CN115246745B - High-temperature-resistant composite component aerogel material and preparation method thereof - Google Patents
High-temperature-resistant composite component aerogel material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-temperature-resistant composite component aerogel material and a preparation method thereof. The method comprises the following steps: preparing a nano oxide dispersion liquid; uniformly mixing the oxide dispersion liquid and the adsorbent through high-speed shearing stirring and ultrasonic treatment to obtain a mixed solution; putting the solution in a closed container for high-temperature hydrothermal reaction to obtain a semisolid gel block; and then carrying out low-density silica sol precursor dipping treatment, aging and drying, then carrying out a heat treatment process, and then carrying out a chemical vapor deposition process and carrying out pyrolysis to prepare the high-temperature-resistant composite component aerogel material. The preparation method can obtain the high-temperature-resistant composite component aerogel material with the temperature resistance of more than 1600 ℃ and high toughness.
Description
Technical Field
The invention relates to the technical field of aerogel preparation, in particular to a high-temperature-resistant composite component aerogel 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 material reaches 80-99.8%, the typical size of the pores is 1-100 nm, and the specific surface area is 200-1000 m 2 A density of as low as 3kg/m 3 The room temperature thermal conductivity coefficient can be as low as 0.012W/m.k. Due to the characteristics, the aerogel material is thermally, acoustically, optically,Has wide application potential in the aspects of micro-electronics 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.
Most of traditional aerogel materials are pearl necklace-shaped structures formed by accumulating nano particles, the aerogel materials with the structures are brittle, and line reinforcement is needed in practical application to achieve structure reinforcement. The structural strength of the aerogel can be effectively improved by adopting a line reinforcing mode, however, the existing RTM (resin transfer molding) process for pressing and injecting glue has requirements on the thickness and the shape of the material, and the problem of internal defects often exists in the material with large size and large thickness. The nanowire aerogel is a novel aerogel material, nanowires are used as basic units, and a three-dimensional network structure with a high specific surface area can be obtained by mutually lapping and winding. Compared with the traditional pearl necklace-shaped aerogel material, the nanowire aerogel has the advantages that the structural strength is improved, the process complexity is reduced, and the problem of powder falling of the traditional aerogel material can be solved. In addition, the three-dimensional network framework of the material has good toughness, can be machined in various shapes and with high precision, and the material is not limited by thickness, size and shape.
While the preparation method of oxide nanowires or nanowires often relies on solvothermal or electrospinning, the prepared nanowires or nanowire components often are amorphous oxides. This means that they undergo a crystal transformation at a temperature, typically a temperature above 1000 f; the transformation process of the crystal form is accompanied with structural collapse or agglomeration, and the micro-morphology of the aerogel is influenced. With the development of aircrafts, higher requirements are provided for the temperature resistance of heat insulation materials, and the temperature resistance of the existing materials cannot meet the requirements, so that the aerogel materials with higher temperature resistance level (more than or equal to 1600 ℃) need to be prepared.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a composite component aerogel material with high toughness and high temperature resistance and a preparation method thereof.
In the invention, the steps of micron-scale wire in-situ growth gel, low-density silica sol precursor doping and chemical vapor carbon deposition are designed, and the aluminum oxide nanowire is converted into a more temperature-resistant alpha phase under the condition of outer layer coating through a heat treatment process, and an outer shell layer is converted into a more temperature-resistant silicon carbide phase. By utilizing the high strength and toughness and high-temperature components of the core-shell structure nanowire, the preparation method can realize the preparation of the aerogel material with the temperature resistance of more than 1600 ℃.
The invention provides a preparation method of a high-temperature-resistant composite component aerogel material with temperature resistance of more than 1600 ℃ and high toughness in a first aspect, which comprises the following steps:
(1) Mixing the alumina nano powder and the acidic solution in deionized water to obtain a mixed solution;
(2) Placing the mixed solution in a closed container for hydrothermal reaction to obtain semisolid gel blocks;
(3) Placing the gel block in a low-density silica sol precursor solution for dipping treatment, sealing the dipped gel block, and performing aging treatment;
(4) Carrying out a solvent replacement process and a supercritical drying step on the gel block after the aging treatment to prepare a nanowire composite aerogel material;
(5) Carrying out heat treatment on the prepared nanowire composite aerogel material;
(6) Carrying out chemical vapor deposition treatment on the nanowire composite aerogel material after the heat treatment;
(7) And (3) carrying out high-temperature pyrolysis on the nanowire composite aerogel material subjected to the chemical vapor deposition treatment to obtain the high-temperature-resistant composite component aerogel material.
Preferably, in the step (1), the alumina nano powder and the acidic solution are mixed in deionized water, and a mixed solution is obtained by stirring and ultrasonic processing.
Preferably, the specific steps of step (1) are: dissolving alumina nano powder with the diameter of 10-100nm in water, adding 0.1-30mmol/L sulfuric acid solution (wherein the total solution is a solution formed by the alumina nano powder, the water and the sulfuric acid) accounting for 1% of the total solution mass, stirring and ultrasonically treating to obtain a mixed solution, adding loose fiber cotton with the diameter of 2-10 mu m and the length of 3-5mm, and dispersing in a high-speed dispersion machine at the rotating speed of 1000-8000r/min for 5-120min, wherein the mass fraction of the nano powder in the mixed solution is 5-20%.
Preferably, the step (2) is to put the mixed solution into a closed container to carry out hydrothermal reaction for 1-48h at 150-300 ℃ to obtain semisolid gel blocks.
Preferably, the specific steps of step (2) are: the reaction needs to be carried out under a fully-closed condition, and the material of the container needs to ensure that the polymer material does not react with the system.
Preferably, the gel block is placed in a low-density silica sol precursor solution in the step (3) and soaked for 6-72h, and then the block body is placed in a container and aged for 2-48h in an oven at 90 ℃ after being sealed.
Preferably, the specific steps of step (3) are: and (3) placing the gel block obtained in the step (2) into a prepared low-density silica sol precursor solution (with solid content of 2-10%) to be soaked for 6-72h, then adding 0.5-2mol/L ammonium fluoride solution as a catalyst according to the proportion of 100.
Preferably, the specific steps of step (4) are: and the solvent replacement adopts ethanol as a solvent, and after 3 times of replacement is carried out according to 10 times of the volume of the gel block, the supercritical drying process of carbon dioxide is carried out. The supercritical drying temperature is 20-60 deg.C, and the pressure is 10-16Mpa.
Preferably, the step (5) is used for carrying out heat treatment on the nanowire composite aerogel material prepared in the step (4), wherein the heat treatment system is carried out in an air atmosphere, the treatment temperature is 1000-1200 ℃, and the treatment time is 0.5-2h.
Preferably, the step (6) is to perform chemical vapor deposition treatment on the nanowire composite aerogel material prepared in the step (5) under the condition of propane (flow rate of 0.2-2 m) 3 H) and argon (flow rate of 0.2-2 m) 3 H) mixed gas, the deposition time is 0-10h, and the deposition temperature is 900-1200 ℃.
Preferably, in the step (7), the nanowire composite aerogel material obtained in the step (6) is put in nitrogen (or argon-hydrogen mixed gas) to be cracked for 0.2 to 48 hours at the temperature of 1200 to 1600 ℃.
The preparation of the high-temperature-resistant composite component aerogel material is realized through the steps.
In a second aspect, the invention provides a high temperature resistant composite component aerogel 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) Compared with the traditional pearl necklace-shaped aerogel material, the pearl necklace-shaped aerogel material has better mechanical strength, the microstructure is formed by mutually winding the nanowires, and the nanowires are bound through the chemical vapor deposition process, so that the structural strength of the material is effectively improved.
(2) The density of the aerogel material prepared by the invention can be as low as 0.16g/cm 3 Compared with other low-density aerogel materials with the same strength, the aerogel material has the characteristic of ultralow density.
(3) The gel process in the preparation method of the aerogel is a hydrothermal process, is different from the traditional RTM (resin transfer molding) pressing glue injection process, is not limited by the shape and size of the reinforcement, and can be used for preparing aerogel materials with any shape and thickness.
(4) In the preparation process, the aerogel material obtained from the gelling and post-treatment processes to the supercritical drying does not have any size shrinkage, the net size molding of the product can be realized, and the problems of cost and cycle increase caused by the machining process are solved.
(5) According to the invention, after the hydrothermal reaction, the post-treatment process of the gel block is set, and the aim is to grow a silicon oxide layer in the nanowire gel block, wherein the silicon oxide layer can form a more temperature-resistant silicon carbide phase with carbon in the subsequent sintering process, so that the overall strength and the temperature resistance of the material are improved.
(6) Different from the preparation of the high-temperature resistant aerogel heat insulation material by a doping modification mode, the invention provides the preparation of the aerogel material with stable structure by a nanowire self-supporting mode for high-temperature resistant high-efficiency heat insulation application, and the improvement method is more feasible. The self-supporting refers to that the unique self microstructure of the material can enable the material to have certain strength without an additional support body.
(7) In the preparation process, the alumina nanowires are coated by the silicon dioxide and the carbon, and the conversion from a gamma phase to an alpha phase is completed under the physical barrier and shape fixation of the silicon dioxide and the carbon, so that the structural collapse in the crystal form conversion process is avoided. After high-temperature treatment, the composite component can form alpha alumina phase and silicon carbide phase which are more temperature-resistant, and the temperature resistance of the material can be effectively improved.
(8) The invention can adopt water phase as reaction medium, and avoids environmental pollution and waste caused by using organic solvent in the preparation process.
(9) The aerogel material prepared by the method disclosed by the invention has excellent high temperature resistance on the premise of keeping low thermal conductivity of less than 0.029W/m.K, and can be used for heat insulation at 1600 ℃ for a long time.
(10) The aerogel prepared by the method contains uniformly dispersed silicon carbide components, has a good radiation-resistant effect, and is beneficial to improving the heat-insulating property of the material at high temperature.
Drawings
FIG. 1 is a flow chart of a preparation scheme of the present invention.
FIG. 2 is a schematic diagram of the structure of the aerogel prepared according to 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 should be apparent that the described embodiments are only some of the embodiments of the present invention, and not all of them. 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 composite component aerogel material in a first aspect, the flow of which is shown in figure 1, the structure of the product obtained in each step is shown in figure 2, and the method comprises the following steps:
(1) Mixing the alumina nano powder and the acid solution in deionized water, and obtaining a mixed solution through stirring (high-speed shearing and stirring) and ultrasound.
The method comprises the following specific steps: dissolving 10-100nm diameter alumina nanometer powder in water, adding 0.1-30mmol/L sulfuric acid solution with the total solution mass of 1%, the nanometer powder mass fraction in the mixed solution is 5-20%, adding 2-10 μm diameter and 3-5mm length fiber loose cotton, and dispersing in a high speed dispersion machine at 1000-8000r/min for 5-120min.
Wherein, the alumina nano powder is used as an adsorbent, and the loose fiber cotton is used as a reinforcement. The loose fiber is short tangent line, the length-diameter ratio of the lines is small, no obvious lap joint structure exists between the lines, and the function of the loose fiber is to toughen the nano-wire aerogel to a certain extent.
(2) Placing the above mixed solution in a sealed container, and performing hydrothermal reaction at 150-300 deg.C for 1-48h to obtain semisolid gel block. As shown in fig. 2, the alumina nanowire aerogel is obtained by this step.
The method comprises the following specific steps: the reaction needs to be carried out under fully closed conditions, and the material of the container needs to be a polymer material which does not react with the system.
(3) And (3) placing the gel block in a low-density silica sol precursor solution for dipping treatment, soaking for 6-72h, then placing the block in a container for sealing, and aging for 2-48h in a 90 ℃ oven.
Wherein, the specific steps for carrying out the dipping treatment are as follows: and (3) placing the gel block obtained in the step (2) into a prepared low-density silica sol precursor solution (with solid content of 2-10%) for 6-72h, then adding 0.5-2mol/L ammonium fluoride solution as a catalyst according to the proportion of 100. Wherein the ammonium fluoride solution is used for promoting the condensation of the low-density silica sol precursor, so that the surface of the nanowire is uniformly coated with the silicon dioxide.
(4) And (4) carrying out a solvent replacement process and a supercritical drying step on the treated gel block obtained in the step (3) to obtain the nanowire composite aerogel material.
The method comprises the following specific steps: and the solvent replacement adopts ethanol as a solvent, and after 3 times of replacement is carried out according to 10 times of the volume of the gel block, the supercritical drying process of carbon dioxide is carried out. The supercritical drying temperature is 20-60 deg.C, and the pressure is 10-16Mpa.
As shown in fig. 2, silicon coating is achieved through steps (3) and (4), and silica-amorphous alumina nanowire aerogel is obtained.
(5) And (3) carrying out heat treatment on the aerogel, wherein the treatment system is that the treatment temperature is 1000-1200 ℃ and the treatment time is 0.5-2h in an air atmosphere. As shown in fig. 2, silica-gamma alumina nanowire aerogel is obtained by this step.
(6) Subjecting the obtained aerogel to chemical vapor deposition under the condition of propane (flow rate of 0.2-2 m) 3 H) and argon (0.2-2 m) 3 H) mixed gas, the deposition time is 0-10h, and the deposition temperature is 900-1200 ℃. As shown in fig. 2, a carbon-silica-gamma alumina nanowire aerogel is obtained through this step.
(7) And (3) putting the aerogel material obtained in the step (6) into nitrogen (or argon-hydrogen mixed gas) for cracking for 0.2-48h at the temperature of 1200-1600 ℃. As shown in fig. 2, a silicon carbide-silica-alpha alumina nanowire aerogel was obtained by this step.
The invention provides a high-temperature-resistant composite component aerogel material in a second aspect, and the preparation of the high-temperature-resistant composite component aerogel material is realized through the steps.
The invention will be further illustrated by way of example, but the scope of protection is not limited to these examples.
Example 1
(1) Mixing the alumina nano powder and the acid solution in deionized water, and stirring and ultrasonically treating to obtain a mixed solution.
The method comprises the following specific steps: dissolving aluminum oxide nano powder with the diameter of 10-15nm in water, adding 10mmol/L sulfuric acid solution accounting for 1% of the total solution mass, and stirring and ultrasonically processing to obtain a mixed solution, wherein the mass fraction of the nano powder in the mixed solution is 8%. Adding loose fiber cotton with diameter of 7 μm and length of 3-5mm, and dispersing in a high-speed disperser at rotation speed of 5000r/min for 30min.
(2) Placing the mixed solution in a closed container, and performing hydrothermal reaction at 230 ℃ for 5h to obtain a semisolid gel block.
The method comprises the following specific steps: the reaction needs to be carried out under fully closed conditions, and the material of the container needs to be a polymer material which does not react with the system.
(3) And (3) placing the gel block in a low-density silica sol precursor solution, soaking for 24h, then adding a catalyst, uniformly mixing, placing the block in a container, sealing, and aging in an oven at 90 ℃ for 24h.
The method comprises the following specific steps: preparing a low-density silica sol precursor (solid content is 5%); after the gel block is completely impregnated, 1.5mol/L ammonium fluoride solution is added as a catalyst according to the proportion of 100. The gel block is immersed in the solution with the liquid level passing over the gel block.
(4) Carrying out a solvent replacement process and a supercritical drying step on the treated gel block obtained in the step (3) to prepare a high-temperature-resistant composite component aerogel material;
the method comprises the following specific steps: and the solvent replacement adopts ethanol as a solvent, and after 3 times of replacement is carried out according to 10 times of the volume of the gel block, the supercritical drying process of carbon dioxide is carried out. The supercritical drying temperature is 50 deg.C, and the pressure is 14Mpa.
(5) And (3) carrying out heat treatment on the aerogel, wherein the treatment system is that the treatment temperature is 1100 ℃ and the treatment time is 0.5h under an air atmosphere.
(6) The obtained aerogel was subjected to a chemical vapor deposition treatment under the condition of propane (flow rate of 1.0 m) 3 H) and argon (1.3 m) 3 H) mixed gas, the deposition time is 2h, and the deposition temperature is 1020 ℃.
(8) And (3) putting the aerogel material obtained in the step (6) into nitrogen (or argon-hydrogen mixed gas) for cracking for 2 hours at the temperature of 1400 ℃.
The aerogel material prepared in example 1 has good structural strength, and the heat insulation performance test of the high-temperature-resistant composite component aerogel material prepared in example 1 shows that the surface of the aerogel material has no light loss, no color change and no shedding, and other performance indexes are shown in table 1.
Example 2
Example 2 is essentially the same as example 1, except that: in the preparation process of the nano dispersion liquid in the step 1, a 10mmol/L sulfuric acid solution with the total solution mass of 0.5 percent is added.
The nano aerogel material prepared in example 2 is tested, the strength is weak, the chalking phenomenon exists, and other performance indexes are shown in table 1.
Example 3
Example 3 is essentially the same as example 1, except that: in the preparation process of the nano dispersion liquid in the step 1, a sulfuric acid solution with the concentration of 10mmol/L and the mass of the total solution of 20% is added.
The nano aerogel material prepared in example 3 is tested, the strength is weak, the chalking phenomenon exists, and other performance indexes are shown in table 1.
Example 4
Example 4 is essentially the same as example 1, except that: and (3) preparing the nano aerogel material at the temperature of 200 ℃ in the hydrothermal reaction in the step (2).
The nano aerogel material prepared in example 4 is tested, the strength is weak, the chalking phenomenon exists, and other performance indexes are shown in table 1.
Example 5
Example 5 is essentially the same as example 1, except that: and (3) performing hydrothermal reaction for 3 hours in the step 2 to obtain the nano aerogel material.
The nano aerogel material prepared in example 5 is tested, and the aerogel is relatively weak in strength and has a chalking phenomenon, and other performance indexes are shown in table 1.
Example 6
Example 6 is essentially the same as example 1, except that: and (4) preparing the high-temperature-resistant composite component aerogel material without the step (3).
The aerogel material prepared in example 6 was tested and found to maintain structural integrity and other performance criteria as shown in table 1.
Example 7
Example 7 is essentially the same as example 1, except that: and (5) preparing the nanowire aerogel material without performing the solvent replacement process in the step (4).
The nanowire aerogel material prepared in example 7 was tested and found to be powdered and difficult to form, and other performance indexes are shown in table 1.
Example 8
Example 8 is essentially the same as example 1, except that: and 4, performing normal-pressure drying instead of the supercritical drying process in the step 4 to obtain the nanowire aerogel composite material.
The nanowire aerogel material prepared in example 8 was tested to have large shrinkage and high density, and other performance indexes are shown in table 1.
Example 9
Example 9 is essentially the same as example 1, except that: and (4) preparing the nanowire aerogel material without performing the heat treatment process in the step (5).
The nanowire aerogel composite material prepared in example 9 was tested to have no chalking, no shrinkage and good moldability, and other performance indexes are shown in table 1.
Example 10
Example 10 is essentially the same as example 1, except that: and (4) preparing the nanowire aerogel material without carrying out the vapor deposition process in the step 6.
The nanowire aerogel composite prepared in example 10 was tested to have no chalking, no shrinkage and good moldability, and other performance indexes are shown in table 1.
Example 11
Example 11 is essentially the same as example 1, except that: and (6) the time of the vapor deposition process in the step 6 is 24 hours, and the nanowire aerogel material is prepared.
The nanowire aerogel composite material prepared in example 11 was tested to have no chalking, no shrinkage and good moldability, and other performance indexes are shown in table 1.
Example 12
Example 12 is essentially the same as example 1, except that: and (4) preparing the nanowire aerogel material without carrying out the pyrolysis process of the step (7).
The nanowire aerogel composite material prepared in example 12 was tested to have no chalking, no shrinkage and good moldability, and other performance indexes are shown in table 1.
Example 13
Example 13 is essentially the same as example 1, except that: and (2) adding a sulfuric acid solution which accounts for 0.1mmol/L of the total solution in an amount of 1% by mass into the reaction system in the step (1) to prepare the nanowire aerogel material.
When the nanowire aerogel composite material prepared in example 13 is tested, the material has poor pulverization and formability, and other performance indexes are shown in table 1.
Example 14
Example 14 is essentially the same as example 1, except that: and (3) soaking the gel block in the low-density silica sol precursor solution (with the solid content of 10%) for 72h to prepare the nanowire aerogel material.
The nanowire aerogel composite prepared in example 14 was tested for non-chalking and good moldability, and other performance indexes are shown in table 1.
Example 15
Example 15 is essentially the same as example 1, except that: and (3) adding 2mol/L ammonium fluoride solution as a catalyst into the reaction system in the step (3) to prepare the nanowire aerogel material.
The nanowire aerogel composite material prepared in example 15 was tested, and the nanowire aerogel composite material was free of chalking and good in moldability, and other performance indexes are shown in table 1.
Example 16
Example 16 is essentially the same as example 1, except that: and (5) the deposition time of the step 6 is 10 hours, and the nanowire aerogel material is prepared.
The nanowire aerogel composite prepared in example 16 was tested for non-chalking and good moldability, and other performance indicators are shown in table 1.
Comparative examples 1 to 3:
comparative examples 1, 2 were prepared according to the methods of examples 1, 2 in CN108249901A, i.e. aerogel materials were prepared by successively carrying out the following steps: sol preparation, nanocrystal self-assembly process, gelation and aging, solvent replacement, supercritical drying and heat treatment process.
Comparative example 3 was prepared according to the method of example 1 in CN110282958A, i.e. the aerogel material was prepared successively through the following steps: the preparation method comprises the following steps of preparation of the special-shaped nanocrystal dispersion liquid, a special-shaped nanocrystal self-assembly process, a gelation reaction process, an aging process, a drying process and a post-treatment process.
Table 1: performance indexes of high-temperature-resistant composite-component aerogel materials prepared in various examples and high-temperature-resistant aerogel materials prepared in comparative examples
Where "-" indicates that no relevant data is available.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, and 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 (9)
1. The preparation method of the high-temperature-resistant composite component aerogel material is characterized by comprising the following steps of:
mixing the alumina nano powder and the acid solution in deionized water to obtain a mixed solution;
placing the mixed solution in a closed container for hydrothermal reaction to obtain semisolid gel blocks;
placing the gel block in a low-density silica sol precursor solution for dipping treatment, sealing the dipped gel block, and performing aging treatment;
carrying out a solvent replacement process and a supercritical drying step on the aged gel block to prepare a nanowire composite aerogel material;
carrying out heat treatment on the prepared nanowire composite aerogel material;
carrying out chemical vapor deposition treatment on the nanowire composite aerogel material after the heat treatment;
carrying out high-temperature pyrolysis on the nanowire composite aerogel material subjected to chemical vapor deposition treatment to obtain a high-temperature-resistant composite component aerogel material;
mixing the alumina nano powder and the acid solution in deionized water to obtain a mixed solution, wherein the mixed solution comprises: dissolving alumina nano powder with the diameter of 10-100nm in deionized water, adding 0.1-30mmol/L sulfuric acid solution accounting for 1% of the total solution mass, stirring and ultrasonically treating to obtain a mixed solution, adding loose fiber cotton with the diameter of 2-10 mu m and the length of 3-5mm, and dispersing in a high-speed dispersion machine at the rotating speed of 1000-8000r/min for 5-120min, wherein the mass fraction of the nano powder in the mixed solution is 5-20%.
2. The method according to claim 1, wherein the hydrothermal reaction is carried out in a closed container at 150-300 ℃ for 1-48h.
3. The method of claim 1, wherein the placing the gel mass in a low density silica sol precursor solution for an impregnation process comprises: and (3) placing the gel block in a low-density silica sol precursor solution for 6-72h, adding 0.5-2mol/L ammonium fluoride solution serving as a catalyst, mixing for 1-24h, and carrying out gel reaction.
4. The method according to claim 1, wherein the aging treatment is an aging treatment in an oven at 90 ℃ for 2 to 48 hours.
5. The method according to claim 1, wherein the gel block after aging treatment is subjected to a solvent substitution process and a supercritical drying step, wherein the solvent substitution is performed 3 times by using ethanol as a solvent and performing the substitution by 10 times the volume of the gel block, and then a carbon dioxide supercritical drying process is performed; the supercritical drying temperature is 20-60 deg.C, and the pressure is 10-16Mpa.
6. The method according to claim 1, wherein the heat treatment is carried out under an air atmosphere at a treatment temperature of 1000 to 1200 ℃ for a treatment time of 0.5 to 2 hours.
7. The method according to claim 1, wherein the chemical vapor deposition treatment adopts a mixed gas of propane and argon, the deposition time is 0-10h, and the deposition temperature is 900-1200 ℃.
8. The method of claim 1, wherein the pyrolysis is carried out in nitrogen, argon, or a mixture of argon and hydrogen for 0.2 to 48 hours at 1200 to 1600 ℃.
9. A high temperature resistant composite component aerogel material prepared according to the method of any of claims 1-8.
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| CN115246745A (en) | 2022-10-28 |
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