Step S6, preparation of heat protection components: Place the high-temperature resistant insulation layer in step S5 on the side of the thin-walled metal radiation layer away from the silicon-based coating, and achieve the covering of the high-temperature resistant insulation layer by bending the side of the thin-walled metal radiation layer. The inner side of the thin-walled metal radiation layer (i.e., the side away from the silicon-based coating) is connected to the high-temperature resistant insulation layer by pre-coating an adhesive.
[0011] Based on further optimization of the above scheme, the cleaning in step S1 is specifically as follows: ultrasonic cleaning is performed using anhydrous ethanol for 13 to 17 minutes; and vacuum drying is performed at a temperature of 60 to 70° C. for 1.3 to 1.7 hours.
[0012] Based on further optimization of the above scheme, the plasma etching in step S1 is specifically as follows: argon gas is used for plasma etching, with a power of 100-150 W, an argon gas flow rate of 18-22 sccm, a vacuum degree of 4.5-5.5 Pa, and an etching time of 5-8 min; the anodic oxidation is specifically as follows: the thin-walled metal radiation layer after plasma etching is used as the anode and graphite is used as the cathode, and a 0.5 mol / L sulfuric acid solution is used as the electrolyte, and oxidation is carried out at a DC voltage of 9-11 V for 12-18 min.
[0013] Based on the further optimization of the above scheme, the mass-volume ratio of the nano-SiO2 particles, anhydrous toluene and hydroxy-terminated polymethylphenylsiloxane in step S2 is 9.5-10.5 g: 95-105 mL: 4.5-5.5 g; the reflux reaction temperature is 75-85℃, and the time is 3.5-4.5 h; the centrifugal drying is as follows: first, use a high-speed centrifuge at a speed of 8000-10000 rpm for 15-20 min, and then place the coated nano-SiO2 particles in a vacuum drying oven at a temperature of 60-80℃ for 2-3 h.
[0014] Based on the further optimization of the above scheme, the mass ratio of the coated nano-SiO2 particles, KH560 and silicone rubber matrix in step S2 is 4.5-5.5: 0.2-0.3: 48-52; the critical state is a temperature of 31.1℃ and a pressure of 7.38 MPa, and the stirring time is 28-32 min.
[0015] Based on the further optimization of the above scheme, the standing time in step S3 is 8-12 min, the drying temperature is 75-85℃, and the drying time is 5-7 min.
[0016] Based on the further optimization of the above scheme, the mass-volume ratio of KH560, phenyltrimethoxysilane and deionized water containing acetic acid in step S4 is 1.8-2.2 g: 4.8-5.2 g: 48-52 mL; the content of acetic acid in the deionized water containing acetic acid is 0.08-0.12 wt%; the low-temperature stirring temperature is 3-5℃, the stirring rate is 120-150 rpm, and the stirring time is 0.8-1.2 h.
[0017] Based on the further optimization of the above scheme, the content of phenyltrimethoxysilane in the bottom layer, the middle layer and the surface layer in step S4 increases in turn, and the content of bismaleimide in the surface layer is lower than that in the bottom layer; specifically, in the bottom layer, the mass ratio of nano-SiO2 / silicone rubber matrix to bismaleimide is 100: 0.45-0.55, and the content of phenyltrimethoxysilane in the hydrolyzed silane mixture accounts for 2.5-3.5 wt% of the nano-SiO2 / silicone rubber matrix; in the middle layer, the mass ratio of nano-SiO2 / silicone rubber matrix to bismaleimide is 100: 0.45-0.55, and the content of phenyltrimethoxysilane in the hydrolyzed silane mixture accounts for 4.5-5.5 wt% of the nano-SiO2 / silicone rubber matrix; in the surface layer, the mass ratio of nano-SiO2 / silicone rubber matrix to bismaleimide is 100: 0.25-0.35, and the content of phenyltrimethoxysilane in the hydrolyzed silane mixture accounts for 7.5-8.5 wt% of the nano-SiO2 / silicone rubber matrix.
[0018] Based on the further optimization of the above scheme, the pre-curing temperature of the bottom layer, the middle layer and the surface layer in the step S4 is 75-85 DEG C, and the pre-curing time is 8-12 min; the spraying thickness of the middle layer is greater than that of the bottom layer, and the bottom layer is equal to the surface layer.
[0019] Based on the further optimization of the above scheme, the gradient temperature curing in the step S4 is specifically as follows: the sprayed thin-wall metal radiation layer is placed in an oven, and is heated at a rate of 4-6 DEG C / min to 75-85 DEG C, and is kept for 28-32 min, then is heated at a rate of 3-4 DEG C / min to 115-125 DEG C, and is kept for 0.8-1.2 h, finally is heated at a rate of 3-4 DEG C / min to 175-185 DEG C, and is kept for 1.8-2.2 h; the annealing is specifically as follows: after curing, the temperature is cooled to 58-62 DEG C with the furnace temperature, and is kept for 1.8-2.2 h, and then is reduced to room temperature at a rate of 0.5-1 DEG C / min.
[0020] The following are the technical effects possessed by the scheme of the present application: The present application realizes the physical and chemical double anchoring through the pretreatment of the thin-wall metal radiation layer by plasma etching and anodic oxidation, and realizes the spraying of the thin-wall metal radiation layer by 3-isocyanate propyl trimethoxysilane and the silicon-based raw material formed by mixing KH560, phenyl trimethoxysilane, nano-SiO2 / silicon rubber matrix and bismaleimide, which not only improves the mechanical properties and wear resistance of the whole silicon-based coating, but also balances the high-temperature resistance and flexibility of the silicon-based coating through dynamic crosslinking and gradient coating design, so as to effectively resist stress and strain in the bending process and high-temperature process of the silicon-based coating on the thin-wall metal radiation layer, and avoid cracks and other problems caused by bending or thermal stress; at the same time, through the design and preparation process of the above-mentioned silicon-based coating and the thin-wall metal radiation layer, the bonding strength between the silicon-based coating and the thin-wall metal radiation layer is effectively improved, and the problems of cracking and peeling of the coating caused by the difference in expansion coefficient between the silicon rubber and the titanium foil are avoided.
[0021] The thermal protection component provided by the present application can match the hot end component, and overcomes the shortcomings of metal corrosion and high-temperature oxidation under extreme environmental conditions; at the same time, the semi-open packaging structure effectively reduces the weight, and realizes light heat insulation; at the same time, the whole thermal protection component has high overall bonding strength, good interface compatibility and good thermal stability, effectively avoids the problems of interlayer separation, coating cracking or peeling in the bending or high-temperature process, and ensures the stability of long-term use. BRIEF DESCRIPTION OF DRAWINGS
[0022] Figure 1 It is the overall structure schematic diagram of the thermal protection component in the embodiment of the present application.
[0023] Figure 2 It is the back view (or bottom view) of the thermal protection component in the embodiment of the present application. It is the back view (or bottom view) of the thermal protection component in the embodiment of the present application.
[0024] 10, silicon-based coating layer; 20, thin-wall metal radiation layer; 21, air interlayer; 31, aerogel thermal insulation material; 32, fiber cloth material. DETAILED DESCRIPTION
[0025] To make the objectives, technical solutions, and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly described below. Obviously, the described embodiments are some but not all of the embodiments of the present application.
[0026] Embodiment 1 A high-temperature-resistant semi-flexible thermal protection component, which comprises, from top to bottom, a silicon-based coating layer, a thin-wall metal radiation layer, and a high-temperature-resistant thermal insulation layer. The high-temperature-resistant thermal insulation layer is made of 16 layers of aerogel thermal insulation material and is wrapped by fiber cloth material. Finally, the high-temperature-resistant thermal insulation layer is sewn by high-temperature fiber suture. The fiber cloth material is basalt fiber cloth, and the aerogel thermal insulation material is glass fiber reinforced aerogel material and basalt fiber reinforced aerogel material. The thickness of the fiber cloth material is 0.1 mm, and the thickness of the single-layer aerogel material is 0.5 mm. The front surface of the thin-wall metal radiation layer corresponds to the high-temperature-resistant thermal insulation layer, and the outer circle of the thin-wall metal radiation layer is bent to wrap the side edges of the high-temperature-resistant thermal insulation layer. The thin-wall metal radiation layer is made of Ti foil and is sequentially subjected to plasma etching, anodic oxidation, and 3-isocyanate propyl trimethoxysilane immersion. The thickness of the thin-wall metal radiation layer is 0.05 mm. The thickness of the bent edge of the thin-wall metal radiation layer is higher than the thickness of the high-temperature-resistant thermal insulation layer, and an air interlayer is formed between the thin-wall metal radiation layer and the high-temperature-resistant thermal insulation layer. The thickness of the air interlayer is 0.5 mm. The outer circle of the thin-wall metal radiation layer is bent to wrap the side edges of the high-temperature-resistant thermal insulation layer, and the width of the protrusion on the back surface of the high-temperature-resistant thermal insulation layer is 50 mm. The silicon-based coating layer is uniformly sprayed on the surface of the side of the thin-wall metal radiation layer away from the high-temperature-resistant thermal insulation layer. The silicon-based coating layer comprises a silicone rubber matrix, phenyl trimethoxysilane, KH560 (γ-glycidyl ether propyl trimethoxysilane), bismaleimide, and nano-SiO2 particles. The silicone rubber matrix is methyl phenyl silicone rubber with a phenyl content of 15%, and the particle size of the nano-SiO2 particles is 20 nm. The thickness of the silicon-based coating layer is 30 μm.
[0027] A preparation method of a high-temperature-resistant semi-flexible thermal protection component, comprising: Step S1, thin-wall metal radiation layer pretreatment: first, the thin-wall metal radiation layer is ultrasonically cleaned with anhydrous ethanol for 13 min, and then the cleaned thin-wall metal radiation layer is vacuum dried at a temperature of 60 ℃ for 1.7 h to remove the oil stains on the surface of the thin-wall metal radiation layer.
[0028] Then, the treated thin-wall metal radiation layer is subjected to plasma etching and anodic oxidation. The plasma etching is performed by using argon with a power of 100 W, an argon flow rate of 18 sccm, a vacuum degree of 4.5 Pa, and an etching time of 8 min. The anodic oxidation is performed by using the thin-wall metal radiation layer after plasma etching as an anode, graphite as a cathode, and 0.5 mol / L sulfuric acid solution as an electrolyte under a direct current voltage of 9 V for 18 min.
[0029] In step S2, the silicon-based coating base liquid is prepared. First, the nano-SiO2 particles are dispersed in anhydrous toluene, and hydroxyl-terminated polymethylphenylsiloxane (molecular weight 5000-10000) is added. The mass-volume ratio of the nano-SiO2 particles, anhydrous toluene, and hydroxyl-terminated polymethylphenylsiloxane is 9.5 g:95 mL:4.5 g. The backflow reaction is carried out under nitrogen protection at a backflow reaction temperature of 75°C for 4.5 h. After centrifugal drying, the coated nano-SiO2 particles are first subjected to high-speed centrifugation at a speed of 8000 rpm for 20 min, and then placed in a vacuum drying oven at a temperature of 60°C for 3 h. The coated nano-SiO2 particles and KH560 are added to a high-pressure reaction kettle, and the silicon rubber matrix is injected. The mass ratio of the coated nano-SiO2 particles, KH560, and silicon rubber matrix is 4.5:0.2:48. After sealing, CO2 is introduced to the critical state, i.e., a temperature of 31.1°C and a pressure of 7.38 MPa. The mixture is uniformly stirred for 28 min, and then depressurized to obtain a uniformly dispersed nano-SiO2 / silicon rubber matrix.
[0030] In step S3, the thin-wall metal radiation layer is treated. The pretreated thin-wall metal radiation layer in step S1 is immersed in 3-isocyanate propyl trimethoxysilane, and then left to stand at room temperature for 8 min. After taking out, the thin-wall metal radiation layer is dried at a temperature of 75°C for 7 min.
[0031] In step S4, the silicon-based coating is sprayed. First, KH560 and phenyltrimethoxysilane are dissolved in deionized water containing acetic acid. The mass-volume ratio of KH560, phenyltrimethoxysilane, and deionized water containing acetic acid is 1.8 g:4.8 g:48 mL, and the acetic acid content is 0.08 wt%. The hydrolyzed silane mixture is formed by low-temperature stirring at a temperature of 3°C, a stirring rate of 120 rpm, and a stirring time of 1.2 h.
[0032] The nano-SiO2 / silicone rubber matrix, the hydrolyzed silane mixed solution and the bismaleimide (BMI) in step S2 are uniformly stirred, and then sprayed on the surface of the thin-walled metal radiation layer in step S3 to form a bottom layer after pre-curing, the pre-curing temperature is 75℃, the pre-curing time is 12min, and the thickness of the bottom layer is 9μm; the content of phenyltrimethoxysilane in the hydrolyzed silane mixed solution in the spraying liquid is adjusted, and the rest of the components are the same as those in the bottom layer, which is sprayed on the surface of the bottom layer to form a middle layer after pre-curing, the pre-curing temperature is 75℃, the pre-curing time is 12min, and the thickness of the middle layer is 12μm; the content of phenyltrimethoxysilane and bismaleimide in the hydrolyzed silane mixed solution in the spraying liquid is adjusted, and then sprayed on the surface of the middle layer to form a surface layer after pre-curing, the pre-curing temperature is 75℃, the pre-curing time is 12min, and the thickness of the surface layer is 9μm; the content of phenyltrimethoxysilane in the bottom layer, the middle layer and the surface layer is gradually increased, and the content of bismaleimide in the surface layer is lower than that in the bottom layer; specifically, in the bottom layer, the mass ratio of nano-SiO2 / silicone rubber matrix to bismaleimide is 100:0.45, and the content of phenyltrimethoxysilane in the hydrolyzed silane mixed solution accounts for 2.5wt% of the nano-SiO2 / silicone rubber matrix; in the middle layer, the mass ratio of nano-SiO2 / silicone rubber matrix to bismaleimide is 100:0.45, and the content of phenyltrimethoxysilane in the hydrolyzed silane mixed solution accounts for 4.5wt% of the nano-SiO2 / silicone rubber matrix; in the surface layer, the mass ratio of nano-SiO2 / silicone rubber matrix to bismaleimide is 100:0.25, and the content of phenyltrimethoxysilane in the hydrolyzed silane mixed solution accounts for 7.5wt% of the nano-SiO2 / silicone rubber matrix.
[0033] Finally, gradient temperature curing and annealing are performed to obtain a thin-walled metal radiation layer with a sprayed silicon-based coating; the gradient temperature curing is as follows: the sprayed thin-walled metal radiation layer is placed in an oven, heated to 75℃ at a rate of 4℃ / min, kept for 32min, then heated to 115℃ at a rate of 3℃ / min, kept for 1.2h, and finally heated to 175℃ at a rate of 3℃ / min, kept for 2.2h; the annealing is as follows: after curing, the temperature is cooled to 58℃ in the oven, kept for 2.2h, and then reduced to room temperature at a rate of 0.5℃ / min.
[0034] Step S5, preparation of high-temperature-resistant thermal insulation layer: first, arrange 16 layers of aerogel thermal insulation materials from top to bottom (according to actual needs, the performance of the aerogel thermal insulation materials can be arranged in a decreasing order according to the direction of the heat source; that is, high-temperature section aerogel thermal insulation materials are placed near the heat source, and then medium-temperature section or low-temperature section aerogel thermal insulation materials are placed); then wrap the arranged 16 layers of aerogel thermal insulation materials with fiber cloth material; finally, connect and suture the wrapped material with high-temperature fiber suture line, and the suture method is V-shaped, to obtain a high-temperature-resistant thermal insulation layer.
[0035] Step S6, heat protection component preparation: place the high-temperature-resistant thermal insulation layer in step S5 on the side of the thin-walled metal radiation layer away from the silicon-based coating, and wrap the high-temperature-resistant thermal insulation layer by bending the side edges of the thin-walled metal radiation layer, and connect (adhere) the inner side (i.e. the side away from the silicon-based coating) of the thin-walled metal radiation layer to the high-temperature-resistant thermal insulation layer by pre-coating an adhesive (the adhesive can be silicone rubber).
[0036] Example 2: A high-temperature-resistant semi-flexible heat protection component, which comprises, from top to bottom, a silicon-based coating, a thin-walled metal radiation layer, and a high-temperature-resistant thermal insulation layer. The high-temperature-resistant thermal insulation layer is made of 7 layers of aerogel thermal insulation material, wrapped by a fiber cloth material, and finally stitched by high-temperature-resistant fiber stitching thread. The fiber cloth material is basalt fiber cloth, and the aerogel thermal insulation material is basalt fiber reinforced aerogel material. The thickness of the fiber cloth material is 0.15 mm, and the thickness of a single layer of aerogel material is 1.2 mm. The front surface of the thin-walled metal radiation layer corresponds to the high-temperature-resistant thermal insulation layer, and the outer circle of the thin-walled metal radiation layer is bent to wrap the side edges of the high-temperature-resistant thermal insulation layer. The thin-walled metal radiation layer is made of Ti foil and is sequentially subjected to plasma etching, anodic oxidation, and 3-isocyanate propyl trimethoxysilane soaking. The thickness of the thin-walled metal radiation layer is 0.1 mm. The thickness of the bent edge of the thin-walled metal radiation layer is higher than the thickness of the high-temperature-resistant thermal insulation layer, forming an air layer between the thin-walled metal radiation layer and the high-temperature-resistant thermal insulation layer. The thickness of the air layer is 0.7 mm. The outer circle of the thin-walled metal radiation layer is bent to wrap the side edges of the high-temperature-resistant thermal insulation layer, and the width protruding on the back surface of the high-temperature-resistant thermal insulation layer is 75 mm. The silicon-based coating is uniformly sprayed on the surface of the side of the thin-walled metal radiation layer away from the high-temperature-resistant thermal insulation layer. The silicon-based coating comprises a silicone rubber matrix, phenyl trimethoxysilane, KH560 (γ-glycidyl ether propyl trimethoxysilane), bismaleimide, and nano-SiO2 particles. The silicone rubber matrix is methyl phenyl silicone rubber with a phenyl content of 15%, and the particle size of the nano-SiO2 particles is 35 nm. The thickness of the silicon-based coating is 50 μm.
[0037] A method for preparing a high-temperature-resistant semi-flexible heat protection component, comprising: Step S1, thin-walled metal radiation layer pretreatment: first, ultrasonic cleaning the thin-walled metal radiation layer with anhydrous ethanol for 15 minutes, and then vacuum drying the cleaned thin-walled metal radiation layer at a temperature of 65°C for 1.5 hours to remove oil stains on the surface of the thin-walled metal radiation layer.
[0038] Then the treated thin-wall metal radiation layer is subjected to plasma etching and anodic oxidation. The plasma etching is performed by using argon with a power of 125 W, an argon flow rate of 20 sccm, a vacuum degree of 5 Pa, and an etching time of 6.5 min. The anodic oxidation is performed by using the thin-wall metal radiation layer after plasma etching as an anode, graphite as a cathode, and 0.5 mol / L sulfuric acid solution as an electrolyte under a direct current voltage of 10 V for 15 min.
[0039] In step S2, the silicon-based coating base liquid is prepared. First, the nano-SiO2 particles are dispersed in anhydrous toluene, and hydroxyl-terminated polymethylphenylsiloxane (molecular weight 5000-10000) is added. The mass-volume ratio of the nano-SiO2 particles, anhydrous toluene, and hydroxyl-terminated polymethylphenylsiloxane is 10 g:100 mL:5 g. The reflux reaction is carried out under nitrogen protection at a reflux reaction temperature of 80℃ for 4 hours. After centrifugal drying, the coated nano-SiO2 particles are first subjected to high-speed centrifugation at a speed of 9000 rpm for 17 minutes, and then placed in a vacuum drying oven at a temperature of 70℃ for 2.5 hours. The coated nano-SiO2 particles and KH560 are added to a high-pressure reaction kettle, and the silicon rubber matrix is injected. The mass ratio of the coated nano-SiO2 particles, KH560, and silicon rubber matrix is 5:0.25:50. After sealing, CO2 is introduced to the critical state, which is a temperature of 31.1℃ and a pressure of 7.38 MPa. The mixture is uniformly stirred for 30 minutes. After pressure relief, a uniformly dispersed nano-SiO2 / silicon rubber matrix is obtained.
[0040] In step S3, the thin-wall metal radiation layer is treated. The pretreated thin-wall metal radiation layer in step S1 is immersed in 3-isocyanate propyl trimethoxysilane, and left to stand at room temperature for 10 minutes. After taking out, it is dried at a temperature of 80℃ for 6 minutes.
[0041] In step S4, the silicon-based coating is sprayed. First, KH560 and phenyltrimethoxysilane are dissolved in deionized water containing acetic acid. The mass-volume ratio of KH560, phenyltrimethoxysilane, and deionized water containing acetic acid is 2 g:5 g:50 mL, and the acetic acid content is 0.1 wt%. The hydrolyzed silane mixture is formed by low-temperature stirring at a temperature of 4℃, a stirring rate of 135 rpm, and a stirring time of 1 hour.
[0042] After the nano-SiO2 / silicone rubber matrix, the hydrolyzed silane mixed solution and the bismaleimide (BMI) in step S2 are uniformly stirred, the mixture is sprayed on the surface of the thin-walled metal radiation layer in step S3, and a bottom layer is formed by pre-curing. The pre-curing temperature is 80°C, the pre-curing time is 10 minutes, and the thickness of the bottom layer is 15μm. The content of phenyltrimethoxysilane in the hydrolyzed silane mixed solution in the spraying liquid is adjusted, and the remaining components are the same as those in the bottom layer. The spraying liquid is sprayed onto the surface of the bottom layer, and a middle layer is formed by pre-curing. The pre-curing temperature is 80°C, the pre-curing time is 10 minutes, and the thickness of the middle layer is 20μm. The contents of phenyltrimethoxysilane and bismaleimide in the spraying liquid are adjusted, and the spraying liquid is sprayed onto the surface of the middle layer to form a surface layer by pre-curing. The pre-curing temperature is 80°C, the pre-curing time is 10 minutes, and the thickness of the surface layer is 15μm. The content of phenyltrimethoxysilane in the bottom layer, the middle layer and the surface layer increases in turn, and the content of bismaleimide in the surface layer is lower than that in the bottom layer. Specifically, in the bottom layer, the mass ratio of nano-SiO2 / silicone rubber matrix to bismaleimide is 100:0.5, and the content of phenyltrimethoxysilane in the hydrolyzed silane mixed solution accounts for 3wt% of the nano-SiO2 / silicone rubber matrix. In the middle layer, the mass ratio of nano-SiO2 / silicone rubber matrix to bismaleimide is 100:0.5, and the content of phenyltrimethoxysilane in the hydrolyzed silane mixed solution accounts for 5wt% of the nano-SiO2 / silicone rubber matrix. In the surface layer, the mass ratio of nano-SiO2 / silicone rubber matrix to bismaleimide is 100:0.3, and the content of phenyltrimethoxysilane in the hydrolyzed silane mixed solution accounts for 8wt% of the nano-SiO2 / silicone rubber matrix.
[0043] Finally, gradient temperature curing and annealing are performed to obtain a thin-walled metal radiation layer with a sprayed silicon-based coating. The gradient temperature curing is as follows: the sprayed thin-walled metal radiation layer is placed in an oven, heated to 80°C at a rate of 5°C / min, kept for 30 minutes, then heated to 120°C at a rate of 3.5°C / min, kept for 1 hour, and finally heated to 180°C at a rate of 3.5°C / min, kept for 2 hours. The annealing is as follows: after curing, the temperature is cooled to 60°C in the furnace, kept for 2 hours, and then reduced to room temperature at a rate of 0.7°C / min.
[0044] In step S5, the high-temperature-resistant thermal insulation layer is prepared as follows: first, arrange the 7 layers of aerogel thermal insulation materials from top to bottom, then wrap the arranged 7 layers of aerogel thermal insulation materials with fiber cloth material, and finally connect and suture the wrapped material with high-temperature-resistant fiber suture line in a V-shaped manner to obtain the high-temperature-resistant thermal insulation layer.
[0045] Step S6, heat protection component preparation: place the high-temperature-resistant thermal insulation layer in step S5 on the side of the thin-walled metal radiation layer away from the silicon-based coating, and wrap the high-temperature-resistant thermal insulation layer by bending the side edges of the thin-walled metal radiation layer, and connect (adhere) the inner side (i.e. the side away from the silicon-based coating) of the thin-walled metal radiation layer to the high-temperature-resistant thermal insulation layer by pre-coating an adhesive (the adhesive can be silicone rubber).
[0046] Example 3: A high-temperature-resistant semi-flexible heat protection component, which comprises, from top to bottom, a silicon-based coating, a thin-walled metal radiation layer, and a high-temperature-resistant thermal insulation layer. The high-temperature-resistant thermal insulation layer is made of 5 layers of aerogel thermal insulation material, wrapped by a fiber cloth material, and finally stitched by high-temperature-resistant fiber stitching thread. The fiber cloth material is glass fiber cloth, and the aerogel thermal insulation material is glass fiber reinforced aerogel material. The thickness of the fiber cloth material is 0.2 mm, and the thickness of a single layer of aerogel material is 2 mm. The front surface of the thin-walled metal radiation layer corresponds to the high-temperature-resistant thermal insulation layer, and the outer circle of the thin-walled metal radiation layer is bent to wrap the side edges of the high-temperature-resistant thermal insulation layer. The thin-walled metal radiation layer is made of Ti foil and is sequentially subjected to plasma etching, anodic oxidation, and 3-isocyanate propyl trimethoxysilane soaking. The thickness of the thin-walled metal radiation layer is 0.15 mm. The thickness of the bent edge of the thin-walled metal radiation layer is higher than the thickness of the high-temperature-resistant thermal insulation layer, forming an air layer between the thin-walled metal radiation layer and the high-temperature-resistant thermal insulation layer. The thickness of the air layer is 1 mm. The outer circle of the thin-walled metal radiation layer is bent to wrap the side edges of the high-temperature-resistant thermal insulation layer, and the width protruding on the back of the high-temperature-resistant thermal insulation layer is 100 mm. The silicon-based coating is uniformly sprayed on the surface of the side of the thin-walled metal radiation layer away from the high-temperature-resistant thermal insulation layer. The silicon-based coating includes a silicone rubber matrix, phenyltrimethoxysilane, KH560 (γ-glycidyl ether propyltrimethoxysilane), bismaleimide, and nano-SiO2 particles. The silicone rubber matrix is methylphenyl silicone rubber with a phenyl content of 15%, and the particle size of the nano-SiO2 particles is 50 nm. The thickness of the silicon-based coating is 70 μm.
[0047] A method for preparing a high-temperature-resistant semi-flexible heat protection component, comprising: Step S1, thin-walled metal radiation layer pretreatment: first clean the thin-walled metal radiation layer with anhydrous ethanol for 17 minutes, and then vacuum dry the cleaned thin-walled metal radiation layer at a temperature of 70°C for 1.3 hours to remove oil stains on the surface of the thin-walled metal radiation layer.
[0048] Then, the treated thin-wall metal radiation layer is subjected to plasma etching and anodic oxidation. The plasma etching is performed by using argon with a power of 150 W, an argon flow rate of 22 sccm, a vacuum degree of 5.5 Pa, and an etching time of 5 min. The anodic oxidation is performed by using the thin-wall metal radiation layer after plasma etching as an anode, graphite as a cathode, and 0.5 mol / L sulfuric acid solution as an electrolyte under a direct current voltage of 11 V for 12 min.
[0049] In step S2, the silicon-based coating base liquid is prepared. First, the nano-SiO2 particles are dispersed in anhydrous toluene, and hydroxyl-terminated polymethylphenylsiloxane (molecular weight 5000-10000) is added. The mass-volume ratio of the nano-SiO2 particles, anhydrous toluene, and hydroxyl-terminated polymethylphenylsiloxane is 10.5 g:105 mL:5.5 g. The backflow reaction is carried out under nitrogen protection at a backflow reaction temperature of 85℃ for 3.5 h. After centrifugal drying, the coated nano-SiO2 particles are first subjected to high-speed centrifugation at a speed of 10000 rpm for 15 min, and then placed in a vacuum drying oven at a temperature of 80℃ for 2 h. The coated nano-SiO2 particles and KH560 are added to a high-pressure reaction kettle, and the silicon rubber matrix is injected. The mass ratio of the coated nano-SiO2 particles, KH560, and silicon rubber matrix is 5.5:0.3:52. After sealing, CO2 is introduced to the critical state, i.e., a temperature of 31.1℃ and a pressure of 7.38 MPa. The mixture is uniformly stirred for 32 min, and then depressurized to obtain a uniformly dispersed nano-SiO2 / silicon rubber matrix.
[0050] In step S3, the thin-wall metal radiation layer is treated. The pretreated thin-wall metal radiation layer in step S1 is immersed in 3-isocyanate propyl trimethoxysilane, and then left to stand at room temperature for 12 min. After taking out, the thin-wall metal radiation layer is dried at a drying temperature of 85℃ for 5 min.
[0051] In step S4, the silicon-based coating is sprayed. First, KH560 and phenyltrimethoxysilane are dissolved in deionized water containing acetic acid. The mass-volume ratio of KH560, phenyltrimethoxysilane, and deionized water containing acetic acid is 2.2 g:5.2 g:52 mL, and the acetic acid content is 0.12 wt%. The hydrolyzed silane mixture is formed by low-temperature stirring at a low-temperature stirring temperature of 5℃, a stirring speed of 150 rpm, and a stirring time of 0.8 h.
[0052] After the nano-SiO2 / silicone rubber matrix, the hydrolyzed silane mixed solution in step S2 and the bismaleimide (BMI) are uniformly stirred, the mixture is sprayed on the surface of the thin-walled metal radiation layer in step S3, and a bottom layer is formed after pre-curing. The pre-curing temperature is 85°C, the pre-curing time is 8min, and the thickness of the bottom layer is 20μm. The content of phenyltrimethoxysilane in the hydrolyzed silane mixed solution in the spraying liquid is adjusted, and the remaining components are the same as those in the bottom layer. The spraying liquid is sprayed onto the surface of the bottom layer, and a middle layer is formed after pre-curing. The pre-curing temperature is 85°C, the pre-curing time is 8min, and the thickness of the middle layer is 30μm. The content of phenyltrimethoxysilane and bismaleimide in the hydrolyzed silane mixed solution in the spraying liquid is adjusted, and the spraying liquid is sprayed onto the surface of the middle layer to form a surface layer after pre-curing. The pre-curing temperature is 85°C, the pre-curing time is 8min, and the thickness of the surface layer is 20μm. The content of phenyltrimethoxysilane in the bottom layer, the middle layer and the surface layer increases in turn, and the content of bismaleimide in the surface layer is lower than that in the bottom layer. Specifically, in the bottom layer, the mass ratio of nano-SiO2 / silicone rubber matrix to bismaleimide is 100:0.55, and the content of phenyltrimethoxysilane in the hydrolyzed silane mixed solution accounts for 3.5wt% of the nano-SiO2 / silicone rubber matrix. In the middle layer, the mass ratio of nano-SiO2 / silicone rubber matrix to bismaleimide is 100:0.55, and the content of phenyltrimethoxysilane in the hydrolyzed silane mixed solution accounts for 5.5wt% of the nano-SiO2 / silicone rubber matrix. In the surface layer, the mass ratio of nano-SiO2 / silicone rubber matrix to bismaleimide is 100:0.35, and the content of phenyltrimethoxysilane in the hydrolyzed silane mixed solution accounts for 8.5wt% of the nano-SiO2 / silicone rubber matrix.
[0053] Finally, gradient temperature curing and annealing are performed to obtain a thin-walled metal radiation layer with a sprayed silicon-based coating. The gradient temperature curing is as follows: the sprayed thin-walled metal radiation layer is placed in an oven, heated to 85°C at a rate of 6°C / min, kept for 28min, then heated to 125°C at a rate of 4°C / min, kept for 0.8h, and finally heated to 185°C at a rate of 4°C / min, kept for 1.8h. The annealing is as follows: after curing, the temperature is cooled to 62°C in the oven, kept for 1.8h, and then reduced to room temperature at a rate of 1°C / min.
[0054] In step S5, the high-temperature-resistant thermal insulation layer is prepared as follows: first, arrange 5 layers of aerogel thermal insulation materials from top to bottom (according to actual needs, the performance of the aerogel thermal insulation materials can be arranged in order of decreasing temperature according to the direction of the heat source; that is, place the high-temperature section aerogel thermal insulation materials near the heat source, and then place the medium-temperature section or low-temperature section aerogel thermal insulation materials); then wrap the arranged 5 layers of aerogel thermal insulation materials with fiber cloth material; finally, connect and suture the wrapped material with high-temperature fiber suture, and the suture method is V-shaped, to obtain a high-temperature-resistant thermal insulation layer.
[0055] Step S6, heat protection member preparation: place the high-temperature-resistant thermal insulation layer in step S5 on the side of the thin-walled metal radiation layer away from the silicon-based coating, and realize the wrapping of the high-temperature-resistant thermal insulation layer through the thin-walled metal radiation layer side bending, and realize the connection (adhesive can use silicone rubber) of the inside of the thin-walled metal radiation layer (i.e. the side away from the silicon-based coating) and the high-temperature-resistant thermal insulation layer through pre-coating adhesive.
[0056] Comparative Example 1: A high-temperature-resistant semi-flexible heat protection member, which comprises a silicon-based coating, a thin-walled metal radiation layer and a high-temperature-resistant thermal insulation layer from top to bottom, the high-temperature-resistant thermal insulation layer is made of 7 layers of aerogel thermal insulation material and is wrapped by fiber cloth material, and finally is sewn by high-temperature fiber suture; the fiber cloth material uses basalt fiber cloth, the aerogel thermal insulation material uses basalt fiber reinforced aerogel material; the thickness of the fiber cloth material is 0.15 mm, and the thickness of the single-layer aerogel material is 1.2 mm. The front surface of the thin-walled metal radiation layer corresponds to the high-temperature-resistant thermal insulation layer, and the outer circle is respectively bent to wrap the side edge of the high-temperature-resistant thermal insulation layer, the thin-walled metal radiation layer uses Ti foil and is sequentially subjected to plasma etching and anodic oxidation; the thickness of the thin-walled metal radiation layer is 0.1 mm. The thickness of the bent edge of the thin-walled metal radiation layer is higher than the thickness of the high-temperature-resistant thermal insulation layer, and an air layer is formed between the thin-walled metal radiation layer and the high-temperature-resistant thermal insulation layer; the thickness of the air layer is 0.7 mm; the outer circle of the thin-walled metal radiation layer is bent to wrap the side edge of the high-temperature-resistant thermal insulation layer, and the width protruding on the back surface of the high-temperature-resistant thermal insulation layer is 75 mm. The silicon-based coating is uniformly sprayed on the surface of the side of the thin-walled metal radiation layer away from the high-temperature-resistant thermal insulation layer, and the silicon-based coating comprises a silicone rubber matrix, a phenyl trimethoxysilane, a KH560 (γ-glycidyl ether propyl trimethoxysilane), a bismaleimide and a nano-SiO2 particle, the silicone rubber matrix uses methyl phenyl silicone rubber with a phenyl content of 15%, and the particle size of the nano-SiO2 particle is 35 nm; the thickness of the silicon-based coating is 50 μm.
[0057] The preparation method thereof is described in Example 2.
[0058] Comparative Example 2: The application discloses a high-temperature-resistant semi-flexible thermal protection component, which comprises, from top to bottom, a silicon-based coating, a thin-wall metal radiation layer and a high-temperature-resistant thermal insulation layer. The high-temperature-resistant thermal insulation layer is made of seven layers of aerogel thermal insulation materials, wrapped by fiber cloth materials and finally sutured by high-temperature fiber suture. The fiber cloth material is basalt fiber cloth, and the aerogel thermal insulation material is basalt fiber reinforced aerogel material. The thickness of the fiber cloth material is 0.15 mm, and the thickness of the single-layer aerogel material is 1.2 mm. The front surface of the thin-wall metal radiation layer corresponds to the high-temperature-resistant thermal insulation layer, and the outer circle of the thin-wall metal radiation layer is bent to wrap the side edges of the high-temperature-resistant thermal insulation layer. The thin-wall metal radiation layer is made of Ti foil and is sequentially subjected to plasma etching, anodic oxidation and 3-isocyanate propyl trimethoxysilane soaking. The thickness of the thin-wall metal radiation layer is 0.1 mm. The thickness of the bent edge of the thin-wall metal radiation layer is higher than the thickness of the high-temperature-resistant thermal insulation layer, and an air interlayer is formed between the thin-wall metal radiation layer and the high-temperature-resistant thermal insulation layer. The thickness of the air interlayer is 0.7 mm. The outer circle of the thin-wall metal radiation layer is bent to wrap the side edges of the high-temperature-resistant thermal insulation layer, and the width of the protrusion on the back surface of the high-temperature-resistant thermal insulation layer is 75 mm. The silicon-based coating is uniformly sprayed on the surface of the thin-wall metal radiation layer away from the high-temperature-resistant thermal insulation layer. The silicon-based coating comprises a silicone rubber matrix, KH560 (γ-glycidyl ether propyl trimethoxysilane), bismaleimide and nano-SiO2 particles. The silicone rubber matrix is methylphenyl silicone rubber with a phenyl content of 15%, and the particle size of the nano-SiO2 particles is 35 nm. The thickness of the silicon-based coating is 50 μm.
[0059] The preparation method is shown in Example 2.
[0060] Comparative Example 3 The application discloses a high-temperature-resistant semi-flexible thermal protection component, which comprises, from top to bottom, a silicon-based coating, a thin-wall metal radiation layer and a high-temperature-resistant heat insulation layer. The high-temperature-resistant heat insulation layer is made of seven layers of aerogel heat insulation materials, wrapped by fiber cloth materials and finally sutured by high-temperature fiber suture. The fiber cloth material is basalt fiber cloth, and the aerogel heat insulation material is basalt fiber reinforced aerogel material. The thickness of the fiber cloth material is 0.15 mm, and the thickness of the single-layer aerogel material is 1.2 mm. The front surface of the thin-wall metal radiation layer corresponds to the high-temperature-resistant heat insulation layer, and the outer circle of the thin-wall metal radiation layer is bent to wrap the side edges of the high-temperature-resistant heat insulation layer. The thin-wall metal radiation layer is made of Ti foil and is sequentially subjected to plasma etching, anodic oxidation and 3-isocyanate propyl trimethoxysilane soaking. The thickness of the thin-wall metal radiation layer is 0.1 mm. The thickness of the bent edge of the thin-wall metal radiation layer is higher than the thickness of the high-temperature-resistant heat insulation layer, and an air interlayer is formed between the thin-wall metal radiation layer and the high-temperature-resistant heat insulation layer. The thickness of the air interlayer is 0.7 mm. The outer circle of the thin-wall metal radiation layer is bent to wrap the side edges of the high-temperature-resistant heat insulation layer, and the width of the protrusion on the back surface of the high-temperature-resistant heat insulation layer is 75 mm. The silicon-based coating is uniformly sprayed on the surface of the thin-wall metal radiation layer away from the high-temperature-resistant heat insulation layer. The silicon-based coating comprises a silicone rubber matrix, phenyl trimethoxysilane, bismaleimide and nano-SiO2 particles. The silicone rubber matrix is methyl phenyl silicone rubber with a phenyl content of 15%, and the particle size of the nano-SiO2 particles is 35 nm. The thickness of the silicon-based coating is 50 microns.
[0061] The preparation method is shown in Example 2.
[0062] Comparative Example 4: A kind of high-temperature-resistant semi-flexible heat protection component, including silicon-based coating, thin-wall metal radiation layer and high-temperature-resistant heat insulation layer from top to bottom in turn, high-temperature-resistant heat insulation layer is by 7 layers of aerogel heat insulation material paving, and by fiber cloth material is wrapped, finally by high-temperature fiber suture line is stitched together;Fiber cloth material uses basalt fiber cloth, aerogel heat insulation material uses basalt fiber reinforced aerogel material;Fiber cloth material thickness is 0.15mm, the thickness of single-layer aerogel material is 1.2mm.Thin-wall metal radiation layer front and high-temperature-resistant heat insulation layer correspond, its outer circle is bent to the side edge of high-temperature-resistant heat insulation layer and is wrapped, thin-wall metal radiation layer uses Ti foil, and successively passes through plasma etching, anodic oxidation and 3-isocyanate propyl trimethoxysilane soaking;Thin-wall metal radiation layer thickness is 0.1mm.Thin-wall metal radiation layer bending edge thickness is higher than the thickness of high-temperature-resistant heat insulation layer, in thin-wall metal radiation layer and high-temperature-resistant heat insulation layer form air interlayer;Air interlayer thickness is 0.7mm;Thin-wall metal radiation layer outer circle is bent and wrapped high-temperature-resistant heat insulation layer side edge, in high-temperature-resistant heat insulation layer back protruding width is 75mm.Silicon-based coating is uniformly sprayed in the surface of thin-wall metal radiation layer side away from high-temperature-resistant heat insulation layer, and silicon-based coating includes silicone rubber matrix, phenyl trimethoxysilane, KH560 (γ-glycidyl ether oxypropyl trimethoxysilane) and bismaleimide, and silicone rubber matrix uses methyl phenyl silicone rubber, and phenyl content is 15%;Silicon-based coating thickness is 50 μm.
[0063] Its preparation method is described in example 2.
[0064] Comparative example 5: A kind of high-temperature-resistant semi-flexible heat protection component, by upper to lower, it includes silicon-based coating, thin-wall metal radiation layer and high-temperature-resistant heat insulation layer in turn, high-temperature-resistant heat insulation layer is by 7 layers aerogel heat insulation material paving, and by fiber cloth material package, finally by high-temperature fiber suture line suture is formed;Fiber cloth material uses basalt fiber cloth, aerogel heat insulation material uses basalt fiber reinforced aerogel material;Fiber cloth material thickness is 0.15mm, the thickness of single layer aerogel material is 1.2mm.Thin-wall metal radiation layer front and high-temperature-resistant heat insulation layer correspond, its outer circle is bent to the side of high-temperature-resistant heat insulation layer and is wrapped, thin-wall metal radiation layer uses Ti foil, and successively passes through plasma etching, anodic oxidation and 3-isocyanate propyl trimethoxysilane soaking;Thin-wall metal radiation layer thickness is 0.1mm.Thin-wall metal radiation layer bending edge thickness is higher than the thickness of high-temperature-resistant heat insulation layer, air interlayer is formed in thin-wall metal radiation layer and high-temperature-resistant heat insulation layer;The thickness of air interlayer is 0.7mm;Thin-wall metal radiation layer outer circle bending wraps the side of high-temperature-resistant heat insulation layer, and the width protruding on the back of high-temperature-resistant heat insulation layer is 75mm.Silicon-based coating is uniformly sprayed on the surface of the side of thin-wall metal radiation layer away from high-temperature-resistant heat insulation layer, and silicon-based coating includes silicone rubber matrix, phenyl trimethoxysilane, KH560 (γ-glycidyl ether propyl trimethoxysilane) and nano-SiO2 particles, silicone rubber matrix uses methyl phenyl silicone rubber, and the phenyl content is 15%, and the particle size of nano-SiO2 particles is 35nm;Silicon-based coating thickness is 50 μm.
[0065] Its preparation method is described in Example 2.
[0066] The heat protection components prepared in Example 1-Example 3, Comparative Example 1-Comparative Example 5 are respectively tested for heat insulation performance and multiple bending test (continuous bending for 10 times), and the test results are as follows:
[0067] As shown in the above table: the heat protection component prepared by the means of the application has excellent heat insulation performance, and the bonding strength between the silicon-based coating and the thin-wall metal radiation layer is high, and the conformability is good, and after multiple bending, it can still have excellent heat insulation performance, and will not have problems such as cracks and peeling.
Claims
1. A high temperature resistant semi-flexible heat protection component, characterized by: From top to bottom, it includes a silicon-based coating, a thin-walled metal radiation layer and a high-temperature resistant thermal insulation layer. The high-temperature resistant thermal insulation layer is stacked by multiple layers of aerogel insulation material, wrapped by fiber cloth material, and finally sewn by high-temperature fiber sutures; the front of the thin-walled metal radiation layer corresponds to the high-temperature resistant thermal insulation layer, and its outer circle is bent to wrap the side of the high-temperature resistant thermal insulation layer. The thickness of the bent edge of the thin-walled metal radiation layer is higher than the thickness of the high-temperature resistant thermal insulation layer, and an air interlayer is formed between the thin-walled metal radiation layer and the high-temperature resistant thermal insulation layer; the silicon-based coating is evenly sprayed on the surface of the thin-walled metal radiation layer away from the high-temperature resistant thermal insulation layer.
2. The high temperature resistant semi-flexible heat protection component according to claim 1, characterized in that: The silicon-based coating comprises a silicone rubber matrix, phenyltrimethoxysilane, KH560, bismaleimide and nano-SiO2 particles. The silicone rubber matrix adopts methylphenyl silicone rubber with a phenyl content of 15%. The particle size of the nano-SiO2 particles is 20-50nm. The thickness of the silicone-based coating is 30-70μm.
3. A high temperature resistant semi-flexible heat protection component according to claim 1 or 2, characterized in that: The thin-walled metal radiation layer is made of Ti foil and is sequentially subjected to plasma etching, anodization and immersion in 3-isocyanatepropyltrimethoxysilane; the thickness of the thin-walled metal radiation layer is 0.05-0.15 mm.
4. A high temperature resistant semi-flexible heat protection component according to claim 2 or 3, characterized in that: The thickness of the air interlayer is 0.5-1 mm; the outer circle of the thin-walled metal radiation layer is bent and wrapped around the side of the high-temperature resistant heat insulation layer, and the width of the protrusion on the back of the high-temperature resistant heat insulation layer is 50-100 mm.
5. A high temperature resistant semi-flexible heat protection component according to claim 2 or 3, characterized in that: The fiber cloth material is one of basalt fiber cloth and glass fiber cloth, and the aerogel insulation material is at least one of glass fiber reinforced aerogel material, basalt fiber reinforced aerogel material, and alumina fiber reinforced aerogel material; the fiber cloth material has a thickness of 0.1 to 0.2 mm, and the thickness of the single-layer aerogel material is 0.5 to 2 mm.
6. The method for preparing a high-temperature resistant semi-flexible heat protection component according to any one of claims 3 to 5, characterized in that: include: Step S1, pre-treatment of the thin-walled metal radiation layer: first, the thin-walled metal radiation layer is cleaned and vacuum-dried to remove oil stains on the surface of the thin-walled metal radiation layer; Then, the processed thin-walled metal radiation layer is subjected to plasma etching and anodization in sequence; Step S2, preparation of silicon-based coating base liquid: first, disperse nano-SiO2 particles in anhydrous toluene, and add terminal hydroxyl polymethylphenylsiloxane, and perform reflux reaction under nitrogen protection. After centrifugal drying, add the coated nano-SiO2 particles and KH560 into an autoclave, and inject the silicone rubber matrix. After sealing, introduce CO2 to a critical state, stir evenly, and release the pressure to obtain a uniformly dispersed nano-SiO2 / silicone rubber matrix; Step S3, thin-walled metal radiation layer treatment: immerse the thin-walled metal radiation layer pretreated in step S1 in 3-isocyanatepropyltrimethoxysilane, let it stand for a period of time at room temperature, take it out and then dry it; Step S4, spraying a silicon-based coating: first, dissolving KH560 and phenyltrimethoxysilane in deionized water containing acetic acid, stirring at low temperature to form a hydrolyzed silane mixture; taking the nano-SiO2 / silicone rubber matrix, the hydrolyzed silane mixture and bismaleimide in step S2, uniformly stirring, spraying them on the surface of the thin-walled metal radiation layer in step S3, and pre-curing to form a bottom layer; adjusting the phenyltrimethoxysilane content of the hydrolyzed silane mixture in the spraying liquid, and the remaining components are the same as those in the bottom layer, spraying them on the surface of the bottom layer, and pre-curing to form a middle layer; adjusting the phenyltrimethoxysilane and bismaleimide contents of the hydrolyzed silane mixture in the spraying liquid, spraying them on the surface of the middle layer, and pre-curing to form a surface layer; finally, performing gradient temperature curing and annealing to obtain a thin-walled metal radiation layer sprayed with a silicon-based coating; Step S5, preparing a high-temperature resistant thermal insulation layer: first, arranging multiple layers of aerogel thermal insulation material from top to bottom, then wrapping the arranged multiple layers of aerogel thermal insulation material with fiber cloth material, and finally connecting the wrapped materials with high-temperature fiber sutures in a V-shaped suture pattern to obtain a high-temperature resistant thermal insulation layer; Step S6, preparation of heat protection components: Place the high-temperature resistant insulation layer in step S5 on the side of the thin-walled metal radiation layer away from the silicon-based coating, and achieve the covering of the high-temperature resistant insulation layer by bending the side of the thin-walled metal radiation layer. The inner side of the thin-walled metal radiation layer is pre-coated with an adhesive to achieve its connection with the high-temperature resistant insulation layer.
7. The method for preparing a high-temperature resistant semi-flexible heat protection component according to claim 6, characterized in that: The cleaning in step S1 specifically includes: ultrasonic cleaning with anhydrous ethanol for 13 to 17 minutes; and vacuum drying at a temperature of 60 to 70° C. for 1.3 to 1.7 hours.
8. The method for preparing a high-temperature resistant semi-flexible heat protection component according to claim 6, characterized in that: The plasma etching in step S1 is specifically as follows: argon gas is used for plasma etching, with a power of 100-150 W, an argon gas flow rate of 18-22 sccm, a vacuum degree of 4.5-5.5 Pa, and an etching time of 5-8 min; the anodization is specifically as follows: the thin-walled metal radiation layer after plasma etching is used as the anode and graphite is used as the cathode, a 0.5 mol / L sulfuric acid solution is used as the electrolyte, and oxidation is carried out at a DC voltage of 9-11 V for 12-18 min.
9. The method for preparing a high-temperature resistant semi-flexible heat protection component according to claim 6, characterized in that: In step S3, the standing time is 8 to 12 minutes, the drying temperature is 75 to 85° C., and the drying time is 5 to 7 minutes.
10. The method for preparing a high-temperature resistant semi-flexible heat protection component according to claim 6, characterized in that: The gradient temperature curing in step S4 is specifically as follows: placing the sprayed thin-walled metal radiation layer in an oven, heating it to 75-85°C at a rate of 4-6°C / min, keeping it warm for 28-32 minutes, then heating it to 115-125°C at a rate of 3-4°C / min, keeping it warm for 0.8-1.2 hours, and finally heating it to 175-185°C at a rate of 3-4°C / min, keeping it warm for 1.8-2.2 hours; annealing is specifically as follows: after curing, cooling it to 58-62°C along with the furnace temperature, keeping it warm for 1.8-2.2 hours, and then cooling it to room temperature at a rate of 0.5-1°C / min.