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Preparation process of silicon-based ceramic aerogel based on ceramic sintering technology

A preparation process and airgel technology, which is applied in the field of silicon-based ceramic airgel preparation technology, can solve the problems that the use temperature is difficult to exceed 1000°C, the use temperature of airgel is not high, and the pores are easy to collapse and break, and achieve microscopic Perfect structure, reduced particle size, and reduced crystallization barrier

Pending Publication Date: 2019-11-26
JIANGSU MIRAFUL NANO MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the heat treatment temperature generally does not exceed 500°C. If the heat treatment temperature is too high, the nanoscale pores will collapse and cause the airgel to be completely densified.
Therefore, the service temperature of airgel is not high. Even after heat treatment, its service temperature is difficult to exceed 1000 ℃, and the mechanical properties of airgel products are not good, and the air pores are easy to collapse and break under the action of external force.

Method used

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  • Preparation process of silicon-based ceramic aerogel based on ceramic sintering technology

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Embodiment 1

[0029] A preparation process of silicon-based ceramic airgel based on ceramic sintering technology, comprising the following steps:

[0030] Step S1, weighing the following raw materials by weight: 10 parts of ethyl orthosilicate, 50 parts of deionized water, 50 parts of absolute ethanol, 15 parts of zirconium oxychloride, 10 parts of zirconium nitrate, 3 parts of sodium fluoride, 3 parts of Silicon oxide, 5 parts silicon nitride, 30 parts glycerin and 50 parts trimethylchlorosilane;

[0031] Step S2, add tetraethyl orthosilicate, deionized water and absolute ethanol into the beaker, heat in a constant temperature water bath at 50°C and magnetically stir at a speed of 120r / min, add 10% ammonia water dropwise until flocs appear in the beaker, Add 10% dilute hydrochloric acid to adjust the pH until the pH is 5.6, mix zirconium oxychloride and zirconium nitrate into the beaker, add sodium fluoride, and stir magnetically at a speed of 150r / min until a colloid is formed;

[0032] ...

Embodiment 2

[0040] A preparation process of silicon-based ceramic airgel based on ceramic sintering technology, comprising the following steps:

[0041] Step S1, weighing the following raw materials by weight: 12 parts of ethyl orthosilicate, 55 parts of deionized water, 52 parts of absolute ethanol, 16 parts of zirconium oxychloride, 10 parts of zirconium nitrate, 4 parts of sodium fluoride, 5 parts of Silicon oxide, 6 parts silicon nitride, 35 parts glycerin and 55 parts trimethylchlorosilane;

[0042] Step S2, add tetraethyl orthosilicate, deionized water and absolute ethanol into the beaker, heat in a constant temperature water bath at 50°C and magnetically stir at a speed of 120r / min, add 10% ammonia water dropwise until flocs appear in the beaker, Add 10% dilute hydrochloric acid to adjust the pH until the pH is 5.6, mix zirconium oxychloride and zirconium nitrate into the beaker, add sodium fluoride, and stir magnetically at a speed of 150r / min until a colloid is formed;

[0043] ...

Embodiment 3

[0047] A preparation process of silicon-based ceramic airgel based on ceramic sintering technology, comprising the following steps:

[0048] Step S1, weighing the following raw materials by weight: 13 parts of ethyl orthosilicate, 60 parts of deionized water, 65 parts of absolute ethanol, 18 parts of zirconium oxychloride, 11 parts of zirconium nitrate, 4 parts of sodium fluoride, 6 parts of Silicon oxide, 6 parts silicon nitride, 45 parts glycerin and 65 parts trimethylchlorosilane;

[0049] Step S2, add tetraethyl orthosilicate, deionized water and absolute ethanol into the beaker, heat in a constant temperature water bath at 50°C and magnetically stir at a speed of 120r / min, add 10% ammonia water dropwise until flocs appear in the beaker, Add 10% dilute hydrochloric acid to adjust the pH until the pH is 5.6, mix zirconium oxychloride and zirconium nitrate into the beaker, add sodium fluoride, and stir magnetically at a speed of 150r / min until a colloid is formed;

[0050] ...

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Abstract

The invention discloses a preparation process of a silicon-based ceramic aerogel based on ceramic sintering technology. The process includes: weighing the following raw materials by weight: 10-15 parts of tetraethyl orthosilicate, 50-65 parts of deionized water, 50-70 parts of anhydrous ethanol, 15-20 parts of zirconium oxychloride, 10-12 parts of zirconium nitrate, 3-5 parts of sodium fluoride, 3-8 parts of silicon oxide, 5-8 parts of silicon nitride, 30-50 parts of glycerin and 50-70 parts of trimethylchlorosilane. Glycerin and trimethylchlorosilane are utilized for replacement, thus strengthening the network structure of gel, at the same time reducing the additional pressure of capillaries in the gel network, effectively avoiding gel collapse during pumping filtration, and solving the technical problems that the aerogel obtained after drying has poor strength, toughness and other mechanical properties, the heat treatment temperature is too high, nanoscale holes can collapse so as tocause complete densification of aerogel, and the air holes of aerogel easily collapse and break.

Description

technical field [0001] The invention belongs to the field of airgel preparation, in particular to a silicon-based ceramic airgel preparation process based on ceramic sintering technology. Background technique [0002] Due to the characteristics of light weight, large specific surface area, and small thermal conductivity, porous materials have set off a wide research boom in the world in recent years. Studies have shown that, without changing the structural state, the larger the porosity and the smaller the pore size of the porous material, the better its thermal insulation performance. [0003] Porous materials include aerogels, porous ceramics, porous metals, etc. Airgel materials have extremely high porosity, and their pore sizes are extremely small, most of which are within the nanoscale range. Because of the above-mentioned characteristics of airgel, it has excellent thermal insulation performance, and is even called a super thermal insulation material. Airgel is obta...

Claims

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Application Information

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IPC IPC(8): C04B38/00C04B35/14C04B35/624
CPCC04B35/14C04B38/0045C04B35/624C04B2235/3244C04B2235/445C04B2235/3873
Inventor 王美兰李万景王宇旭徐海波林天明
Owner JIANGSU MIRAFUL NANO MATERIAL CO LTD
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