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CN-121989526-A - Ceramic fiber aerogel composite material with good high-temperature resistance and elasticity and preparation method thereof

CN121989526ACN 121989526 ACN121989526 ACN 121989526ACN-121989526-A

Abstract

The invention relates to the field of ceramic composite material preparation, and particularly discloses a ceramic fiber aerogel composite material with good high-temperature resistance and elasticity and a preparation method thereof, wherein the preparation method comprises the following steps of S1-ceramic nanofiber preparation, namely adding an aluminum source compound and glacial acetic acid into absolute ethyl alcohol to obtain an aluminum source mixed solution, adding the aluminum source mixed solution into a composite solution containing a silicon source compound, a catalyst and water, adding a spinning auxiliary agent, stirring for 5-10 h to obtain a precursor solution, carrying out electrostatic spinning to obtain the precursor nanofiber, calcining to obtain the ceramic nanofiber, S2-composite material preparation, namely soaking the ceramic nanofiber into a modified solution, adding a composite binder into the modified solution, stirring and dispersing, taking out after the ceramic nanofiber stays for 30-50 min, stacking layer by layer to form a layered three-dimensional structure, freezing for 5-10 min through liquid nitrogen, forming, freezing and drying for 20-30 h, and annealing in an inert atmosphere to obtain the composite material. The ceramic fiber aerogel composite material provided by the invention has high-temperature stability and excellent mechanical property and heat insulation property.

Inventors

  • ZHAO XINGLEI
  • JIANG PAN
  • WANG PENG
  • CHEN XINYI
  • JIANG XUBO

Assignees

  • 嘉兴富瑞邦新材料科技有限公司

Dates

Publication Date
20260508
Application Date
20260210

Claims (10)

  1. 1. The preparation method of the ceramic fiber aerogel composite material with good high-temperature resistance and elasticity is characterized by comprising the following steps: The preparation method of the S1-ceramic nanofiber comprises the steps of adding an aluminum source compound and glacial acetic acid into absolute ethyl alcohol to obtain an aluminum source mixed solution, adding the aluminum source mixed solution into a composite solution containing a silicon source compound, a catalyst and water, adding a spinning auxiliary agent, stirring for 5-10 hours to obtain a precursor solution, carrying out electrostatic spinning to obtain a precursor nanofiber, and calcining to obtain the ceramic nanofiber; and S2-preparing a composite material, namely immersing ceramic nano fibers in a modifying liquid, adding a composite binder, stirring and dispersing, taking out the ceramic nano fibers after the ceramic nano fibers stay for 30-50 min, stacking the ceramic nano fibers layer by layer to form a layered three-dimensional structure, freezing the layered three-dimensional structure by liquid nitrogen for 5-10 min for molding, freeze-drying the layered three-dimensional structure for 20-30 h, and finally annealing the layered three-dimensional structure in an inert atmosphere to obtain the composite material.
  2. 2. The preparation method of the ceramic fiber aerogel composite material with good high-temperature resistance and elasticity according to claim 1 is characterized in that in the step S1, the silicon source compound is ethyl orthosilicate, the aluminum source compound is isopropyl aluminum oxide, and the mass ratio of the silicon source compound to the aluminum source compound is (1-4): 1.
  3. 3. The preparation method of the ceramic fiber aerogel composite material with good high-temperature resistance and elasticity according to claim 1, wherein in the step S1, the spinning auxiliary agent is at least one of polyvinyl alcohol, polyvinylpyrrolidone and polyethylene oxide, and the mass ratio of the spinning auxiliary agent in a precursor solution is 5-20wt%.
  4. 4. The method for preparing a ceramic fiber aerogel composite material with good high-temperature resistance and elasticity according to claim 1, wherein in the step S2, the modifying liquid is an aqueous suspension of carbon nanofibers.
  5. 5. The method for preparing the ceramic fiber aerogel composite material with good high-temperature resistance and elasticity according to claim 4, wherein in the step S2, the mass ratio of the ceramic nanofibers to the carbon nanofibers in the aqueous suspension of the nanofibers is (1-2.3): 1.
  6. 6. The method for preparing the ceramic fiber aerogel composite material with good high-temperature resistance and elasticity according to claim 1, wherein in the step S2, the composite binder is a mixture of aluminum dihydrogen phosphate and a modified silicon binder.
  7. 7. The method for preparing the ceramic fiber aerogel composite material with good high-temperature resistance and elasticity according to claim 6, wherein the preparation steps of the modified silicon binder are as follows: (1) Sequentially adding toluene, hydroxyl-terminated polydimethylsiloxane, methyltrimethoxysilane, silicon nitride and simethicone into a reactor, stirring for 10-30 min, stirring for 20-30 min under a vacuum degree of 0.04-0.08 MPa, adding an organosilicon cross-linking agent and a catalyst 2, and stirring for 10-20 min to obtain a mixture; (2) And (3) adding polyacrylamide and deionized water into a reactor, stirring for 2-6 hours, adding the mixture obtained in the step (1), and stirring for 1-2 hours to obtain the modified silicon binder.
  8. 8. The preparation method of the ceramic fiber aerogel composite material with good high-temperature resistance and elasticity, which is characterized in that in the step (1), the mass ratio of the hydroxyl-terminated polydimethylsiloxane to the methyltrimethoxysilane to the silicon nitride is 10 (0.2-0.5): 2-8.
  9. 9. The method for preparing the ceramic fiber aerogel composite material with good high-temperature resistance and elasticity according to claim 7, wherein in the step (2), the addition amount of the polyacrylamide is 1-2 times of the mass of the mixture.
  10. 10. A ceramic fiber aerogel composite with good high-temperature resistance and elasticity according to any one of claims 1 to 9, wherein the ceramic fiber aerogel composite at least comprises the following properties of plastic deformation less than or equal to 14.5% under 1000-cycle compression condition with strain of 60%, volume loss rate of calcination at 1300 ℃ for 1h less than or equal to 18.4%, and thermal conductivity of 0.025-0.043W/(mK).

Description

Ceramic fiber aerogel composite material with good high-temperature resistance and elasticity and preparation method thereof Technical Field The invention relates to the field of ceramic composite material preparation, and particularly discloses a ceramic fiber aerogel composite material with good high-temperature resistance and elasticity and a preparation method thereof. Background The aerogel is a nanometer advanced material with a three-dimensional network structure, the space network structure is filled with air medium, the advantages of high porosity, low density, low heat conductivity and the like are achieved, the heat preservation and insulation performance is excellent, the ceramic fiber material has the advantages of good continuity, excellent mechanical property and the like, therefore, the aerogel and the ceramic fiber material are compositely used, the ceramic fiber material is used as reinforcement and is doped into the aerogel, and the novel composite material with more excellent mechanical property and thermal property is a hot spot studied in the current heat insulation material. According to the element types, the traditional ceramic aerogel composite material can be divided into a single ceramic aerogel, a binary ceramic aerogel, a ternary ceramic aerogel and a multi-element ceramic aerogel, and the ceramic aerogel composite material has more excellent performance due to the element composition of different types and numbers. The invention patent with the application number 202311144000.4 discloses a preparation method of a silica ceramic fiber aerogel heat insulation film, which comprises the following steps of preparing spinning solution by a sol-gel method, dissolving a zirconium source in water, adding a phase inhibitor to form solution A, dissolving a silicon source in water to form solution B, mixing the solution A and the solution B, adding a polymer template, uniformly mixing to obtain the spinning solution, preparing a precursor film by electrostatic spinning, calcining the precursor film, and hydrophobically modifying the fiber film. The heat insulation film disclosed by the invention is a zirconia-silica ceramic fiber film, zirconia mainly exists in a tetragonal crystal form in silica-doped zirconia fibers, and the flexibility and the continuity of the fibers are better through air flow assisted electrostatic spinning. The silicon, zirconium and yttrium in the heat insulation film are uniformly distributed in the fiber, so that the heat insulation film has uniform texture and good comprehensive performance. However, as the interface bonding effect between the fiber and the aerogel is unstable, the composite material is extremely easy to fall off powder only by carrying out hydrophobic modification on the obtained fiber membrane, and in addition, the mechanical property of the composite material still has room for improvement. In view of the above, the invention discloses a ceramic fiber aerogel composite material with good high-temperature resistance and elasticity. Disclosure of Invention Aiming at the defects of the prior art, the invention discloses a ceramic fiber aerogel composite material with good high-temperature resistance and elasticity and a preparation method thereof. The ceramic fiber aerogel composite material provided by the invention has high stability at high temperature, and has excellent mechanical property and heat insulation property. In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the invention provides a preparation method of a ceramic fiber aerogel composite material with good high-temperature resistance and elasticity, which comprises the following steps: The preparation method of the S1-ceramic nanofiber comprises the steps of adding an aluminum source compound and glacial acetic acid into absolute ethyl alcohol to obtain an aluminum source mixed solution, adding the aluminum source mixed solution into a composite solution containing a silicon source compound, a catalyst and water, adding a spinning auxiliary agent, stirring for 5-10 hours to obtain a precursor solution, carrying out electrostatic spinning to obtain a precursor nanofiber, and calcining to obtain the ceramic nanofiber; and S2-preparing a composite material, namely immersing ceramic nano fibers in a modifying liquid, adding a composite binder, stirring and dispersing, taking out the ceramic nano fibers after the ceramic nano fibers stay for 30-50 min, stacking the ceramic nano fibers layer by layer to form a layered three-dimensional structure, freezing the layered three-dimensional structure by liquid nitrogen for 5-10 min for molding, freeze-drying the layered three-dimensional structure for 20-30 h, and finally annealing the layered three-dimensional structure in an inert atmosphere to obtain the composite material. Preferably, the technological parameters of the electrostatic spinning are that the inner diameter of an injection nee