阅读说明：本技术 一种耐高温抗辐射夹层热防护材料及其制备方法 (High-temperature-resistant anti-radiation interlayer thermal protection material and preparation method thereof ) 是由 张恩爽 贺丽娟 李文静 雷朝帅 张昊 张凡 于 2021-08-20 设计创作，主要内容包括：本发明涉及一种耐高温抗辐射夹层热防护材料及其制备方法。所述方法：将气凝胶隔热芯层材料进行打孔和疏水化；将纤维织物铺设在气凝胶隔热芯层材料的上下表面,并缝合成隔热组件；将隔热组件浸渍在铝溶胶中,然后先在40～80℃下干燥4～12h,然后在100～150℃下干燥1～6h,得到初级致密化隔热组件；将初级致密化隔热组件在两个以上不同温度阶段进行分级热处理；采用聚碳硅烷前驱体刷涂分级热处理后材料的表面,然后依次进行固化和裂解,制得耐高温抗辐射夹层热防护材料。本发明方法制得的耐高温抗辐射夹层热防护材料具有抗辐射、耐高温、低密度、高效隔热、结构强度高,抗冲刷性能优异的特点,可应用在高温、高热流下的隔热领域。(The invention relates to a high-temperature-resistant and radiation-resistant interlayer thermal protection material and a preparation method thereof. The method comprises the following steps: perforating and hydrophobizing the aerogel heat insulation core layer material; laying fiber fabrics on the upper and lower surfaces of the aerogel heat insulation core layer material, and sewing the fiber fabrics into a heat insulation component; dipping the heat insulation assembly in alumina sol, drying for 4-12 h at 40-80 ℃, and then drying for 1-6 h at 100-150 ℃ to obtain a primary densified heat insulation assembly; carrying out graded heat treatment on the primary densified heat insulation assembly at more than two different temperature stages; and brushing a polycarbosilane precursor on the surface of the material subjected to graded heat treatment, and then sequentially curing and cracking to prepare the high-temperature-resistant and radiation-resistant interlayer heat protection material. The high-temperature-resistant and radiation-resistant interlayer thermal protection material prepared by the method has the characteristics of radiation resistance, high temperature resistance, low density, high-efficiency heat insulation, high structural strength and excellent scouring resistance, and can be applied to the field of heat insulation under high temperature and high heat flow.)

1. A preparation method of a high-temperature-resistant and radiation-resistant interlayer thermal protection material is characterized by comprising the following steps:

(1) sequentially performing punching treatment and hydrophobization treatment on the aerogel heat insulation core layer material to obtain a hydrophobization aerogel heat insulation core layer material;

(2) laying a fiber fabric on the upper surface and the lower surface of the hydrophobization aerogel heat insulation core layer material to obtain a laminated assembly, and sewing the laminated assembly by adopting a sewing line to obtain a heat insulation assembly;

(3) dipping the heat insulation assembly in alumina sol to obtain a heat insulation assembly dipped with the alumina sol, drying the heat insulation assembly dipped with the alumina sol at 40-80 ℃ for 4-12 h, and drying at 100-150 ℃ for 1-12 h to obtain a primary densified heat insulation assembly;

(4) carrying out graded heat treatment on the primary densified heat insulation assembly at more than two different temperature stages to obtain a high-temperature-resistant interlayer heat protection material;

(5) and brushing a polycarbosilane precursor on the surface of the high-temperature-resistant interlayer thermal protection material, and then sequentially curing and cracking the high-temperature-resistant interlayer thermal protection material coated with the polycarbosilane precursor to prepare the high-temperature-resistant anti-radiation interlayer thermal protection material.

2. The method according to claim 1, wherein the aluminum sol is prepared by:

(a) uniformly dispersing the submicron-grade aluminum oxide particles, the nano particles, the water-soluble resin and the tetraethoxysilane by using water to obtain an aluminum oxide solution;

(b) and adding a surfactant into the alumina solution, uniformly stirring, and then carrying out ultrasonic treatment to obtain the aluminum sol.

3. The method of claim 2, wherein:

the particle size of the submicron alumina particles is 100-300 nm;

the particle size of the nano particles is 10-60nm, and preferably, the nano particles are nano alumina particles and/or nano silica particles;

the water-soluble resin is one or more of water-based acrylic resin, water-based epoxy resin, water-based organic silicon resin and water-based polyurethane resin;

the surfactant is one or more of sodium lauryl sulfate, linear alkyl benzene sulfonate and fatty alcohol-polyoxyethylene ether sodium sulfate;

the mass ratio of the submicron alumina particles to the nanoparticles is 100: (5-30);

in the alumina solution, the mass percentage of the water-soluble resin is 0.1-5%;

in the alumina solution, the mass percentage of the water is 50-70%;

in the alumina solution, the mass percentage of the ethyl orthosilicate is 1-10%;

the dosage of the surfactant is 0.05-0.5% of the mass of the alumina solution;

the solid content of the aluminum sol is 10-40%;

in the step (b), the stirring time is 0.5-5 h; and/or

The ultrasonic treatment time is 10-120 min, preferably 20-60 min.

4. The production method according to claim 1, wherein in step (5):

the curing temperature is 100-300 ℃, and the curing time is 1-12 h; and/or

The cracking is carried out in an inert atmosphere, the cracking temperature is 700-1200 ℃, and the cracking time is 1-12 h.

5. The production method according to any one of claims 1 to 4, characterized in that, in step (1):

the aerogel heat insulation core layer is made of a high-temperature-resistant aerogel material or is formed by compounding a fiber cotton felt and a high-temperature-resistant aerogel material, and preferably, the fiber cotton felt is a mullite fiber cotton felt, a carbon fiber cotton felt, a silicon carbide fiber cotton felt or an alumina fiber cotton felt;

the hydrophobic agent adopted for the hydrophobic treatment is a siloxane hydrophobic agent and/or a fluorosilane hydrophobic agent, and preferably, the amount of the adopted hydrophobic agent is 1-15% of the mass of the aerogel heat insulation core layer material; and/or

The temperature of the hydrophobic treatment is 80-150 ℃, and the time of the hydrophobic treatment is 1-4 d.

6. The production method according to any one of claims 1 to 4, characterized in that, in step (2):

the suture line adopts alumina fiber bundles, and preferably, the suture line adopts the alumina fiber bundles which are subjected to twisting and/or hardening treatment;

the sewing adopts Z-direction sewing;

the sewing distance of the sewing is 8-15 mm; and/or

The diameter of a needle hole of a sewing needle adopted by sewing is 1-2 mm.

7. The production method according to any one of claims 1 to 4, characterized in that, in step (2):

the fiber fabric is a fiber braided fabric obtained by braiding one or more than two of alumina fiber, mullite fiber, carbon fiber and silicon carbide fiber; and/or

The thickness of the fiber fabric laid on the upper surface and the lower surface of the hydrophobic aerogel heat insulation core layer material is 0.1-3 mm independently.

8. The production method according to any one of claims 1 to 4, characterized in that:

in the step (3), the impregnation is vacuum impregnation, and the conditions of the vacuum impregnation are as follows: carrying out vacuum impregnation for 0.1-1 h at the temperature of 20-30 ℃ and the vacuum degree of 0.1-0.5 MPa;

in the step (3), before the obtained heat insulation component impregnated with the alumina sol is dried, the obtained heat insulation component impregnated with the alumina sol is placed at room temperature for 1-12 hours;

before the step (4) is carried out, the step (3) is repeated for 2-10 times; and/or

The method also comprises the step of repeating the step (5) for 1-10 times.

9. The production method according to any one of claims 1 to 4, characterized in that, in step (4):

the step heat treatment in more than two different temperature stages comprises first temperature stage heat treatment, second temperature stage heat treatment, third temperature stage heat treatment, fourth temperature stage heat treatment and fifth temperature stage heat treatment;

the temperature of the first temperature stage heat treatment is 200-450 ℃, and the time of the first temperature stage heat treatment is 1-10 h;

the temperature of the second temperature stage heat treatment is 450-600 ℃, and the time of the second temperature stage heat treatment is 1-10 h;

the temperature of the heat treatment in the third temperature stage is 700-900 ℃, and the time of the heat treatment in the third temperature stage is 1-10 h;

the temperature of the heat treatment in the fourth temperature stage is 1000-1150 ℃, and the time of the heat treatment in the fourth temperature stage is 1-10 h;

the temperature of the heat treatment in the fifth temperature stage is 1150-1300 ℃, and the time of the heat treatment in the fifth temperature stage is 1-10 h.

10. The high-temperature-resistant and radiation-resistant interlayer thermal protection material prepared by the preparation method of any one of claims 1 to 9.

Technical Field

The invention relates to the technical field of preparation of external heat-proof and heat-insulating materials, in particular to a high-temperature-resistant and radiation-resistant interlayer heat protection material and a preparation method thereof.

Background

The nano porous aerogel material is a gel material with a dispersion medium of gas, is a nano porous solid material with a network structure formed by mutually accumulating colloidal particles or high polymer molecules, and the size of pores in the material is in the order of nanometers. The porosity of the porous ceramic is as high as 80-99.8%, the typical size of the pores is 1-100 nm, and the specific surface area is 200-1000 m²A density of as low as 3kg/m³The room temperature thermal conductivity can be as low as 0.012W/m.k. Due to the characteristics, the aerogel material has wide application potential in the aspects of thermal, acoustic, optical, microelectronic and particle detection. Currently, the widest field of application of aerogels is still the field of thermal insulation, since the unique nanostructure of aerogels can effectively reduce convection conduction, solid phase conduction and thermal radiation.

Because the three-dimensional porous characteristic of aerogel, it has exhibited the fragile characteristics of structure, though the fibre reinforcement process need be carried out to the in-service use aerogel, can improve the structural strength of aerogel to a certain extent, nevertheless to the outer heat protection application under the high air current erodees, still need further to improve the antiscour performance of material. Chinese patent application CN201711291795.6 discloses a method for preparing a thermal protection material with a sandwich structure and a thermal protection material prepared by the method, wherein a prepreg preparation process of resin impregnated fabric is adopted to prepare a sandwich external thermal protection material with high surface strength; however, the temperature resistance of the prepared sandwich structure thermal protection material is not more than 1100 ℃ at most due to the limitation of a material system. Chinese patent application CN201811066573.9 discloses a multilayer composite thermal protection material and a preparation method thereof, the method utilizes a multilayer fiber combination mode to prepare the thermal protection material with high temperature resistance and high heat insulation efficiency, the temperature resistance can reach 1600 ℃, however, a plurality of materials need to be combined in the patent application, the preparation process is difficult to control, and the surface of the thermal protection material in the patent application is not toughened, and the anti-scouring performance is insufficient.

With the development of science and technology, various fields put higher requirements on the temperature resistance, structural strength and high-temperature heat-insulating property of heat-insulating materials, so that an effective method is needed to be developed for preparing a high-temperature-resistant and radiation-resistant interlayer heat protection material.

Disclosure of Invention

In order to solve one or more technical problems in the prior art, the invention provides a high-temperature-resistant and radiation-resistant interlayer thermal protection material and a preparation method thereof. The high-temperature-resistant and radiation-resistant interlayer thermal protection material prepared by the method has the characteristics of high temperature resistance, low density, high efficiency in heat insulation, radiation resistance, high structural strength and excellent scouring resistance.

The invention provides a preparation method of a high-temperature-resistant and radiation-resistant interlayer thermal protection material in a first aspect, which comprises the following steps:

(1) sequentially performing punching treatment and hydrophobization treatment on the aerogel heat insulation core layer material to obtain a hydrophobization aerogel heat insulation core layer material;

(2) laying a fiber fabric on the upper surface and the lower surface of the hydrophobization aerogel heat insulation core layer material to obtain a laminated assembly, and sewing the laminated assembly by adopting a sewing line to obtain a heat insulation assembly;

(3) dipping the heat insulation assembly in alumina sol to obtain a heat insulation assembly dipped with the alumina sol, drying the heat insulation assembly dipped with the alumina sol at 40-80 ℃ for 4-12 h, and drying at 100-150 ℃ for 1-12 h to obtain a primary densified heat insulation assembly;

(4) carrying out graded heat treatment on the primary densified heat insulation assembly at more than two different temperature stages to prepare a high-temperature-resistant interlayer heat protection material;

(5) and brushing a polycarbosilane precursor on the surface of the high-temperature-resistant interlayer thermal protection material, and then sequentially curing and cracking the high-temperature-resistant interlayer thermal protection material coated with the polycarbosilane precursor to prepare the high-temperature-resistant anti-radiation interlayer thermal protection material.

Preferably, the aluminum sol is prepared by the following steps:

(a) uniformly dispersing the submicron-grade aluminum oxide particles, the nano particles, the water-soluble resin and the tetraethoxysilane by using water to obtain an aluminum oxide solution;

(b) and adding a surfactant into the alumina solution, uniformly stirring, and then carrying out ultrasonic treatment to obtain the aluminum sol.

Preferably, the particle size of the submicron alumina particles is 100-300 nm; the particle size of the nano particles is 10-60nm, and preferably, the nano particles are nano alumina particles and/or nano silica particles; the water-soluble resin is one or more of water-based acrylic resin, water-based epoxy resin, water-based organic silicon resin and water-based polyurethane resin; the surfactant is one or more of sodium lauryl sulfate, linear alkyl benzene sulfonate and fatty alcohol-polyoxyethylene ether sodium sulfate; the mass ratio of the submicron alumina particles to the nanoparticles is 100: (5-30); in the alumina solution, the mass percentage of the water-soluble resin is 0.1-5%; in the alumina solution, the mass percentage of the water is 50-70%; in the alumina solution, the mass percentage of the ethyl orthosilicate is 1-10%; the dosage of the surfactant is 0.05-0.5% of the mass of the alumina solution; the solid content of the aluminum sol is 10-40%; in the step (b), the stirring time is 0.5-5 h; and/or the time of ultrasonic treatment is 10-120 min, preferably 20-60 min.

Preferably, in step (5): the curing temperature is 100-300 ℃, and the curing time is 1-12 h; and/or the cracking is carried out in an inert atmosphere, the cracking temperature is 700-1200 ℃, and the cracking time is 1-12 h.

Preferably, in step (1): the aerogel heat insulation core layer is made of a high-temperature-resistant aerogel material or is formed by compounding a fiber cotton felt and a high-temperature-resistant aerogel material, and preferably, the fiber cotton felt is a mullite fiber cotton felt, a carbon fiber cotton felt, a silicon carbide fiber cotton felt or an alumina fiber cotton felt; the hydrophobic agent adopted for the hydrophobic treatment is a siloxane hydrophobic agent and/or a fluorosilane hydrophobic agent, and preferably, the amount of the adopted hydrophobic agent is 1-15% of the mass of the aerogel heat insulation core layer material; and/or the temperature of the hydrophobic treatment is 80-150 ℃, and the time of the hydrophobic treatment is 1-4 d.

Preferably, in step (2): the suture line adopts alumina fiber bundles, and preferably, the suture line adopts the alumina fiber bundles which are subjected to twisting and/or hardening treatment; the sewing adopts Z-direction sewing; the sewing distance of the sewing is 8-15 mm; and/or the diameter of a needle hole of a suture needle adopted by the suture is 1-2 mm.

Preferably, in step (2): the fiber fabric is a fiber braided fabric obtained by braiding one or more than two of alumina fiber, mullite fiber, carbon fiber and silicon carbide fiber; and/or the thickness of the fiber fabric laid on the upper surface and the lower surface of the hydrophobic aerogel heat insulation core layer material is 0.1-3 mm independently.

Preferably, in step (3), the impregnation is vacuum impregnation under the following conditions: carrying out vacuum impregnation for 0.1-1 h at the temperature of 20-30 ℃ and the vacuum degree of 0.1-0.5 MPa; in the step (3), before the obtained heat insulation component impregnated with the alumina sol is dried, the obtained heat insulation component impregnated with the alumina sol is placed at room temperature for 1-12 hours; before the step (4) is carried out, the step (3) is repeated for 2-10 times; and/or the method further comprises the step of repeating the step (5) 1-10 times.

Preferably, in step (4): the step heat treatment in more than two different temperature stages comprises first temperature stage heat treatment, second temperature stage heat treatment, third temperature stage heat treatment, fourth temperature stage heat treatment and fifth temperature stage heat treatment; the temperature of the first temperature stage heat treatment is 200-450 ℃, and the time of the first temperature stage heat treatment is 1-10 h; the temperature of the second temperature stage heat treatment is 450-600 ℃, and the time of the second temperature stage heat treatment is 1-10 h; the temperature of the heat treatment in the third temperature stage is 700-900 ℃, and the time of the heat treatment in the third temperature stage is 1-10 h; the temperature of the heat treatment in the fourth temperature stage is 1000-1150 ℃, and the time of the heat treatment in the fourth temperature stage is 1-10 h; the temperature of the heat treatment in the fifth temperature stage is 1150-1300 ℃, and the time of the heat treatment in the fifth temperature stage is 1-10 h.

In a second aspect, the invention provides a high temperature and radiation resistant interlayer thermal protection material prepared by the preparation method of the first aspect of the invention.

Compared with the prior art, the invention at least has the following beneficial effects:

(1) the heat insulation component impregnated with the alumina sol is subjected to primary densification by adopting a step-by-step drying process, and then densification heat treatment is performed by adopting a graded heat treatment process, wherein the graded heat treatment process realizes that the sol with different particle sizes can be sintered and crosslinked, and can realize the gradual hardening of the high-temperature resistant interlayer heat protection material panel, the graded heat treatment process realizes the gradual solidification and ceramic treatment of the material, can slow down the crystal form transformation process of the material, avoids the structural collapse of a porous structure in the rapid shrinkage process, realizes the strengthening and toughening of the microstructure of the high-temperature resistant interlayer heat protection material, is beneficial to the formation of a high-temperature resistant phase, ensures that a nanometer framework is more stable, and improves the structural strength and the scouring resistance of the material.

(2) Different from other methods for preparing the interlayer heat insulation material, the invention provides that the alumina fiber fabric with higher temperature resistance grade is used as a panel material, the silicon-aluminum composite alumina sol with better temperature resistance grade is used as a base material, and meanwhile, the panel of the high-temperature-resistant interlayer heat protection material is subjected to coating modification, and a silicon carbide component with good stability at high temperature and radiation resistance is introduced, so that the prepared high-temperature-resistant radiation-resistant interlayer heat protection material can be effectively used for high-temperature-resistant high-efficiency heat insulation application, and the improvement method is more feasible.

(3) In some preferred embodiments of the present invention, the matrix material alumina sol contains sub-micron alumina particles and graded particles of nano-particles, wherein the sub-micron alumina particles can effectively improve the temperature resistance of the material, and the nano-particles can be filled in the pores of the fiber fabric to effectively improve the densification degree of the material; in addition, the alumina sol containing the graded particles can simultaneously avoid the problem that the fibers are fragile due to strong bonding between the nano particles and the fibers.

(4) In some more preferred embodiments of the invention, the aluminum sol is a silicon-aluminum composite component, and after high-temperature treatment, the silicon-aluminum composite component can form a mullite phase with higher temperature resistance, so that the temperature resistance of the high-temperature-resistant and radiation-resistant interlayer thermal protection material can be more effectively improved; the silicon carbide coating formed by the invention can form a sand brick-like structure with oxide components, the structural strength is greatly improved compared with that of the traditional material, and the integral strength of the high-temperature-resistant and radiation-resistant interlayer thermal protection material and the strength of a panel can be greatly improved.

(5) The surface of the high-temperature resistant interlayer heat protection material prepared in some preferred embodiments of the invention is modified by a coating, the heat conductivity of the material can be further reduced by introducing a silicon carbide coating with radiation resistance, the temperature resistance of the material is improved, and the prepared high-temperature resistant radiation resistant interlayer heat protection material has excellent high-temperature resistance under the premise of keeping low heat conductivity less than 0.04W/m & lt K & gt, can realize the temperature resistance limit of 1600 ℃ of 1800s, has the characteristics of high temperature resistance, low density and high-efficiency heat insulation, and can be applied to the field of high-efficiency heat insulation under high temperature and high heat flow.

(6) The high-temperature-resistant and radiation-resistant interlayer thermal protection material prepared by the method has high overall strength and excellent scour resistance, the compression strength of the high-temperature-resistant and radiation-resistant interlayer thermal protection material prepared in some preferred embodiments is 1.5-2.5 MPa at room temperature, the tensile strength of the high-temperature-resistant and radiation-resistant interlayer thermal protection material at the heat-resistant temperature is not lower than 5MPa, the tensile strength of a panel at the room temperature is more than 100MPa, and the tensile strength of the panel at the heat-resistant temperature is more than 25 MPa.

Drawings

FIG. 1 is a flow chart of the preparation of some embodiments of the present invention.

Fig. 2 is an SEM image of the upper panel modified with silicon carbide coating, which is included in the refractory and radiation resistant interlayer thermal protective material prepared in example 1 of the present invention.

Fig. 3 is an optical photograph of the upper panel modified with silicon carbide coating and made of the refractory and radiation resistant interlayer thermal protective material prepared in example 1 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 preparation method of a high-temperature-resistant and radiation-resistant interlayer thermal protection material in a first aspect, which comprises the following steps:

(1) sequentially performing punching treatment and hydrophobization treatment on the aerogel heat insulation core layer material to obtain a hydrophobization aerogel heat insulation core layer material; in the invention, the aerogel heat insulation core layer material is preferably a high-temperature resistant aerogel material or is formed by compounding a fiber cotton felt and the high-temperature resistant aerogel material, wherein the high-temperature resistant aerogel material is a high-temperature resistant aerogel material which takes oxide nanocrystals as a framework or exists in a nanocrystal assembling process in the preparation process, the source and the type of the high-temperature resistant aerogel material are not particularly limited, for example, the material can be a high temperature resistant aerogel material disclosed in chinese patent application CN108249901A, a high temperature resistant special-shaped nanocrystalline aerogel material disclosed in chinese patent application CN110282958A, a high temperature resistant alumina nanocrystalline aerogel material disclosed in chinese patent application CN111252789A, a high temperature resistant high performance aerogel composite material disclosed in chinese patent application CN111925194A, a high temperature resistant anti-radiation aerogel composite material disclosed in chinese patent application CN111943654A, a reusable high temperature resistant nanocrystalline aerogel material disclosed in chinese patent application CN111943704A, and the like; in the invention, firstly, the aerogel heat insulation core layer material is punched so as to be convenient for Z-direction sewing with fiber fabric and Z-direction fixing, and then hydrophobic treatment is carried out to obtain the hydrophobic aerogel heat insulation core layer material; the present invention does not specifically limit the perforation treatment and the hydrophobization treatment, and can be carried out by a conventional method; preferably, when the punching treatment is carried out, the hole diameter of the punching is 1-2 mm, and the hole distance is 5-20 mm, more preferably 8-15 mm; in the invention, for example, the aerogel heat insulation core layer material is subjected to perforating, and then the aerogel heat insulation core layer material is subjected to vacuum hydrophobization treatment by using a siloxane hydrophobic reagent and/or a fluorosilane hydrophobic reagent to obtain a hydrophobized aerogel heat insulation core layer material; the invention discovers that after the aerogel heat insulation core layer material is subjected to hydrophobic treatment, the density and the heat conductivity coefficient of the finally prepared high-temperature-resistant and radiation-resistant interlayer heat protection material can be obviously reduced.

(2) Laying a fiber fabric on the upper surface and the lower surface of the hydrophobization aerogel heat insulation core layer material to obtain a laminated assembly, and sewing the laminated assembly by adopting a sewing line to obtain a heat insulation assembly; in the invention, the suture line is preferably made of high-temperature-resistant alumina fiber bundles, and preferably, the suture line is made of twisted and/or hardened alumina fiber bundles, which is beneficial to suture and improvement of the overall strength of the material; in the present invention, the twisting refers to winding a plurality of suture threads into one strand; the hardening treatment refers to hardening treatment of the head (end) of the alumina fiber; the invention has no special limitation on the parameters of the twisting and hardening treatment, and can adopt the conventional means; the invention has no special requirements on the specification of the alumina fiber bundle, and the existing common alumina fiber bundle can be adopted.

(3) Immersing the heat insulation assembly in an aluminum sol to obtain an aluminum sol-impregnated heat insulation assembly, drying the aluminum sol-impregnated heat insulation assembly at 40-80 ℃ (e.g., 40 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃ or 80 ℃) for 4-12 h (e.g., 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5, 10, 10.5, 11, 11.5 or 12h), and then drying at 100-150 ℃ (e.g., 100 ℃, 105 ℃, 110 ℃, 115 ℃, 120 ℃, 125 ℃, 130 ℃, 135 ℃, 140 ℃, 145 ℃ or 150 ℃) for 1-12 h (e.g., 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5, 10, 10.5, 11, 11.5 or 12h) to obtain a primary heat insulation assembly; in the present invention, it is preferable that the drying is performed by evacuation.

(4) Carrying out graded heat treatment on the primary densified heat insulation assembly at more than two different temperature stages to prepare a high-temperature-resistant interlayer heat protection material; in the invention, the high-temperature resistant interlayer thermal protection material comprises an upper panel, a lower panel and an aerogel thermal insulation core layer material positioned between the upper panel and the lower panel; the upper panel and the lower panel are formed by at least a step-by-step drying process and a grading heat treatment process after the fiber fabrics are soaked in the aluminum sol; in the upper and lower panels of the present invention, the panel having the functions of heat insulation, load bearing, erosion resistance, etc. is marked as the upper panel of the heat protection material of the high temperature resistant and radiation resistant interlayer.

(5) Brushing a polycarbosilane precursor on the surface of the high-temperature-resistant interlayer thermal protection material, and then sequentially carrying out curing and cracking on the high-temperature-resistant interlayer thermal protection material coated with the polycarbosilane precursor to prepare a high-temperature-resistant radiation-resistant interlayer thermal protection material (which can be abbreviated as a radiation-resistant interlayer thermal protection material); preferably, before the steps of curing and cracking are carried out in sequence, the step of vacuumizing and removing bubbles of the high-temperature-resistant interlayer thermal protection material coated with the polycarbosilane precursor is carried out; the method has no special requirement on the step of removing bubbles by vacuumizing, and can be carried out by adopting the conventional operation; the polycarbosilane precursor is not particularly required by the invention, and can be formed by using polycarbosilane precursors commonly used for forming silicon carbide coatings in the prior art, preferably, the polycarbosilane precursor comprises a solute and a solvent, wherein the solute is selected from one or more of solid Polycarbosilane (PCS), perhydropolycarbosilane (AHPCS) and Liquid Polycarbosilane (LPCS), and/or the solvent is selected from one or more of butanone, xylene and toluene; in the present invention, the liquid polycarbosilane may be, for example, a vinyl-containing Liquid Polycarbosilane (LPVCS). In the invention, when the polycarbosilane ceramic precursor is liquid polycarbosilane, the surface of the high-temperature resistant interlayer thermal protection material can be directly brushed by the liquid polycarbosilane; in the invention, preferably, the mass percentage of the solute contained in the polycarbosilane precursor is 40-60 wt%, that is, the concentration of the polycarbosilane precursor is 40-60 wt%; the invention has no special requirement on the brushing thickness, so that the polycarbosilane precursor can be uniformly brushed on the surface of the high-temperature resistant interlayer heat protection material, preferably, the thickness of the polycarbosilane precursor in a single brushing is 1-10%, more preferably 3-6% of the thickness of the fiber fabric paved on the surface of the hydrophobic aerogel heat insulation core material, specifically, for example, the thickness of the polycarbosilane precursor in a single brushing on the upper surface of the high-temperature resistant interlayer heat protection material is 1-10%, more preferably 3-6% of the thickness of the fiber fabric paved on the upper surface of the hydrophobic aerogel heat insulation core material, the thickness of the polycarbosilane precursor in a single brushing on the lower surface of the high-temperature resistant interlayer heat protection material is 1-10% of the thickness of the fiber fabric paved on the lower surface of the hydrophobic aerogel heat insulation core material, more preferably 3-6%; in the invention, the high temperature resistant and radiation resistant interlayer thermal protection material comprises a high temperature resistant interlayer thermal protection material and a silicon carbide coating formed on the surface of the high temperature resistant interlayer thermal protection material, namely the high temperature resistant and radiation resistant interlayer thermal protection material comprises an upper panel with the silicon carbide coating, a lower panel with the silicon carbide coating and an aerogel heat insulation core layer material positioned between the upper panel coated with the silicon carbide coating and the lower panel coated with the silicon carbide coating.

The heat insulation component impregnated with the alumina sol is subjected to primary densification by adopting a step-by-step drying process, and then densification heat treatment is performed by adopting a graded heat treatment process, wherein the graded heat treatment process realizes that the sol with different particle sizes can be sintered and crosslinked, and can realize the gradual hardening of a panel of the high-temperature-resistant interlayer heat protection material; according to the invention, coating modification is carried out on the panel of the high-temperature-resistant interlayer thermal protection material, and the silicon carbide component with good stability and radiation resistance at high temperature is introduced, so that the prepared high-temperature-resistant radiation-resistant interlayer thermal protection material can be more effectively used for high-temperature-resistant high-efficiency heat insulation application.

The invention can determine the grading heat treatment temperature of the material according to the use temperature and the use pressure of the high-temperature-resistant and radiation-resistant interlayer heat protection material, the unstable phase of the material tends to be stable after the material is pretreated at a certain temperature, the material can be further used in the environment, and the higher the heat treatment temperature is, the higher the density of the material is, and the heat insulation effect can be correspondingly reduced.

According to some preferred embodiments, the aluminum sol is prepared by:

(a) uniformly dispersing the submicron-grade aluminum oxide particles, the nano particles, the water-soluble resin and the tetraethoxysilane by using water to obtain an aluminum oxide solution; in the invention, for example, the dispersion can be carried out uniformly by stirring, and the stirring time can be, for example, 0.5 to 5 hours, preferably 0.5 to 1.5 hours; the invention discovers that the addition of the water-soluble resin is beneficial to improving the integral formability of the panel of the primary densified heat insulation assembly before graded heat treatment and promoting the assembly and bonding among micro-nano particles, thereby effectively improving the integral strength of the high-temperature-resistant and radiation-resistant interlayer heat protection material and the panel strength; in the present invention, the sub-micron alumina particles, such as sub-micron alumina particles of alpha alumina crystal form, can be directly purchased from the market, and the nanoparticles, such as amorphous nano alumina particles and/or amorphous nano silica particles, can be directly purchased from the market;

(b) adding a surfactant into the alumina solution, uniformly stirring, and then carrying out ultrasonic treatment to obtain the aluminum sol; in the present invention, the surfactant is added so that the sol particles do not settle.

The invention discovers that the alumina sol containing the submicron alumina particles and the graded particles of the nano particles prepared by the steps (a) and (b) can effectively improve the temperature resistance of the material, and the nano particles can be filled in the pores of the fiber fabric to effectively improve the densification degree of the material; the particle size and the crystal form of the adopted alumina sol are set for high-temperature and high-strength performance, the component adopts submicron alumina particles of alpha alumina crystal form with high-temperature resistance level as main basic components, the alpha alumina mainly can improve the temperature resistance of the panel, and the nanometer alumina particles and the nanometer silica particles in the alumina sol are used as bonding phases which are melted at high temperature, so that the density of the panel can be effectively improved, and the overall strength of the panel is improved; in addition, the alumina sol containing the graded particles can simultaneously avoid the problem that the fibers are fragile due to strong bonding between the nano particles and the fibers; in addition, the alumina sol prepared in the step (a) and the step (b) is a silicon-aluminum composite component, and the silicon-aluminum composite component can form a mullite phase with a higher temperature resistance phase, so that the temperature resistance of the high-temperature-resistant and radiation-resistant interlayer thermal protection material can be effectively improved; the invention adopts the silicon-aluminum composite alumina sol with better temperature resistance grade as the base material, so that the prepared high-temperature-resistant radiation-resistant interlayer thermal protection material can be effectively used for high-temperature-resistant light heat insulation application. The invention discovers that if the alumina sol of the silicon-aluminum composite component is prepared by only adopting the nano particles, the water-soluble resin and the tetraethoxysilane under the action of the surfactant, the prepared primary densified heat insulation component has serious contraction of the panel after the graded heat treatment, and the temperature resistance and the mechanical property of the finally prepared high-temperature-resistant radiation-resistant interlayer heat protection material are obviously reduced; if the silica sol in the prior art is adopted to dip the heat insulation component, the temperature resistance of the finally prepared high-temperature-resistant radiation-resistant interlayer heat protection material can be obviously reduced, so that the temperature resistance of the finally prepared high-temperature-resistant radiation-resistant interlayer heat protection material can only reach 1200 ℃.

According to some preferred embodiments, the sub-micron alumina particles have a particle size of 100 to 300 nm; the particle size of the nano-particles is 10-60nm, preferably, the nano-particles are nano-alumina particles and/or nano-silica particles, and more preferably, the nano-particles are nano-alumina particles; the water-soluble resin is one or more of water-based acrylic resin, water-based epoxy resin, water-based organic silicon resin and water-based polyurethane resin; the invention has no special limit to the waterborne acrylic resin, the waterborne epoxy resin, the waterborne organic silicon resin and the waterborne polyurethane resin, and can adopt products which can be sold on the market directly; the surfactant is one or more of sodium lauryl sulfate, sodium linear alkylbenzene sulfonate (such as sodium dodecyl benzene sulfonate) and sodium fatty alcohol-polyoxyethylene ether sulfate.

According to some preferred embodiments, the mass ratio of the sub-micron alumina particles to the nanoparticles is 100: (5-30) (e.g., 100:5, 100:10, 100:15, 100:20, 100:25, or 100:30), more preferably 100: (10-20); in the present invention, it is preferable that the mass ratio of the sub-micron alumina particles to the nanoparticles is 100: (5-30), the reason is that the invention discovers that if the content of the submicron alumina particles is too high, the bonding phase component which is molten at high temperature is too little, and the bonding phase component can not play a role in effective bonding, so that the compactness of the panel can not be effectively improved, and the integral strength of the panel can not be effectively improved, and if the content of the submicron alumina particles is too low, the improvement of the temperature resistance of the material is not facilitated.

According to some preferred embodiments, the mass percentage of the water-soluble resin in the alumina solution is 0.1-5% (e.g., 0.1%, 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, or 5%), and the addition of the water-soluble resin is beneficial to improving the integral formability of the primary densified heat insulation assembly before the step heat treatment, and promoting the assembly and bonding among the micro-nano particles, thereby effectively improving the integral strength and the panel strength of the high-temperature-resistant and radiation-resistant interlayer heat protection material; in the alumina solution, the mass percentage of the water is 50-70% (for example, 50%, 55%, 60%, 65% or 70%); in the alumina solution, the weight percentage of the ethyl orthosilicate is 1-10% (e.g. 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5% or 10%); the amount of the surfactant is 0.05-0.5% (e.g., 0.05%, 0.08%, 0.1%, 0.2%, 0.3%, 0.4%, or 0.5%) of the mass of the alumina solution; in the present invention, it is preferable that the alumina solution contains the following components in percentage by mass: 50-70% of water; 1-10% of ethyl orthosilicate; 0.1-5% of water-soluble resin; the balance is submicron alumina particles and nanoparticles, and the mass ratio of the submicron alumina particles to the nanoparticles is 100: (5-30), the aluminum oxide solution in the formula is beneficial to ensuring that the aluminum sol with the solid content of 10-40% is prepared.

According to some preferred embodiments, the aluminum sol has a solid content of 10 to 40% (e.g., 10%, 15%, 20%, 25%, 30%, 35%, or 40%), more preferably, the aluminum sol has a solid content of 15 to 30%; in the invention, the preferred aluminum sol with the solid content of 10-40% is obtained, so that the high solid content is facilitated under the condition of ensuring that dispersed particles in the aluminum sol do not settle, the dipping times of the fiber fabric can be effectively reduced, and the preparation efficiency is improved; in the present invention, the solid content of the alumina sol refers to the sum of the mass percentages of sub-micron alumina particles, nanoparticles (e.g., nano alumina particles), and nano silica particles produced from tetraethoxysilane.

According to some preferred embodiments, in step (b), the stirring time is 0.5 to 5 hours (e.g. 0.5, 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5 or 5 hours), preferably 0.5 to 1.5 hours; and/or the time of the ultrasonic treatment is 10-120 min (for example, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 95, 100, 105, 110, 115 or 120min), preferably 20-60 min (for example, 20, 25, 30, 35, 40, 45, 50, 55 or 60 min); the present invention is not particularly limited in the rotational speed of the stirring and the power of the ultrasonic treatment.

According to some preferred embodiments, in step (5): the curing temperature is 100-300 ℃ (such as 180 ℃, 200 ℃, 250 ℃ or 300 ℃), and the curing time is 1-12 h (such as 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 or 12 h); in some more preferred embodiments, the curing comprises a first temperature stage curing, a second temperature stage curing, and a third temperature stage curing; the curing temperature of the first temperature stage is 100-140 ℃ (such as 100 ℃, 120 ℃ or 140 ℃), and the curing time of the first temperature stage is 1-4 h, preferably 1-2 h; the curing temperature of the second temperature stage is 150-200 ℃ (150 ℃, 180 ℃ or 200 ℃), and the curing time of the second temperature stage is 1-4 h, preferably 1-2 h; the curing temperature of the third temperature stage is 200-300 ℃ (such as 200 ℃, 220 ℃, 250 ℃, 280 ℃ or 300 ℃), and the curing time of the third temperature stage is 1-4 h, preferably 1-2 h; and/or the cracking is carried out under an inert atmosphere, the temperature of the cracking is 700-1200 ℃, preferably (such as 700 ℃, 750 ℃, 800 ℃, 850 ℃, 900 ℃, 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃ or 1200 ℃) is preferably 700-1100 ℃, and the time of the cracking is 1-12 h (such as 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 or 12h), preferably 2-4 h (such as 2, 2.5, 3, 3.5 or 4 h); in the invention, the temperature rise rate in the cracking process can be 1-5 ℃/min, for example; in the invention, the ceramic yield of the silicon carbide coating formed by sequentially carrying out the steps of curing and cracking on the polycarbosilane precursor can be 50-85%, for example; in the present invention, the inert atmosphere may be, for example, an argon and/or nitrogen atmosphere; the invention finds that the silicon carbide coating formed under the protection of inert atmosphere can realize good oxidation resistance.

According to some preferred embodiments, in step (1): the aerogel heat insulation core layer is made of a high-temperature-resistant aerogel material or is formed by compounding a fiber cotton felt and a high-temperature-resistant aerogel material, and preferably, the fiber cotton felt is a mullite fiber cotton felt, a carbon fiber cotton felt, a silicon carbide fiber cotton felt or an alumina fiber cotton felt; in the invention, when the aerogel heat insulation core layer material is formed by compounding the fiber cotton felt and the high-temperature-resistant aerogel material, the high-temperature-resistant aerogel material is distributed in the pores of the fiber cotton felt. Compared with the silicon dioxide aerogel in the prior art, the high-temperature-resistant aerogel material disclosed by the invention can obviously improve the bonding strength between the panel of the high-temperature-resistant and radiation-resistant interlayer thermal protection material and the material of the aerogel heat insulation core layer and improve the temperature resistance of the high-temperature-resistant and radiation-resistant interlayer thermal protection material.

According to some preferred embodiments, in step (1), the hydrophobizing treatment is performed by using a hydrophobic agent of siloxane type and/or fluorosilane type, preferably by using an amount of 1 to 15% by mass (e.g., 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5, 10, 10.5, 11, 11.5, 12, 12.5, 13, 13.5, 14, 14.5 or 15%) of the aerogel thermal insulation core material; in the present invention, the siloxane-based hydrophobic agent may be, for example, one or more of trimethylmethoxysilane, trimethylethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, dimethylmethoxysilane, dimethylethoxysilane, methyltrimethoxysilane, methyltriethoxysilane, phenyltriethoxysilane, and pentafluorophenyltriethoxysilane; the fluorosilane-based hydrophobic agent may be, for example, one or more of tridecafluoroctyltrimethoxysilane, heptadecafluorodecyltrimethoxysilane, and pentafluorophenyltrimethoxysilane. According to some preferred embodiments, the temperature of the hydrophobization treatment is 80 to 150 ℃ (e.g., 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃, 105 ℃, 110 ℃, 115 ℃, 120 ℃, 125 ℃, 130 ℃, 135 ℃, 140 ℃, 145 ℃ or 150 ℃), and the time of the hydrophobization treatment is 1 to 4d (e.g., 1, 1.5, 2, 2.5, 3, 3.5 or 4 d); in some specific embodiments, for example, the aerogel thermal insulation core material after the perforation treatment is placed in a closed container, and the hydrophobization treatment is performed after the vacuum pumping, the temperature of the hydrophobization treatment is 80-150 ℃, and the time of the hydrophobization treatment is 1-4 d, wherein the unit "d" represents the time unit "day".

According to some preferred embodiments, in step (2): the suture line adopts alumina fiber bundles, and preferably, the suture line adopts the alumina fiber bundles which are subjected to twisting and/or hardening treatment; in the invention, preferably, the suture line is made of a high-temperature-resistant alumina fiber bundle, and the invention finds that the high-temperature-resistant radiation-resistant interlayer thermal protection material prepared by sewing the alumina fiber bundle does not have fracture of the suture line and does not have the phenomenon that the panel is separated from the aerogel thermal insulation core layer material when the erosion resistance test is carried out, and if the mullite fiber bundle is used as the suture line for sewing, the finally obtained radiation-resistant interlayer thermal protection material has fracture of the suture line and separation of the panel and the aerogel thermal insulation core layer material when the erosion resistance test is carried out, and the heat-resistant temperature of the radiation-resistant interlayer thermal protection material can be obviously reduced.

According to some preferred embodiments, the stitching is Z-direction stitching, and in the present invention, the fiber fabric and the hydrophobized aerogel thermal insulation core layer material are preferably fixed by Z-direction stitching.

The sewing distance and the diameter of the needle hole of the sewing are not particularly required, and in some specific embodiments, the sewing distance of the sewing is preferably 8-15 mm; and/or the diameter of a needle hole of a suture needle adopted by the suture is preferably 1-2 mm.

According to some preferred embodiments, in step (2): the fiber fabric is a fiber woven fabric obtained by weaving one or any two or more of alumina fibers, mullite fibers, carbon fibers and silicon carbide fibers, and more preferably, the fiber woven fabric is a fiber woven fabric made of alumina fibers (abbreviated as alumina fiber woven fabric); the invention preferably adopts the alumina fiber fabric with higher temperature resistance grade as the panel material and adopts the composite alumina sol with better temperature resistance grade as the matrix material to prepare the radiation-resistant interlayer heat-insulating material, which can be effectively used for high-temperature-resistant light heat-insulating application, and the improvement method is more feasible.

According to some preferred embodiments, the thickness of the fiber fabric laid on the upper and lower surfaces of the hydrophobic aerogel thermal insulation core material is independently 0.1 to 3mm, and in some specific embodiments, the thickness of the fiber fabric laid on the upper surface of the hydrophobic aerogel thermal insulation core material is, for example, 1.8 to 3mm, and the thickness of the fiber fabric laid on the lower surface of the hydrophobic aerogel thermal insulation core material is, for example, 0.1 to 1.5 mm.

According to some preferred embodiments, in step (1), the thickness of the aerogel thermal insulation core layer material before the perforation treatment and the hydrophobic treatment are sequentially performed is 5 to 30mm, preferably 10 to 25 mm.

According to some preferred embodiments, in step (3), the impregnation is vacuum impregnation under the following conditions: vacuum impregnation is carried out for 0.1-1 h under the conditions that the temperature is 20-30 ℃ and the vacuum degree is 0.1-0.5 MPa.

According to some preferred embodiments, in step (3), before drying the obtained aluminum sol-impregnated heat insulation assembly, the obtained aluminum sol-impregnated heat insulation assembly is first placed at room temperature for 1 to 12 hours (e.g., 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, or 12 hours), and more preferably for 4 to 8 hours; in some specific embodiments, step (3) is: dipping the heat insulation assembly in alumina sol to obtain a heat insulation assembly dipped with the alumina sol, then placing the heat insulation assembly dipped with the alumina sol at room temperature (20-30 ℃) for 1-12 h, drying at 40-80 ℃ for 4-12 h, and drying at 100-150 ℃ for 1-12 h to obtain a primary densified heat insulation assembly; the invention discovers that the obtained heat insulation assembly soaked with the alumina sol is firstly placed at room temperature for 1-12 hours, more preferably for 4-8 hours, and then a step-by-step drying process is carried out, so that a high-temperature-resistant and radiation-resistant interlayer heat protection material with compact interior can be obtained, the bonding strength between a panel of the high-temperature-resistant and radiation-resistant interlayer heat protection material and an aerogel heat insulation core layer material can be improved, and the high-temperature mechanical property and the heat resistance temperature of the high-temperature-resistant and radiation-resistant interlayer heat protection material can be effectively improved; if the obtained heat insulation assembly soaked with the alumina sol is directly subjected to a one-step drying process, a large amount of floating gel exists on the surface of the finally prepared anti-radiation interlayer heat protection material, the interior of the finally prepared anti-radiation interlayer heat protection material is not compact enough, the bonding strength of the aerogel heat insulation core layer material and the panel is weak, the mechanical property of the anti-radiation interlayer heat protection material is reduced, and the temperature resistance is reduced.

According to some preferred embodiments, before step (4), step (3) is repeated for 2 to 10 times (for example, 2, 3, 4, 5, 6, 7, 8, 9 or 10 times), in the present invention, step (3) is preferably repeated for 2 to 10 times, more preferably step (3) is repeated for 2 to 5 times.

According to some preferred embodiments, the method further comprises the step of repeating the step (5) for 1 to 10 times (for example, 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10 times), preferably for 2 to 6 times (for example, 2, 3, 4, 5 or 6 times), so as to improve the compactness of the formed silicon carbide coating, and thus to better improve the oxidation resistance and temperature resistance of the high-temperature radiation-resistant interlayer heat protection material.

According to some preferred embodiments, in step (4): the step heat treatment in more than two different temperature stages comprises first temperature stage heat treatment, second temperature stage heat treatment, third temperature stage heat treatment, fourth temperature stage heat treatment and fifth temperature stage heat treatment; the temperature of the first temperature stage heat treatment is 200 ℃ to 450 ℃ (for example, 200 ℃, 250 ℃, 300 ℃, 350 ℃, 400 ℃ or 450 ℃), and the time of the first temperature stage heat treatment is 1 to 10 hours (for example, 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10 hours), preferably 1 to 5 hours (for example, 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5 or 5 hours); the temperature of the second temperature stage heat treatment is 450 ℃ -600 ℃ (450 ℃, 500 ℃, 550 ℃ or 600 ℃), and the time of the second temperature stage heat treatment is 1-10 h (such as 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10h), preferably 1-5 h (such as 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5 or 5 h); the temperature of the heat treatment in the third temperature stage is 700-900 ℃, and the time of the heat treatment in the third temperature stage is 1-10 h (for example, 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10h), preferably 1-5 h (for example, 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5 or 5 h); the temperature of the heat treatment in the fourth temperature stage is 1000-1150 ℃, and the time of the heat treatment in the fourth temperature stage is 1-10 h (for example, 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10h), preferably 1-5 h (for example, 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5 or 5 h); the temperature of the heat treatment in the fifth temperature stage is 1150-1300 ℃ (for example 1150 ℃, 1200 ℃, 1250 ℃ or 1300 ℃), and the time of the heat treatment in the fifth temperature stage is 1-10 h (for example 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10h), preferably 1-5 h (for example 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5 or 5 h); in the present invention, the heat treatment for classification may be performed in a muffle furnace, for example, and the temperature increase rate may be 1 to 10 ℃/min (for example, 1, 2, 3, 4, 5, 6, 7, 8, 9, or 10 ℃/min).

In the present invention, the step heat treatment in the two or more different temperature stages is preferably performed by the first temperature stage heat treatment, the second temperature stage heat treatment, the third temperature stage heat treatment, the fourth temperature stage heat treatment and the fifth temperature stage heat treatment, because the panel of the primary densified heat insulation assembly obtained in step (3) is subjected to the low temperature treatment at 450 ℃ in the first stage to solidify the organic matter, which is beneficial to uniformly stacking the micro-nano particles; after the first stage step is carried out, carrying out a second stage, and carrying out heat treatment at 450-600 ℃ to be beneficial to slowly decomposing the organic matter content in the panel; after the second stage is finished, performing a third stage, and performing heat treatment at 700-900 ℃, so that low-temperature phase sintering in the panel matrix is facilitated, and the panel strength is increased; after the third stage is finished, performing heat treatment at 1000-1150 ℃ in a fourth stage, so as to facilitate medium-temperature phase sintering in the panel matrix, further filling a molten phase into large particle gaps, increasing the density of the panel and improving the strength; and (3) after the fourth stage is finished, performing heat treatment at 1150-1300 ℃ in the fifth stage, so that high-temperature phase sintering in the panel matrix is facilitated, the panel is further integrated, the density of the panel is increased, a high-temperature stable phase is generated, the strength is improved, and the high-temperature radiation-resistant interlayer thermal protection material with a strong structural framework is obtained. The invention discovers that the strength of the panel can be obviously improved by adopting the grading heat treatment process comprising five temperature stages compared with the grading heat treatment process comprising two temperature stages or the one-step heat treatment process, thereby being beneficial to improving the scouring resistance of the finally prepared high-temperature-resistant and radiation-resistant interlayer heat protection material.

According to some specific embodiments, the preparation of the high temperature and radiation resistant interlayer thermal protection material comprises the following steps:

firstly, the existing high-temperature-resistant aerogel material is used as an aerogel heat insulation core layer material, and the aerogel heat insulation core layer material is subjected to punching treatment and hydrophobization treatment to obtain a hydrophobization aerogel heat insulation material core layer;

secondly, laying fiber fabrics on the upper surface and the lower surface of the hydrophobic aerogel heat insulation core layer material, and sewing the upper fiber fabric panel and the lower fiber fabric panel of the hydrophobic aerogel heat insulation core layer material to obtain a heat insulation assembly; wherein, the suture line adopts high-temperature resistant alumina fiber bundles.

Thirdly, adding the submicron alumina particles, the nano alumina particles, the water-soluble resin and the tetraethoxysilane into water and uniformly stirring to obtain a uniformly dispersed alumina solution; adding a surfactant into the alumina solution, uniformly stirring, and performing ultrasonic treatment to obtain uniformly dispersed alumina sol.

Putting the heat insulation assembly obtained in the step (II) into the alumina sol obtained in the step (III) for vacuum impregnation, wherein the vacuum impregnation comprises the following steps: vacuumizing and dipping for 0.1-1 h under the conditions that the temperature is 25 ℃ and the vacuum degree is 0.1-0.5 MPa, then placing the heat insulation assembly dipped with the alumina sol at the room temperature of 25 ℃ for 1-12 h, drying at the temperature of 40-80 ℃ for 4-12 h under the vacuumizing condition, and then drying at the temperature of 100-150 ℃ for 1-12 h to obtain the primary densified heat insulation assembly.

And fifthly, repeating the step (iv) for 2-10 times.

Sixthly, carrying out a grading heat treatment process on the material obtained in the fifth step to obtain a high-temperature resistant interlayer heat protection material; the grading heat treatment system comprises a first temperature stage heat treatment, a second temperature stage heat treatment, a third temperature stage heat treatment, a fourth temperature stage heat treatment and a fifth temperature stage heat treatment; the temperature of the first temperature stage heat treatment is 200-450 ℃, and the time of the first temperature stage heat treatment is 1-10 h; the temperature of the second temperature stage heat treatment is 450-600 ℃, and the time of the second temperature stage heat treatment is 1-10 h; the temperature of the heat treatment in the third temperature stage is 700-900 ℃, and the time of the heat treatment in the third temperature stage is 1-10 h; the temperature of the heat treatment in the fourth temperature stage is 1000-1150 ℃, and the time of the heat treatment in the fourth temperature stage is 1-10 h; the temperature of the heat treatment in the fifth temperature stage is 1150-1300 ℃, and the time of the heat treatment in the fifth temperature stage is 1-10 h.

Seventhly, brushing a polycarbosilane precursor on the surface of the high-temperature-resistant interlayer heat protection material, and then sequentially curing and cracking the high-temperature-resistant interlayer heat protection material coated with the polycarbosilane precursor; the curing temperature is 100-300 ℃, and the curing time is 1-12 h; the cracking is carried out in an inert atmosphere, the cracking temperature is 1000-1200 ℃, and the cracking time is 1-12 h.

Eighthly, repeating the step (1) to (10) times to prepare the high-temperature-resistant and radiation-resistant interlayer thermal protection material.

The invention finds that under the combined action of the steps I to II, the preparation of the high-temperature-resistant and radiation-resistant interlayer thermal protection material with excellent scour resistance, good high-temperature resistance, stable structure at high temperature, light weight and high strength after high-temperature heat treatment is more favorably ensured; the invention discovers that when the high-temperature-resistant and radiation-resistant interlayer thermal protection material is prepared, the deletion of any step is not beneficial to preparing the high-temperature-resistant and radiation-resistant interlayer thermal protection material with the best comprehensive performance.

In a second aspect, the invention provides a high temperature and radiation resistant interlayer thermal protection material prepared by the preparation method of the first aspect of the invention. The aerogel heat insulation core layer material of the high temperature resistant and radiation resistant interlayer heat protection material prepared by the method has high bonding strength with a panel, high integral structure strength, excellent mechanical property, excellent scour resistance, temperature resistance up to more than 1600 ℃, service time of 1800s or more, the high temperature resistant and radiation resistant interlayer heat protection material prepared in some preferred embodiments has the compression strength of 1.5-2.5 MPa at room temperature, the tensile strength of not less than 5MPa at the heat resistance temperature, the room temperature tensile strength of the panel is more than 100MPa, and the tensile strength of more than 25MPa at the heat resistance temperature.

The invention will be further illustrated by way of example, but the scope of protection is not limited to these examples.

Example 1

Firstly, adopting a high-temperature-resistant special-shaped nanocrystalline aerogel material with the thickness of 10mm as an aerogel heat-insulating core layer material, performing punching on the aerogel heat-insulating core layer material, and then performing hydrophobization treatment to obtain a hydrophobization aerogel heat-insulating material core layer; the high-temperature-resistant special-shaped nanocrystalline aerogel material is prepared by the method of example 4 in Chinese patent application CN110282958A, and has the heat-resistant temperature of 1400 ℃; the hydrophobic treatment comprises the following steps: placing the mechanically perforated aerogel heat insulation core layer material into a closed container, adding a trimethoxy methyl silane hydrophobic reagent accounting for 15% of the mass of the aerogel heat insulation core layer material, vacuumizing, and performing hydrophobic treatment, wherein the temperature of the hydrophobic treatment is 100 ℃, and the time of the hydrophobic treatment is 2 d.

Laying fiber fabrics woven by adopting alumina fibers on the upper surface and the lower surface of the hydrophobization aerogel heat insulation core layer material, and sewing the upper fiber fabric panel and the lower fiber fabric panel (Z-direction sewing) on the hydrophobization aerogel heat insulation core layer material to obtain a heat insulation assembly; wherein, the suture line adopts high-temperature resistant alumina fiber bundles which are twisted and hardened at the ends; the thickness of the fiber fabric laid on the upper surface of the hydrophobized aerogel heat insulation core layer material was 2mm, and the thickness of the fiber fabric laid on the lower surface of the hydrophobized aerogel heat insulation core layer material was 0.5 mm.

Thirdly, adding the submicron alumina particles, the nano alumina particles, the water-soluble resin and the ethyl orthosilicate into water and uniformly stirring (stirring time is 30min) to obtain a uniformly dispersed alumina solution; adding a surfactant into the alumina solution, uniformly stirring (stirring time is 30min), and carrying out ultrasonic treatment (ultrasonic treatment is 40min) to obtain uniformly dispersed alumina sol, wherein the alumina sol comprises alpha-phase alumina, amorphous alumina and amorphous silica; the alumina solution comprises the following components in percentage by mass: 65% of water; 10% of ethyl orthosilicate; 2.5% of water-soluble resin; the balance is submicron alumina particles and nanometer alumina particles, and the mass ratio of the submicron alumina particles to the nanometer alumina particles is 100: 15; the dosage of the surfactant is 0.08 percent of the mass of the alumina solution; wherein the submicron alumina particles are alpha alumina crystal form submicron alumina particles with the particle size range of 100-300nm, the nano alumina particles are amorphous alumina nano particles with the particle size range of 10-60nm, the water-soluble resin is water-based epoxy resin, and the surfactant is sodium lauryl sulfate.

Putting the heat insulation assembly obtained in the step (II) into the alumina sol obtained in the step (III) for vacuum impregnation, wherein the vacuum impregnation comprises the following steps: carrying out vacuum impregnation for 1h under the conditions that the temperature is 25 ℃ and the vacuum degree is 0.25MPa, then placing the heat insulation assembly impregnated with the alumina sol at the room temperature of 25 ℃ for 6h, then drying at 60 ℃ for 12h under the vacuum condition, and then drying at 120 ℃ for 6h to obtain the primary densified heat insulation assembly.

Fifthly, repeating the step (iv) for 2 times.

Sixthly, carrying out a grading heat treatment process on the material obtained in the fifth step to obtain the high-temperature resistant interlayer heat protection material; the grading heat treatment system comprises a first temperature stage heat treatment, a second temperature stage heat treatment, a third temperature stage heat treatment, a fourth temperature stage heat treatment and a fifth temperature stage heat treatment; the temperature of the first temperature stage heat treatment is 200 ℃, and the time of the first temperature stage heat treatment is 2 hours; the temperature of the heat treatment in the second temperature stage is 500 ℃, and the time of the heat treatment in the second temperature stage is 2 hours; the temperature of the heat treatment in the third temperature stage is 900 ℃, and the time of the heat treatment in the third temperature stage is 2 hours; the temperature of the heat treatment in the fourth temperature stage is 1100 ℃, and the time of the heat treatment in the fourth temperature stage is 2 hours; the temperature of the heat treatment in the fifth temperature stage is 1200 ℃, and the time of the heat treatment in the fifth temperature stage is 2 hours.

Seventhly, brushing a polycarbosilane precursor on the surface of the high-temperature-resistant interlayer heat protection material, and then sequentially curing and cracking the high-temperature-resistant interlayer heat protection material coated with the polycarbosilane precursor after vacuumizing and removing bubbles; the thickness of the polycarbosilane precursor coated on the upper surface of the high-temperature resistant interlayer heat protection material is 3% of the thickness of the fiber fabric laid on the upper surface of the hydrophobization aerogel heat insulation core layer material, the thickness of the polycarbosilane precursor coated on the lower surface of the high-temperature resistant interlayer heat protection material is 3% of the thickness of the fiber fabric laid on the lower surface of the hydrophobization aerogel heat insulation core layer material, the polycarbosilane precursor comprises a solid polycarbosilane solute and a xylene solvent, and the polycarbosilane precursor is a xylene solution of solid polycarbosilane with the concentration of 50 wt%; the curing procedure is as follows: curing at 120 ℃ for 1.5h, then curing at 180 ℃ for 1.5h, and finally curing at 250 ℃ for 1.5 h; the temperature of the cracking is 1100 ℃, the time of the cracking is 2h, and the cracking is carried out in a nitrogen atmosphere.

Eighthly, repeating the step of seventhly 3 times to prepare the high-temperature-resistant and radiation-resistant interlayer thermal protection material.

The heat insulation performance test of the high temperature resistant and radiation resistant interlayer heat protection material in example 1 shows that the surface of the high temperature resistant and radiation resistant interlayer heat protection material has no light loss, no color change and no shedding, and other performance indexes are shown in table 1.

The density of the high temperature and radiation resistant interlayer thermal protection material prepared in example 1 is 0.5g/cm³The service temperature is 1600 ℃, the service time is 1800s or more, and the room-temperature thermal conductivity is 0.04W/m.K.

The linear shrinkage rate in example 1 was 0.2% for the high temperature resistant interlayer thermal protection material prepared in step (c) compared to the material without the step (e) (the material obtained in step (d)) of the step (c); similarly, the linear shrinkage in other examples and comparative examples in table 1 refers to the linear shrinkage of the high temperature resistant interlayer thermal protective material obtained after the heat treatment compared with the material without the heat treatment process.

The use temperature of the high temperature resistant and radiation resistant interlayer thermal protection material prepared in example 1 is 1600 ℃, the use time is 1800s, which indicates that after the high temperature resistant and radiation resistant interlayer thermal protection material prepared in this example is used at 1600 ℃ for 1800s, the linear shrinkage rate of the high temperature resistant and radiation resistant interlayer thermal protection material used at 1600 ℃ is not more than 5% compared with that of the high temperature resistant and radiation resistant interlayer thermal protection material before use, that is, the heat resistance temperature of the high temperature resistant and radiation resistant interlayer thermal protection material can reach 1600 ℃, and when the high temperature resistant and radiation resistant interlayer thermal protection material is used at a higher temperature for 1800s, the linear shrinkage rate can be more than 5%; similarly, the heat-resistant temperatures of other examples and comparative examples in Table 1 (except comparative example 4) mean that the linear shrinkage of 1800s used at the heat-resistant temperature is not more than 5%, while the linear shrinkage of 1800s used at a temperature higher than the heat-resistant temperature is more than 5%; the heat resistant temperature of 1500 c in comparative example 3 means that the linear shrinkage rate of the high temperature resistant interlayer heat protection material after use at 1500 c is not more than 5% compared with the high temperature resistant interlayer heat protection material before use after use at 1500 c for 1200 s.

The tensile strength of the high temperature resistant and radiation resistant interlayer thermal protection material prepared in example 1 at the heat resistant temperature of 1600 ℃ is 10MPa, and the compression strength at room temperature is 1.7MPa, and the results are shown in Table 1; example 1 the prepared high temperature and radiation resistant interlayer thermal protective material comprising the upper panel formed with the silicon carbide coating layer was also tested for room temperature tensile strength and thermal resistance at 1600 c, and the results are shown in table 1.

Example 2

Example 2 is essentially the same as example 1, except that:

in the step I, the hydrophobization treatment is not carried out on the aerogel heat insulation core layer material subjected to the mechanical punching, but the subsequent steps II to III are directly carried out.

The performance test of the anti-radiation interlayer thermal protection material prepared in the example 2 is the same as that of the example 1, and the density of the anti-radiation interlayer thermal protection material prepared in the example 2 is more than 1.5g/cm³The heat conductivity coefficient at room temperature is as high as 0.12W/m.K, and other performance indexes are shown in Table 1.

Example 3

Example 3 is essentially the same as example 1, except that:

in the second step, mullite fiber bundles are used as suture lines.

The anti-scouring performance test is carried out on the anti-radiation interlayer thermal protection material prepared in the example 3, the fracture of the sewing line of the anti-radiation interlayer thermal protection material is found, the panel is separated from the aerogel heat insulation core layer material, and other performance indexes are shown in the table 1.

Example 4

Example 4 is essentially the same as example 1, except that:

and sixthly, changing the grading heat treatment process into a one-step heat treatment process, and directly carrying out heat treatment on the material obtained in the step (v) at 1200 ℃ for 10 hours to obtain the high-temperature-resistant interlayer heat protection material.

The anti-scouring performance test is carried out on the anti-radiation interlayer thermal protection material prepared in the example 4, the panel is broken after the surface of the anti-radiation interlayer thermal protection material is examined, and other performance indexes are shown in the table 1.

Example 5

Example 5 is essentially the same as example 1, except that:

the third step is: adding nanometer alumina particles, water-soluble resin and ethyl orthosilicate into water, and stirring uniformly (stirring time is 30min) to obtain uniformly dispersed alumina solution; adding a surfactant into the alumina solution, uniformly stirring (stirring time is 30min), and carrying out ultrasonic treatment (ultrasonic treatment is 40min), so as to obtain uniformly dispersed aluminum sol, wherein the aluminum sol comprises components of amorphous alumina and amorphous silica, and the aluminum sol only comprises nano sol particles; the alumina solution comprises the following components in percentage by mass: 65% of water; 10% of ethyl orthosilicate; 2.5% of water-soluble resin; the balance of nano alumina particles; the dosage of the surfactant is 0.08 percent of the mass of the alumina solution; wherein, the nano alumina particles are amorphous alumina nano particles with the particle size range of 10-60nm, the water-soluble resin is water-based epoxy resin, and the surfactant is sodium lauryl sulfate.

The radiation-resistant interlayer thermal protection material prepared in example 5 was subjected to the graded heat treatment in step (c) to cause severe shrinkage of the panel, and other performance indexes were as shown in table 1.

Example 6

Example 6 is essentially the same as example 1, except that:

in the fifth step, only repeat the fourth step 1 times.

Mechanical property tests are carried out on the anti-radiation interlayer thermal protection material prepared in the example 6, and the panel of the anti-radiation interlayer thermal protection material is found to be soft and cannot bear stress, and other performance indexes are shown in table 1.

Example 7

Example 7 is essentially the same as example 1, except that:

the fourth step is: and (3) placing the heat insulation assembly obtained in the step (II) into the alumina sol obtained in the step (III) for vacuum impregnation, wherein the vacuum impregnation comprises the following steps: and carrying out vacuum impregnation for 1h under the conditions that the temperature is 25 ℃ and the vacuum degree is 0.25MPa, and then directly drying the heat insulation assembly impregnated with the alumina sol for 2h at 120 ℃ to obtain a primary densified heat insulation assembly.

The surface of the anti-radiation interlayer thermal protection material prepared in the example 7 has a large amount of floating glue, the interior of the material is not compact enough, and other performance indexes are shown in the table 1.

Example 8

Example 8 is essentially the same as example 1, except that:

the third step is: adding submicron-grade alumina particles, water-soluble resin and tetraethoxysilane into water, and uniformly stirring (stirring time is 30min) to obtain a uniformly dispersed alumina solution; adding a surfactant into the alumina solution, uniformly stirring (stirring time is 30min), and carrying out ultrasonic treatment (ultrasonic treatment is 40min) to obtain uniformly dispersed alumina sol, wherein the alumina sol comprises alpha-phase alumina and amorphous silica; the alumina solution comprises the following components in percentage by mass: 65% of water; 10% of ethyl orthosilicate; 2.5% of water-soluble resin; the balance is submicron-grade alumina particles, and the dosage of the surfactant is 0.08 percent of the mass of the alumina solution; wherein the submicron alumina particles are alpha alumina crystal form submicron alumina particles with the particle size range of 100-300nm, the water-soluble resin is water-based epoxy resin, and the surfactant is sodium lauryl sulfate.

The performance index of the radiation resistant interlayer thermal protection material prepared in example 8 is shown in table 1.

Example 9

Example 9 is essentially the same as example 1, except that:

the third step is: adding submicron-grade alumina particles, nano alumina particles, water-soluble resin and tetraethoxysilane into water, and uniformly stirring (stirring time is 30min) to obtain a uniformly dispersed alumina solution; adding a surfactant into the alumina solution, uniformly stirring (stirring time is 30min), and carrying out ultrasonic treatment (ultrasonic treatment is 40min) to obtain uniformly dispersed alumina sol, wherein the alumina sol comprises alpha-phase alumina, amorphous alumina and amorphous silica; the alumina solution comprises the following components in percentage by mass: 65% of water; 10% of ethyl orthosilicate; 2.5% of water-soluble resin; the balance is submicron alumina particles and nanometer alumina particles, and the mass ratio of the submicron alumina particles to the nanometer alumina particles is 100: 35; the dosage of the surfactant is 0.08 percent of the mass of the alumina solution; wherein the submicron alumina particles are alpha alumina crystal form submicron alumina particles with the particle size range of 100-300nm, the nano alumina particles are amorphous alumina nano particles with the particle size range of 10-60nm, the water-soluble resin is water-based epoxy resin, and the surfactant is sodium lauryl sulfate.

The performance index of the radiation resistant interlayer thermal protection material prepared in example 9 is shown in table 1.

Example 10

Example 10 is essentially the same as example 1, except that:

the third step is: adding submicron-grade alumina particles, nano alumina particles and tetraethoxysilane into water, and uniformly stirring (stirring time is 30min) to obtain a uniformly dispersed alumina solution; adding a surfactant into the alumina solution, uniformly stirring (stirring time is 30min), and carrying out ultrasonic treatment (ultrasonic treatment is 40min) to obtain uniformly dispersed alumina sol, wherein the alumina sol comprises alpha-phase alumina, amorphous alumina and amorphous silica; the alumina solution comprises the following components in percentage by mass: 65% of water; 10% of ethyl orthosilicate; the balance is submicron alumina particles and nanometer alumina particles, and the mass ratio of the submicron alumina particles to the nanometer alumina particles is 100: 15; the dosage of the surfactant is 0.08 percent of the mass of the alumina solution; wherein the submicron alumina particles are alpha alumina crystal form submicron alumina particles with the particle size range of 100-300nm, the nano alumina particles are amorphous alumina nano particles with the particle size range of 10-60nm, and the surfactant is sodium lauryl sulfate.

The performance index of the radiation resistant interlayer thermal protection material prepared in example 10 is shown in table 1.

Example 11

Example 11 is essentially the same as example 1, except that:

the fourth step is: and (3) placing the heat insulation assembly obtained in the step (II) into the alumina sol obtained in the step (III) for vacuum impregnation, wherein the vacuum impregnation comprises the following steps: and (3) vacuumizing and soaking for 1h under the conditions that the temperature is 25 ℃ and the vacuum degree is 0.25MPa, and then drying the heat insulation assembly soaked with the alumina sol at 60 ℃ for 12h under the vacuumizing condition, and then drying at 120 ℃ for 6h to obtain the primary densified heat insulation assembly.

The performance index of the radiation resistant interlayer thermal protection material prepared in example 11 is shown in table 1.

Example 12

Example 12 is essentially the same as example 1, except that:

the step of: carrying out a grading heat treatment process on the material obtained in the fifth step to prepare a high-temperature resistant interlayer heat protection material; wherein the graded heat treatment system comprises a first temperature stage heat treatment and a second temperature stage heat treatment; the temperature of the first temperature stage heat treatment is 200 ℃, and the time of the first temperature stage heat treatment is 4 hours; the temperature of the second temperature stage heat treatment is 1100 ℃, and the time of the second temperature stage heat treatment is 6 h.

The performance index of the radiation resistant interlayer thermal protection material prepared in example 12 is shown in table 1.

Comparative example 1

Comparative example 1 is substantially the same as example 1 except that:

the aerogel heat insulation core layer material adopted in the step I is a silicon dioxide aerogel material in the prior art.

The performance indexes of the radiation-resistant interlayer thermal protection material prepared in the comparative example 1 are shown in table 1.

Comparative example 2

Comparative example 2 is substantially the same as example 1 except that:

and directly adopting the silica sol in the prior art to replace the alumina sol in the step III to dip the heat insulation component.

The performance indexes of the radiation-resistant interlayer thermal protection material prepared in the comparative example 2 are shown in table 1.

Comparative example 3

Comparative example 3 is substantially the same as example 1 except that:

the fiber fabric adopted in the second step is a fiber fabric woven by quartz fibers.

The performance indexes of the radiation-resistant interlayer thermal protection material prepared in the comparative example 3 are shown in table 1.

Comparative example 4

Comparative example 4 is substantially the same as example 1 except that:

the present comparative example does not include step (c) and step (viii).

The density of the high temperature resistant interlayer thermal protection material prepared in the comparative example 4 is 0.45g/cm³The service temperature is 1500 ℃, the service time is 1200s, the room temperature thermal conductivity is 0.044W/m.K, and the linear shrinkage rate is only 0.2%; the tensile strength of the high-temperature resistant interlayer thermal protection material at the heat resistance temperature of 1500 ℃ is 5MPa, the compression strength at the room temperature is 1.5MPa, the tensile strength of the high-temperature resistant interlayer thermal protection material prepared in the comparative example 1 at the room temperature comprises an upper panel of which the tensile strength is 85MPa, and the tensile strength at the heat resistance temperature of 1500 ℃ is 26 MPa.

The performance indexes of the high-temperature resistant interlayer thermal protection material prepared in the comparative example 4 are shown in the table 1.

In particular, the tensile strength at high temperature of the radiation resistant interlayer thermal protection material prepared in each example and comparative example in table 1 and the tensile strength at high temperature of the upper panel of the radiation resistant interlayer thermal protection material are tested to be the tensile strength at the heat resistant temperature; in table 1, "strong bond", "medium bond" and "weak bond" indicate the magnitude of the bonding strength between the panel and the aerogel thermal insulation core material, and "strong bond", "medium bond" and "weak bond" indicate that the bonding strength between the panel and the aerogel thermal insulation core material is decreased in the order of magnitude.

The invention has not been described in detail and is in part known to those of skill in the art.

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.