CN107459359B - Silica-based light ceramic thermal protection material and preparation method and application thereof - Google Patents
Silica-based light ceramic thermal protection material and preparation method and application thereof Download PDFInfo
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Abstract
the invention relates to a silica-based lightweight ceramic thermal protection material and a preparation method and application thereof. The thermal protection material takes a rigid heat insulation tile as a base body, is compounded with Si-O-C aerogel, and the surface of the thermal protection material is coated with a strengthening coating. The preparation method comprises the following steps: preparing a rigid heat insulation tile matrix and a Si-O-C sol precursor, soaking the rigid heat insulation tile matrix with the Si-O-C sol precursor, sequentially aging, solvent replacement and supercritical drying to obtain a rigid heat insulation tile base Si-O-C aerogel composite material, and coating a surface strengthening coating on the outer surface of the rigid heat insulation tile base Si-O-C aerogel composite material to obtain the silica-based lightweight ceramic thermal protection material. The material prepared by the invention has the characteristics of low density, high compressive strength, low ablation rate, low thermal conductivity, high emissivity, good heat insulation effect, excellent airflow scouring resistance and the like, and can be used as an outer surface thermal protection material of an outer space exploration aircraft.
Description
Technical Field
The invention relates to the technical field of functional composite materials, in particular to a silica-based lightweight ceramic thermal protection ablation material and a preparation method and application thereof.
Background
When an interplanetary aircraft such as a Mars probe enters the extraterrestrial planetary atmosphere at a high speed and then enters the earth atmosphere from the extraterrestrial space, severe pneumatic heating can be generated due to extremely high speed, so that thermal protection measures must be implemented on the outer surface of the aircraft. The weight of the aircraft determines the thrust requirements of the required launch vehicle and thus the feasibility of the project. Therefore, it is critical to the engineering realization to reduce the weight of the outer surface thermal protection system of the remote interplanetary exploration aircraft.
The early high-density ablative thermal protection materials such as polytetrafluoroethylene, three-dimensional quartz fabric/phenolic aldehyde composite materials, carbon-phenolic aldehyde composite materials and the like are used for an ablative thermal protection system of a high-speed ballistic missile, the carbon-phenolic aldehyde composite materials, advanced carbon-carbon composite materials and the like can be used for not only the thermal protection of a ballistic missile, but also the ablative thermal protection system of a near-earth orbit reentry aircraft, the density of the materials is more than or equal to 1.0g/cm 3, two medium-density ablative thermal protection materials with the density within the range of 0.4-1.0 g/cm 3 are developed in the Arbourdon-moon project in the United states, the densities of the AVCOAT-5026 and SLA-561V are both about 0.6g/cm 3 after multiple actual check on the flying in the US lunge project and the Mars detection project, the COAT-5026 material is actually a honeycomb reinforced resin composite material with a surface compounded with a thermal control coating, and the AVCOAT is similar to the heat protection material used in the atmospheric layer of the China again.
The density of the two types of light ablative materials is about 0.27g/cm 3. the PICA and the SIRCA are subjected to multiple actual flight engineering tests in the detection process of American mars, the existing airship and returnable cabin bottom surface ablative heat protection materials of space exploration companies are PICA materials, the American patent No. 5536562 discloses a type of quartz fiber impregnated with organic resin with the density ranging from 0.15 g/cm 3, but the light ablative heat protection material prepared by the aerogel serving as a substrate has the density ranging from 0.27g/cm 3, and the air flow resistance performance of the quartz fiber impregnated with organic resin is not enough in the range of 3, the density of the aerogel impregnated with the SIRCA prepared by the aerogel serving as a substrate is 0.27-0.82 g/cm 3, and the air flow resistance performance of the aerogel impregnated with the silica fiber prepared by a vacuum impregnation method and a low-alkaline silicone-based aerogel impregnation process is not enough to obtain a low-compressive strength composite material with a low-compressive strength of Si-C and a low-compressive strength of aerogel impregnated with a silica-alumina sol, which is prepared by a low-alumina sol-alumina sol-alumina sol-alumina-silica-alumina-silica gel-silica-alumina-silica gel-alumina-silica.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides the silica-based light ceramic thermal protection material with low density, high compressive strength, low ablation rate, low thermal conductivity, high emissivity, good thermal insulation effect and excellent airflow scouring resistance, and the preparation method and the application thereof.
The invention provides a silica-based lightweight ceramic thermal protection material in a first aspect, which comprises a rigid heat-insulating tile-based Si-O-C aerogel composite material and a surface strengthening coating formed on the outer surface of the rigid heat-insulating tile-based Si-O-C aerogel composite material; the rigid heat insulation tile base Si-O-C aerogel composite material comprises a rigid heat insulation tile base body and Si-O-C aerogel compounded in the rigid heat insulation tile base body.
Preferably, the rigid heat insulation tile base body is composed of 1-5% of boron oxide by mass, 50-99% of quartz fiber by mass and 0-49% of fiber reinforcement by mass.
Preferably, the fibers in the fiber reinforcement are selected from the group consisting of alumina fibers, mullite fibers, aluminosilicate fibers, zirconia fibers, and yttrium aluminum garnet fibers.
Preferably, the surface enhancing coating comprises a room temperature curing silicone and a high emissivity filler.
Preferably, the high emissivity filler is selected from the group consisting of glass frit, silicon tetraboride, silicon hexaboride, boron carbide, zirconium carbide, silicon carbide, hafnium carbide, molybdenum disilicide, and tantalum disilicide.
The invention provides a preparation method of a silica-based lightweight ceramic thermal protection material in a second aspect, which comprises the following steps:
(1) preparing a rigid heat insulation tile base body: uniformly mixing 1-5% by mass of boron nitride, 50-99% by mass of quartz fiber and 0-49% by mass of fiber reinforcement with water, filtering to obtain a solid mixture, drying and sintering the solid mixture to obtain a rigid heat insulation tile substrate;
(2) Preparation of a Si-O-C sol precursor: uniformly mixing alkoxy silane with an alcohol solvent, and preparing a Si-O-C sol precursor by taking an acidic reagent as a catalyst;
(3) Dipping the rigid heat insulation tile matrix prepared in the step (1) by using the Si-O-C sol precursor prepared in the step (2), standing to enable the Si-O-C sol precursor to be gelled to prepare a rigid heat insulation tile base Si-O-C wet gel composite material, and sequentially aging, solvent replacing and drying the rigid heat insulation tile base Si-O-C wet gel composite material to prepare a rigid heat insulation tile base Si-O-C aerogel composite material;
(4) Preparing a surface strengthening coating: preparing a surface strengthening coating containing room temperature curing silicone resin, a catalyst, a cross-linking agent, a dispersion medium and high-emissivity fillers, and coating the surface strengthening coating on the outer surface of the rigid heat-insulation tile-based Si-O-C aerogel composite material prepared in the step (3) to form a surface strengthening coating, so as to obtain the silica-based lightweight ceramic thermal protection material.
Preferably, the alkoxy silane in the step (2) consists of methyltrimethoxy silane and dimethyldimethoxy silane, and the mass ratio of the methyltrimethoxy silane to the dimethyldimethoxy silane is (200-300): 50-75).
Preferably, the alcohol solvent in step (2) is preferably absolute ethanol; the acidic reagent in step (2) is selected from the group consisting of nitric acid, hydrochloric acid and sulfuric acid; vacuum impregnation is adopted in the impregnation in the step (3); the solvent replacement in the step (3) is carried out in an alcohol solvent, preferably absolute ethyl alcohol; the drying in the step (3) is supercritical drying, preferably supercritical carbon dioxide drying; in the step (4), the catalyst is dibutyltin dilaurate; the cross-linking agent in the step (4) is tetraethoxysilane; and/or the dispersion medium in step (4) is selected from the group consisting of toluene, o-xylene, p-xylene, m-xylene, and acetone.
The present invention provides, in a third aspect, a silica-based lightweight ceramic heat shield member made of the silica-based lightweight ceramic heat shield material provided in the first aspect of the present invention or the silica-based lightweight ceramic heat shield material produced by the production method provided in the second aspect of the present invention.
The present invention provides, in a fourth aspect, the silica-based lightweight ceramic thermal protection material provided in the first aspect of the invention or the silica-based lightweight ceramic thermal protection material prepared by the preparation method provided in the second aspect of the invention and the use of the silica-based lightweight ceramic thermal protection member provided in the third aspect of the invention in a thermal protection material for an exterior surface of an aircraft.
Compared with the prior art, the invention at least has the following beneficial effects:
1. The density of the silica-based lightweight ceramic thermal protection material prepared by the invention is as low as 0.20-0.25 g/cm 3, the compressive strength is as high as 1.0-1.5 MPa, and the thermal protection system on the outer surface of the remote interplanetary exploration aircraft can meet the requirements of density and strength at the same time.
2. The Si-O-C aerogel prepared by the invention is uniformly dispersed in pores of the rigid heat insulation tile, the heat conduction coefficient of the heat protection material is greatly reduced by the nano structure of the aerogel, the heat conductivity is 0.05-0.1W/m.K, in addition, the Si-O-C aerogel is heated and decomposed into small molecular gases such as SiO, CO 2 and the like under the action of high temperature and heat flow, and a large amount of incident heat flow can be simultaneously taken away when the gas volatilizes, so the heat insulation effect is good, and the heat insulation effect is obviously superior to that of a common aerogel material.
3. The surface of the silica-based light ceramic thermal protection material prepared by the invention is coated with the reinforced coating, the airflow scouring resistance of the silica-based light ceramic thermal protection material is superior to that of similar materials such as SIRCA, the residual carbon rate of the reinforced coating on the surface of the silicon resin is high, and a compact layer is formed by high-temperature ablation, so that the ablation speed of the silica-based light ceramic thermal protection material is reduced, in addition, the reinforced coating on the surface contains high-emissivity fillers, and the high-emissivity fillers are oxidized and ablated under the high-temperature aerobic condition and are vitrified on the surface, so that a high-emissivity coating is formed on the surface of the material, and the atmospheric radiation heat transfer is greatly enhanced, so that the surface temperature.
4. The surface strengthening coating related in the preparation method can be used for machining the surface of the rigid heat insulation tile base Si-O-C aerogel composite material to be coated into a surface with larger roughness in advance, so that the contact area between the coating and the rigid heat insulation tile base body is increased, the bonding strength of the coating is obviously improved, and the bonding strength of the surface strengthening coating is as high as 2.0-2.5 MPa, so that the surface strengthening coating is not easy to fall off and damage.
5. The invention can be used for preparing silica-based lightweight ceramic thermal protection members with various shapes and sizes according to design drawings, and has important application value in the outer surface thermal protection material of the outer space exploration aircraft.
drawings
FIG. 1 is a process flow diagram of the preparation method of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention provides a silica-based lightweight ceramic thermal protection material and a preparation method and application thereof.
The invention provides a silica-based lightweight ceramic thermal protection material in a first aspect, which comprises a rigid heat-insulating tile-based Si-O-C aerogel composite material and a surface strengthening coating formed on the outer surface of the rigid heat-insulating tile-based Si-O-C aerogel composite material; the rigid heat insulation tile base Si-O-C aerogel composite material comprises a rigid heat insulation tile base body and Si-O-C aerogel compounded in the rigid heat insulation tile base body.
In some preferred embodiments, the rigid heat insulation tile matrix consists of 1-5% by mass of boron oxide, 50-99% by mass of quartz fibers and 0-49% by mass of fiber reinforcement.
In some preferred embodiments, the fibers in the fiber reinforcement are selected from the group consisting of alumina fibers, mullite fibers, aluminosilicate fibers, zirconia fibers, and yttrium aluminum garnet fibers.
In some preferred embodiments, the surface enhancing coating comprises a room temperature curing silicone and a high emissivity filler.
in some preferred embodiments, the high emissivity filler is selected from the group consisting of glass frit, silicon tetraboride, silicon hexaboride, boron carbide, zirconium carbide, silicon carbide, hafnium carbide, molybdenum disilicide, and tantalum disilicide.
The invention provides a preparation method of a silica-based lightweight ceramic thermal protection material in a second aspect, wherein a process flow chart of the preparation method of the thermal protection material is shown in figure 1, and specifically, the preparation method comprises the following steps:
(1) Preparing a rigid heat insulation tile base body: uniformly stirring and filtering 1-5% (such as 1%, 2%, 3%, 4% or 5%) of boron nitride by mass, 50-99% (such as 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95% or 99%) of quartz fiber by mass, and 0-49% (such as 0%, 1%, 3%, 5%, 8%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45% or 49%) of fiber reinforcement by mass for 1-2 hours (such as 1, 1.5 or 2 hours) to obtain a solid mixture, and then sequentially drying and sintering the obtained solid mixture to obtain a rigid heat insulation tile substrate; the boron nitride is used as a sintering aid; the fiber in the fiber reinforcement is a high temperature resistant substance selected from the group consisting of alumina fiber, mullite fiber, alumina silicate fiber, zirconia fiber and yttrium aluminum garnet fiber. Specifically, for example, 100g of quartz fiber is taken, 1-5 g of boron nitride powder and 3-10 kg of deionized water are added, and a fiber reinforcement-free rigid heat insulation tile substrate used in occasions with lower temperature (less than or equal to 1000 ℃) is prepared; or 50-99 g of quartz fiber and 1-50 g of alumina fiber are taken, 0.5-7.8 g of boron nitride powder and 3-10 kg (such as 3, 4, 5, 6, 7, 8, 9 or 10kg) of deionized water are added, and the fiber reinforcement-containing rigid heat insulation tile matrix used in occasions with high temperature (more than 1000 ℃) is prepared.
(2) Preparation of a Si-O-C sol precursor: uniformly mixing alkoxy silane with an alcohol solvent, and preparing a Si-O-C sol precursor by taking an acidic reagent as a catalyst; the alkoxy silane consists of methyltrimethoxy silane and dimethyl dimethoxy silane, and the mass ratio of the methyltrimethoxy silane to the dimethyl dimethoxy silane is (200-300) to (50-75); the alcohol solvent is preferably absolute ethyl alcohol; the acidic reagent is selected from the group consisting of nitric acid, hydrochloric acid, and sulfuric acid. Specifically, 200 to 300g (e.g., 200, 220, 250, 280 or 300g) of methyltrimethoxysilane and 50 to 75g (e.g., 50, 55, 60, 65, 70 or 75g) of dimethyldimethoxysilane are fully mixed with 300 to 400mL (e.g., 300, 320, 350, 380 or 400mL) of ethanol under magnetic stirring, 200 to 300mL (e.g., 200, 220, 250, 280 or 300mL) of an acidic reagent (e.g., nitric acid, hydrochloric acid or sulfuric acid) with the concentration of 1 to 1.5mol/L (e.g., 1, 1.1, 1.2, 1.3, 1.4 or 1.5mol/L) is slowly dropped as a catalyst, the hydrolysis reaction rate is controlled, and stirring is continued for 5 to 8 minutes (e.g., 5, 6, 7 or 8 minutes) after the dropping of the acidic reagent is completed to prepare the Si-O-C sol precursor.
(3) Dipping the rigid heat insulation tile matrix prepared in the step (1) by using the Si-O-C sol precursor prepared in the step (2), standing to enable the Si-O-C sol precursor to be gelled to prepare a rigid heat insulation tile base Si-O-C wet gel composite material, and sequentially aging, solvent replacing and drying the rigid heat insulation tile base Si-O-C wet gel composite material to prepare a rigid heat insulation tile base Si-O-C aerogel composite material; the impregnation adopts vacuum impregnation; the aging is room temperature aging, for example, the aging can be placed at room temperature for 24-48 hours (for example, 24, 30, 36, 42 or 48 hours); the solvent replacement is carried out in an alcohol solvent, preferably absolute ethanol; the drying is supercritical drying, preferably supercritical carbon dioxide drying.
(4) Preparing a surface strengthening coating: preparing a surface strengthening coating containing room temperature curing silicone resin, a catalyst, a cross-linking agent, a dispersion medium and high-emissivity fillers, and coating the surface strengthening coating on the outer surface of the rigid heat-insulation tile-based Si-O-C aerogel composite material prepared in the step (3) to form a surface strengthening coating, so as to obtain a silica-based lightweight ceramic thermal protection material; the catalyst is dibutyltin dilaurate; the cross-linking agent is ethyl orthosilicate; the dispersion medium is selected from the group consisting of toluene, o-xylene, p-xylene, m-xylene, and acetone; the high-emissivity filler is selected from the group consisting of glass powder, silicon tetraboride, silicon hexaboride, boron carbide, zirconium carbide, silicon carbide, hafnium carbide, molybdenum disilicide and tantalum disilicide, and preferably is selected from the group consisting of silicon tetraboride, boron carbide and borosilicate glass powder with the softening temperature of 600-1100 ℃. In another preferred embodiment, high emissivity fillers such as molybdenum disilicide, tantalum disilicide, and silicon hexaboride can be added in suitable amounts as desired. Specifically, for example, 100 to 120g (for example, 100, 110 or 120g) of the room temperature curing silicone rubber precursor, 10 to 15g (for example, 10, 11, 12, 13, 14 or 15g) of the silicon tetraboride powder, 10 to 15g (for example, 10, 11, 12, 13, 14 or 15g) of the boron carbide powder, 10 to 15g (for example, 10, 11, 12, 13, 14 or 15g) of the borosilicate glass powder with a softening temperature of 600 to 1100 ℃ (for example, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃ or 1100 ℃) and 100 to 120g (for example, 100, 110 or 120g) of the paraxylene are uniformly mixed in a container; uniformly mixing 1-1.2 g (such as 1, 1.1 or 1.2g) of ethyl orthosilicate, 0.1-0.2 g (such as 0.1, 0.15 or 0.2g) of dibutyltin dilaurate and 100-120 g (such as 100, 110 or 120g) of p-xylene in another container, mixing the mixed solution in the two containers together, rapidly stirring for 3-5 minutes (such as 3, 4 or 5 minutes) to obtain a surface strengthening coating, coating (such as spraying or brushing) the prepared surface strengthening coating on the outer surface of the rigid heat insulation tile-based Si-O-C aerogel composite material, and curing the silicone resin at room temperature after the p-xylene contained in the surface strengthening coating is volatilized to form a porous surface strengthening coating. In another preferred embodiment, before the surface strengthening coating is applied, the surface of the rigid heat insulation tile base Si-O-C aerogel composite material to be coated can be machined into a surface with larger roughness in advance, so that the contact area between the coating and the rigid heat insulation tile base body is increased.
the present invention provides, in a third aspect, a silica-based lightweight ceramic thermal protection member made of the silica-based lightweight ceramic thermal protection material described in the present invention. The thermal protection component provided by the invention needs to be machined to a required size according to a design drawing, a negative tolerance of 0.05-0.2 mm (such as 0.05, 0.1, 0.15 or 0.2mm) is reserved on the outer surface, preferably a negative tolerance of 0.1-0.2 mm (such as 0.1, 0.15 or 0.2mm), and then a surface strengthening coating is coated on the outer surface.
The present invention provides, in a fourth aspect, the silica-based lightweight ceramic thermal protection material provided in the first aspect of the invention or the silica-based lightweight ceramic thermal protection material prepared by the preparation method provided in the second aspect of the invention and the use of the silica-based lightweight ceramic thermal protection member provided in the third aspect of the invention in a thermal protection material for an exterior surface of an aircraft.
Example 1
And (3) stirring 100g of quartz fiber, 5g of boron nitride powder and 10kg of deionized water for 2 hours, filtering, pressing a filter cake to a pre-calculated height, and then drying and sintering to obtain the quartz fiber rigid heat insulation tile. Then, 200g of methyltrimethoxysilane, 50g of dimethyldimethoxysilane and 300mL of absolute ethyl alcohol are poured into a 5000mL beaker and are fully and uniformly mixed by magnetic stirring; then slowly dripping 200mL of nitric acid catalyst with the concentration of 1mol/L, using an ice water mixed bath outside a beaker, controlling the hydrolysis reaction speed, continuing stirring for 5 minutes after the dripping of the nitric acid is finished to obtain the required Si-O-C sol precursor, placing the prepared rigid heat insulation tile into a vacuum impregnation tank, vacuumizing until the gauge pressure is 0.01MPa, then injecting the Si-O-C sol precursor into the vacuum impregnation tank, standing to make the Si-O-C sol gel to obtain a rigid heat insulation tile base Si-O-C wet gel composite material, placing the rigid heat insulation tile base Si-O-C wet gel composite material for 48 hours at room temperature to further age the Si-O-C wet gel, immersing the aged rigid heat insulation tile base Si-O-C wet gel composite material into absolute ethyl alcohol for solvent replacement, and drying by supercritical carbon dioxide to obtain the rigid heat-insulating tile-based Si-O-C aerogel composite material. Finally, uniformly mixing 100g of room-temperature cured silicone rubber precursor, 10g of silicon tetraboride powder, 10g of boron carbide powder, 10g of borosilicate glass powder with the softening temperature of 800 ℃ and 100g of paraxylene in a container; and uniformly mixing 1g of ethyl orthosilicate, 0.1g of dibutyltin dilaurate and 100g of p-xylene in another container, mixing the mixed solution in the two containers together, quickly stirring for 4 minutes to obtain a surface strengthening coating, brushing the surface strengthening coating on the outer surface of the rigid heat-insulating tile-based Si-O-C aerogel composite material, and curing the silicon resin at room temperature after the p-xylene is volatilized to form a porous surface strengthening coating, thereby preparing the silicon dioxide-based lightweight ceramic thermal protection material.
The index detection result of the silicon dioxide-based light ceramic thermal protection material comprises that the density of the silicon dioxide-based light ceramic thermal protection material is 0.20g/cm 3, the thermal conductivity is 0.05W/m.K, the compressive strength is 1.35MPa, the emissivity is 0.9, the bonding strength of the surface strengthening coating is 2.5MPa, and in an oxygen/acetylene flame ablation test of 4.5MW/m 2, the linear ablation rate and the mass ablation rate of the silicon dioxide-based light ceramic thermal protection material are respectively 0.018mm/s and 0.03 g/s.
Comparative example 1
and (3) adding 5g of boron nitride powder and 10kg of deionized water into 100g of quartz fiber, stirring for 2 hours, filtering, pressing a filter cake to a pre-calculated height, and then drying and sintering to obtain the all-quartz fiber rigid heat insulation tile. Then 15g of methyltrimethoxysilane, 15g of ethyl orthosilicate and 50mL of absolute ethyl alcohol are put into a beaker, and a certain amount of hydrochloric acid is added until the pH value of the solution is 3; simultaneously weighing 50mL of anhydrous ethanol and 90mL of distilled water into the other beaker, simultaneously putting the two beakers into a magnetic stirrer, stirring for half an hour to uniformly mix the two beakers, setting the temperature of the magnetic stirrer to be 60 ℃, and controlling the stirring speed to be based on that the liquid cannot be splashed out. And mixing the two solutions together half an hour later, after the reaction is finished, putting the mixture into a magnetic stirrer, stirring the mixture for one hour, taking out the beaker, cooling the beaker at room temperature, adding a certain amount of ammonia water when the temperature of the solution is reduced to the room temperature, measuring the pH value of the solution until the pH value is 8, putting the solution into the magnetic stirrer again, and stirring the solution until the solution is uniformly mixed but no gel exists to obtain the Si-O-C sol precursor. And then placing 1.58g of the prepared rigid heat insulation tile in a vacuum impregnation tank, vacuumizing to gauge pressure of 0.01MPa, then injecting a Si-O-C sol precursor into the vacuum impregnation tank, standing to enable the Si-O-C sol to gel to obtain a rigid heat insulation tile base Si-O-C wet gel composite material, then placing the rigid heat insulation tile base Si-O-C wet gel composite material at room temperature for 48 hours to further age the Si-O-C wet gel, immersing the aged rigid heat insulation tile base Si-O-C wet gel composite material in absolute ethyl alcohol for solvent replacement, and drying by supercritical carbon dioxide to obtain the rigid heat insulation tile base Si-O-C aerogel composite material. And finally, putting the rigid heat insulation tile base Si-O-C aerogel composite material into a pyrolysis furnace for pyrolysis, setting the flow rate of nitrogen at 0.2mL/min, setting the initial temperature at 50 ℃, heating to 150 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 15min, heating to 400 ℃ at a heating rate of 2 ℃/min, keeping the temperature for 30min, heating to 1200 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 2 hours, turning off a power supply, and cooling to room temperature to obtain the rigid heat insulation tile base Si-O-C aerogel composite material. Finally, uniformly mixing 100g of room-temperature cured silicone rubber precursor, 10g of silicon tetraboride powder, 10g of boron carbide powder, 10g of borosilicate glass powder with the softening temperature of 800 ℃ and 100g of paraxylene in a container; and uniformly mixing 1g of ethyl orthosilicate, 0.1g of dibutyltin dilaurate and 100g of p-xylene in another container, mixing the mixed solution in the two containers together, quickly stirring for 4 minutes to obtain a surface strengthening coating, brushing the surface strengthening coating on the outer surface of the rigid heat-insulating tile-based Si-O-C aerogel composite material, and curing the silicon resin at room temperature after the p-xylene is volatilized to form a porous surface strengthening coating, thereby preparing the silicon dioxide-based lightweight ceramic thermal protection material.
Index detection is carried out on the rigid heat insulation tile-based Si-O-C aerogel composite material and the silica-based light ceramic thermal protection material, and the obtained results are as follows:
the density of the rigid heat insulation tile-based Si-O-C aerogel composite material is 0.14g/cm 3, the compressive strength is 0.135MPa, and the density of the silica-based lightweight ceramic thermal protection material is 0.18g/cm 3, and the compressive strength is 0.135 MPa.
Comparative example 2
comparative example 2 was conducted in substantially the same manner as comparative example 1 except that: 3.33g of rigid heat insulation tile is placed in a vacuum impregnation tank, and the rigid heat insulation tile is impregnated by using a Si-O-C sol precursor.
Index detection is carried out on the rigid heat insulation tile-based Si-O-C aerogel composite material and the silica-based light ceramic thermal protection material, and the obtained results are as follows:
The density of the rigid heat insulation tile-based Si-O-C aerogel composite material is 0.23g/cm 3, the compressive strength is 0.45MPa, and the density of the silica-based lightweight ceramic thermal protection material is 0.25g/cm 3, and the compressive strength is 0.45 MPa.
Comparative example 3
comparative example 3 was conducted in substantially the same manner as comparative example 1 except that: 7.5g of the rigid heat insulation tile is placed in a vacuum impregnation tank, and the rigid heat insulation tile is impregnated by using a Si-O-C sol precursor.
index detection is carried out on the rigid heat insulation tile-based Si-O-C aerogel composite material and the silica-based light ceramic thermal protection material, and the obtained results are as follows:
the density of the rigid heat insulation tile-based Si-O-C aerogel composite material is 0.35g/cm 3, the compressive strength is 0.85MPa, and the density of the silica-based lightweight ceramic thermal protection material is 0.38g/cm 3, and the compressive strength is 0.85 MPa.
comparative example 4
Comparative example 4 was conducted in substantially the same manner as comparative example 1 except that: and (3) putting 12.6g of the rigid heat insulation tile into a vacuum impregnation tank, and impregnating the rigid heat insulation tile with the Si-O-C sol precursor.
Index detection is carried out on the rigid heat insulation tile-based Si-O-C aerogel composite material and the silica-based light ceramic thermal protection material, and the obtained results are as follows:
the density of the rigid heat insulation tile-based Si-O-C aerogel composite material is 0.49g/cm 3, the compressive strength is 1.0MPa, and the density of the silica-based lightweight ceramic thermal protection material is 0.52g/cm 3, and the compressive strength is 1.0 MPa.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (7)
1. A preparation method of a silica-based lightweight ceramic thermal protection material is characterized by comprising the following steps:
(1) Preparing a rigid heat insulation tile base body: uniformly mixing 1-5% by mass of boron nitride, 50-99% by mass of quartz fiber and 0-49% by mass of fiber reinforcement with water, filtering to obtain a solid mixture, drying and sintering the solid mixture to obtain a rigid heat insulation tile substrate;
(2) Preparation of a Si-O-C sol precursor: uniformly mixing alkoxy silane with an alcohol solvent, and preparing a Si-O-C sol precursor by taking an acidic reagent as a catalyst;
(3) Dipping the rigid heat insulation tile matrix prepared in the step (1) by using the Si-O-C sol precursor prepared in the step (2), standing to enable the Si-O-C sol precursor to be gelled to prepare a rigid heat insulation tile base Si-O-C wet gel composite material, and sequentially aging, solvent replacing and drying the rigid heat insulation tile base Si-O-C wet gel composite material to prepare a rigid heat insulation tile base Si-O-C aerogel composite material;
(4) Preparing a surface strengthening coating: preparing a surface strengthening coating containing room-temperature curing silicone resin, dibutyltin dilaurate, ethyl orthosilicate, a dispersion medium and a high-emissivity filler, and coating the surface strengthening coating on the outer surface of the rigid heat-insulating tile-based Si-O-C aerogel composite material prepared in the step (3) to form a surface strengthening coating, so as to obtain a silicon dioxide-based lightweight ceramic thermal protection material;
The thermal protection material comprises a rigid thermal insulation tile-based Si-O-C aerogel composite material and a surface strengthening coating formed on the outer surface of the rigid thermal insulation tile-based Si-O-C aerogel composite material; the surface strengthening coating comprises room temperature curing silicone resin and high emissivity filler; the rigid heat insulation tile base Si-O-C aerogel composite material comprises a rigid heat insulation tile base body and Si-O-C aerogel compounded in the rigid heat insulation tile base body.
2. The method of claim 1, wherein:
The alkoxy silane in the step (2) consists of methyltrimethoxy silane and dimethyldimethoxy silane, and the mass ratio of the methyltrimethoxy silane to the dimethyldimethoxy silane is (200-300) to (50-75).
3. The method of claim 1, wherein:
The alcohol solvent in the step (2) is absolute ethyl alcohol;
The acidic reagent in step (2) is selected from the group consisting of nitric acid, hydrochloric acid and sulfuric acid;
Vacuum impregnation is adopted in the impregnation in the step (3);
The solvent replacement in the step (3) is carried out in an alcohol solvent;
The drying in the step (3) is supercritical drying; and/or
The dispersion medium in the step (4) is selected from the group consisting of toluene, o-xylene, p-xylene, m-xylene and acetone.
4. The production method according to claim 3, characterized in that:
the solvent replacement in step (3) is carried out in absolute ethanol.
5. The production method according to claim 3, characterized in that:
the drying in the step (3) is supercritical carbon dioxide drying.
6. a silica-based lightweight ceramic thermal protection member characterized by:
The thermal protection member is made of a silica-based lightweight ceramic thermal protection material prepared by the method of any one of claims 1 to 5.
7. Use of a silica-based lightweight ceramic thermal protection material prepared by the method of any one of claims 1 to 5 or the silica-based lightweight ceramic thermal protection component of claim 6 in a thermal protection material for an exterior surface of an aircraft.
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| CN111908932B (en) * | 2020-07-21 | 2023-06-20 | 山东工业陶瓷研究设计院有限公司 | Light high-efficiency heat-proof and heat-insulating integrated heat protection material and preparation method thereof |
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