Preparation method of rare earth doped silicon dioxide aerogel

A silicon dioxide and rare earth doping technology, which is applied in chemical instruments and methods, inorganic chemistry, silicon compounds, etc., can solve the problems of low porosity, low pore size, increased thermal conductivity, and inapplicability of high-temperature heat insulation, etc., to improve the use of Temperature, high production efficiency, and favorable effects for mass production

Pending Publication Date: 2021-11-16
ZHONGKE RUNZI (CHONGQING) ENERGY SAVING TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As an environmental barrier coating, rare earth silicate has good high temperature stability and excellent heat insulation performance, but the existing rare earth silicate ceramics have low porosity (50%-70%) and large pore size ( 0.4~3.5um), thermal conductivity will increase rapidly in high temperature environment, not suitable for high temperature insulation

Method used

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  • Preparation method of rare earth doped silicon dioxide aerogel
  • Preparation method of rare earth doped silicon dioxide aerogel
  • Preparation method of rare earth doped silicon dioxide aerogel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] This embodiment includes the following steps:

[0021] (1) Add 20.8g TEOS, 55.2g absolute ethanol and 5.4g H 2 0, mechanically stirred for 15min, and 3.65g mass fraction was added dropwise thereto through the constant pressure funnel as the diluent of hydrochloric acid ethanol of 0.05wt%, and after stirring for 120min, it was sealed and left standing at room temperature for 24h to obtain the molar ratio n(TEOS):n(C 2 h 5 OH): n(H 2 O)=1:12:3 SiO 2 Sol.

[0022] (2) 34.8g Y(NO 3 ) 3 4H 2 O powder was dissolved in 10.8g of water, heated at 50°C for 30min, and cooled to room temperature to obtain Y(NO 3 ) 3 solution.

[0023] (3) Weigh 0.684g of the material obtained in step (2), slowly drop into 9.31g of SiO 2 In the sol, stir magnetically for 30 min.

[0024] (4) Drop ammonia water and ethanol diluent into the material obtained in step (3), stir evenly, and let stand to gel.

[0025] (5) the above Y-SiO 2 The gel was airtight and aged for 24 hours before sup...

Embodiment 2

[0028] This embodiment includes the following steps:

[0029] (1) Add 20.8g TEOS, 32.2g absolute ethanol and 5.4g H 2 0, mechanically stirred for 15min, dripped 3.65g massfraction of 0.05wt% hydrochloric acid ethanol diluent therein with a speed of 6s / drops through a constant pressure funnel, sealed and stood still at room temperature for 24h after stirring for 120min, and obtained the molar ratio n(TEOS ):n(C 2 h 5 OH): n(H 2 O)=1:7:3 SiO 2 Sol.

[0030] (2) 34.8g Y(NO 3 ) 3 4H 2 O powder was dissolved in 10.8g of water, heated at 50°C for 30min, and cooled to room temperature to obtain Y(NO 3 ) 3 solution.

[0031] (3) Weigh 0.137g of the material obtained in step (2), slowly drop into 12.8g of SiO 2 In the sol, stir magnetically for 30 min.

[0032] (4) Drop ammonia water and ethanol diluent into the material obtained in step (3), stir evenly, and let stand to gel.

[0033] (5) the above Y-SiO 2 The gel was airtight and aged for 24 hours before supercritical d...

Embodiment 3

[0036] The preparation method of the present embodiment comprises the following steps:

[0037] (1) Add 20.8g TEOS, 92g absolute ethanol and 5.4g H 2 0, mechanically stirred for 15min, dripped 3.65g of hydrochloric acid ethanol diluent with a mass fraction of 0.05wt% through a constant pressure funnel at a speed of 6s / drop, stirred for 120min and then sealed at room temperature for 24h, so that the hydrolysis reaction was sufficient and slow Carried out to obtain the molar ratio n(TEOS):n(C 2 h 5 OH): n(H 2 O)=1:20:3 SiO 2 Sol.

[0038] (2) 34.8g Y(NO 3 ) 3 4H 2 O powder was dissolved in 10.8g of water, heated at 50°C for 30min, and cooled to room temperature to obtain Y(NO 3 ) 3 solution.

[0039] (3) Weigh 0.228g of the material obtained in step (2), slowly drop into 12.2g of SiO 2 In the sol, stir magnetically for 30 min.

[0040] (4) Drop ammonia water and ethanol diluent into the material obtained in step (3), stir evenly, and let stand to gel.

[0041] (5) t...

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Abstract

The invention discloses a preparation method of rare earth doped silicon dioxide aerogel, and belongs to aerogel preparation. The preparation method comprises the following steps: sequentially adding tetraethoxysilane, ethanol and water into a container according to a ratio, mechanically stirring, adding hydrochloric acid, stirring again, sealing, standing, and carrying out a sufficient hydrolysis reaction to obtain SiO2 sol; dissolving Y (NO3) 3.4 H2O powder in water, carrying out heating reaction, cooling to room temperature to obtain a Y (NO3) 3 solution, dropwise adding the Y (NO3) 3 solution into the SiO2 sol, and uniformly stirring; dropwise adding ammonia water, and standing to obtain Y-SiO2 gel; and sealing, standing and aging, and then carrying out supercritical drying to obtain the blocky Y-SiO2 aerogel. The rare earth elements are doped into the silicon dioxide aerogel, so that the use temperature of the silicon dioxide aerogel is increased, the heat conductivity coefficient of the aerogel is reduced, and the obtained aerogel is low in density, high in specific surface area and good in heat insulation performance. The method is simple in process, high in production efficiency, low in equipment requirement and beneficial to large-scale production, and the problem that rare earth elements are non-uniformly dispersed in a silicon dioxide matrix is solved.

Description

technical field [0001] The invention belongs to the technical field of airgel preparation, and in particular relates to a preparation method of rare earth-doped silica airgel. Background technique [0002] With the rapid development of supersonic aircraft, the nose cone, wing and engine nozzle of the aircraft have been subjected to aerodynamic heating for a long time, and the traditional thermal insulation materials can no longer meet the current use requirements. Thermal material is very necessary. Airgel is a new type of thermal insulation material with nanoscale pores, in which SiO 2 Aerogels are currently the most widely used. But due to SiO 2 Airgel is easy to sinter and collapse at high temperature, and its long-term use temperature is only 650 °C. Therefore, the high temperature stability is generally improved by doping heterogeneous elements. As an environmental barrier coating, rare earth silicate has good high temperature stability and excellent heat insulatio...

Claims

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Application Information

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IPC IPC(8): C01B33/155C01B33/158
CPCC01B33/155C01B33/1585C01P2004/01C01P2004/03C01P2006/17C01P2006/10C01P2006/12C01P2006/16
Inventor 余煜玺李璐
Owner ZHONGKE RUNZI (CHONGQING) ENERGY SAVING TECH CO LTD
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