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Preparation method of polymer precursor ceramic aerogel

A precursor ceramic and aerogel technology, applied in the field of ceramic aerogel, can solve the problems of high oxygen content, low ceramic yield, insufficient purity of ceramic aerogel, etc., to achieve simplified process, high ceramic yield, shortening time The effect of preparation time

Active Publication Date: 2021-03-23
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ceramic airgel prepared by this method is not pure enough, the oxygen content is high, and the ceramic yield is low

Method used

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  • Preparation method of polymer precursor ceramic aerogel
  • Preparation method of polymer precursor ceramic aerogel
  • Preparation method of polymer precursor ceramic aerogel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Under the protection of nitrogen, 5 g of precursor polymers were uniformly dispersed in 95 g of n-hexane to obtain a precursor solution with a concentration of 5 wt %; 3 μL of 0.1 wt % Karstedt catalyst solution was added to the precursor solution, and under nitrogen protection, After stirring evenly, transfer it to a pressure reactor filled with nitrogen, and react at 160°C for 4 hours to obtain a light yellow silicon carbide precursor wet gel; after taking it out, soak it in cyclohexane for 2 days, and replace the cyclohexane 3 times; the wet gel was passed through supercritical CO 2 Dry 3 times, each time for 3 days, to obtain the silicon carbide precursor airgel; place the airgel in a high-temperature tube furnace, and raise the temperature to 1500°C at a rate of 3°C / min under high-purity argon, And keep it warm for 2 hours to obtain silicon carbide ceramic airgel. The obtained silicon carbide ceramic airgel has a density of 0.2g / cm 3 , with a specific surface are...

Embodiment 2

[0039] Under the protection of nitrogen, 20 g of the precursor polymer was uniformly dispersed in 80 g of tetrahydrofuran to obtain a precursor solution with a concentration of 20 wt %; 2 μL of 0.1 wt % Karstedt catalyst solution was added to the precursor solution, and stirred under the protection of nitrogen After uniformity, transfer to a pressure reactor filled with nitrogen, and react at 100 °C for 5 hours to obtain a light yellow silicon carbide precursor wet gel; after taking it out, soak it in tetrahydrofuran for 2 days, and replace tetrahydrofuran 3 times during the period; The silicon carbide precursor airgel was obtained by freeze-drying the gel; the airgel was placed in a high-temperature tube furnace, and under high-purity argon, the temperature was raised to 800°C at a rate of 5°C / min, and kept for 4h , to obtain silicon carbide ceramic airgel. The obtained silicon carbide ceramic airgel has a density of 0.361g / cm 3 , the specific surface area is 820m 2 / g, the...

Embodiment 3

[0041] Under the protection of nitrogen, 10 g of the precursor polymer was uniformly dispersed in 90 g of chloroform to obtain a precursor solution with a concentration of 10 wt %; 1 μL of 0.01 wt % Karstedt catalyst solution was added to the precursor solution, and the , after stirring evenly, transferred to a pressure reactor filled with nitrogen, and reacted at 200°C for 6 hours to obtain a light yellow silicon carbide precursor wet gel; after taking it out, soak it in chloroform for 2 days, and replace the chloroform during the process 3 times; pass the wet gel through supercritical CO 2 Dry 3 times, each time for 3 days, to obtain the silicon carbide precursor airgel; place the airgel in a high-temperature tube furnace, and raise the temperature to 1500°C at a rate of 6°C / min under high-purity argon, And keep it warm for 1 hour to obtain silicon carbide ceramic airgel. The obtained silicon carbide ceramic airgel has a density of 0.187g / cm 3 , the specific surface area i...

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Abstract

The invention provides a preparation method of polymer precursor ceramic aerogel, which comprises the following steps of: under the protection of inert atmosphere, uniformly dispersing polycarbosilaneas a polymer precursor in an organic solvent to prepare a precursor solution; placing the precursor solution in an inert atmosphere, selectively adding a platinum catalyst, and carrying out a hydrosilylation reaction to obtain precursor gel; drying the precursor gel to obtain precursor aerogel; and placing the precursor aerogel in an inert atmosphere for high-temperature cracking to obtain the ceramic aerogel. According to the method, the used raw materials are simple in composition, the precursor synthesis process is simple, additional vinyl substances are avoided, and the obtained silicon carbide ceramic aerogel is low in oxygen content, high in purity, adjustable in C / Si ratio and high in ceramic yield.

Description

technical field [0001] The invention belongs to the field of ceramic airgel, and relates to a preparation method of a polymer precursor ceramic airgel. Background technique [0002] Extreme environments such as rapid heat exchange and prolonged high temperature place stringent requirements on thermal insulation materials. Ceramic airgel is considered as a good thermal insulation material due to its low density, low thermal conductivity, high porosity, high specific surface area, excellent fire resistance and corrosion resistance. [0003] Polymer precursor ceramics are ceramic materials obtained by direct pyrolysis of polymer ceramic precursors, which can be used to prepare ceramic fibers, ceramic coatings, ceramic films, ceramic matrix composites, etc. Ceramic materials prepared by conversion of polymer precursors have great application prospects in the field of heat insulation materials due to their unique nano-multiphase structure, strong designability of precursors, goo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/571C04B35/622C04B38/00
CPCC04B35/571C04B35/622C04B38/0045C04B2235/77C04B2235/963C04B2235/6562C04B2235/6567C04B38/0054C04B38/0067
Inventor 贺丽娟黄红岩张恩爽权成刘圆圆张凡李文静杨洁颖赵英民张昊
Owner AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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