Ultra high temperature ceramic based aerogel material and preparation method thereof

A technology of ultra-high temperature ceramics and aerogels, which can be applied to ceramic products, other household appliances, household appliances, etc., and can solve the problems of easy pulverization of precursors

Active Publication Date: 2017-07-11
江苏先进无机材料研究院
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of the current research is limited to the use of liquid precursors to prepare nano-scale ultra-high temperature ceramic single-phase and composite powders, and only a few works have combined foaming technology to prepare ultra-high temperature porous ceramics. It may be due to the fact that the precursor is easily pulverized during the drying and heat treatment ceramic conversion process

Method used

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  • Ultra high temperature ceramic based aerogel material and preparation method thereof
  • Ultra high temperature ceramic based aerogel material and preparation method thereof
  • Ultra high temperature ceramic based aerogel material and preparation method thereof

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preparation example Construction

[0032] Preparation of precursor sol

[0033] In one embodiment, in order to prepare transition metal boride / silicon carbide composite airgel material or transition metal boride / transition metal carbide / silicon carbide composite airgel material, soluble transition metal precursor, organic silicon ( Silicon source), soluble carbon source and boron source are dissolved in the solvent to form a mixed solution. In another embodiment, in order to prepare a transition metal carbide / silicon carbide composite airgel material, a soluble transition metal precursor, organic silicon and a soluble carbon source are dissolved in a solvent to form a mixed solution. "Soluble" here means being soluble in the above-mentioned solvents. When forming the mixed solution, the order of adding the raw materials is not limited, as long as the raw materials are mixed uniformly.

[0034] The soluble transition metal precursor can be an oxychloride or hydroxide containing the transition metal, or an orga...

Embodiment 1

[0045] Add 50g of zirconium n-butoxide and 10g of ethyl orthosilicate dropwise into 50g of ethanol and stir to mix. After stirring for 30 minutes, add 44.42g of glycerol according to the C / Zr molar ratio of 10 and the C / Si molar ratio of 3 , Add 56.95g of triethyl borate according to the B / Zr molar ratio of 3, and react in a water bath at 40°C for 2 hours to obtain the precursor of zirconium boride / silicon carbide; pour the precursor into a beaker and place it in an oven at 90°C for curing for 12 Hours, after curing, naturally cool to room temperature and demould to obtain the zirconium boride / silicon carbide precursor xerogel; place the xerogel in an electric furnace and heat it to 1600°C for 2 hours under an argon atmosphere to make it Carbothermal reduction reaction; after the reaction, naturally cool to room temperature.

[0046] In the experiment, the photo of the zirconium boride / silicon carbide airgel obtained through high-temperature carbothermal reduction reaction is ...

Embodiment 2

[0048] In order to prepare zirconium boride / silicon carbide airgel material, 50g of zirconium n-butoxide and 10g of ethyl orthosilicate were added dropwise to 50g of ethanol and stirred and mixed. After stirring for 30 minutes, according to the C / Zr molar ratio of 10, When the C / Si molar ratio is 3, add 44.42 g of glycerol, and when the B / Zr molar ratio is 10, add 189.8 g of triethyl borate. All the other operations are the same as described in Example 1. The porosity, pore size distribution and density of the prepared airgel material were measured by mercury intrusion porosimetry, wherein the porosity was 80.9%, the pore diameter was 0.8-1.2 μm, and the density was 0.76 g / cm 3 .

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Abstract

The invention relates to an ultra high temperature ceramic based aerogel material and a preparation method thereof. The preparation method comprises the following steps: a soluble transition metal precursor, organosilicon and soluble carbon and boron sources are dissolved in a solvent to obtain a mixed solution for reaction at 30 to 80 DEG C to obtain a precursor sol, or the soluble transition metal precursor, the organosilicon and the soluble carbon source are dissolved in a solvent to obtain a mixed solution for reaction at 30 to 80 DEG C to obtain a precursor sol; the obtained composite precursor is cured to obtain an aerogel preform; and the ultra high temperature ceramic based aerogel material is obtained by ceramic conversion of the obtained aerogel preform under protection of atmosphere at 1000 to 1800 DEG C.

Description

technical field [0001] The invention relates to an ultra-high temperature ceramic-based airgel material, in particular to a method for preparing an ultra-high-temperature ceramic-based airgel material by controlling the composition of the precursor sol of the ultra-high temperature ceramic and its drying process, and belongs to non- The technical field of preparation of oxide ceramic materials. Background technique [0002] Ultra-high temperature ceramics refer to a type of ceramic material that can maintain physical and chemical stability in a high temperature environment (>1800°C) and a reaction atmosphere. This type of material is mainly composed of borides, carbides, etc. compounds and nitrides. Ultra-high temperature ceramics have the advantages of high melting point, low saturated vapor pressure, and good chemical and microstructural stability in the heat flow ablation environment, so ultra-high temperature ceramics are considered to be powerful for high-temperatur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/565C04B35/58C04B35/56C04B38/00
Inventor 李飞黄晓
Owner 江苏先进无机材料研究院
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