Antimony-doped tin oxide aerogel and preparation method thereof

A technology doped with tin dioxide and antimony, which is applied in the direction of tin oxide, etc., can solve the problems of high density of antimony-doped tin dioxide material, complex preparation process, and unsuitability for production, and achieve stable airgel pore structure and process Simple, short-cycle effect

Inactive Publication Date: 2018-01-09

SHANDONG RES & DESIGN ACADEMY OF IND CERAMICS

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AI-Extracted Technical Summary

Problems solved by technology

[0003] At present, the preparation methods of ATO mainly include hydrothermal method, co-precipitation method, sol-gel method, etc., and the hydrothermal method is relatively complicated.

The antimony-doped tin dioxide material prepared by the chemical precipitation method described in patent CN103553120A has a relatively high density, and requires strict con...

Abstract

The invention belongs to the technical field of nanogel materials, and in particular relates to antimony-doped tin oxide aerogel and a preparation method thereof. The antimony-doped tin oxide aerogelis prepared from tin salt, antimony salt, an organic solvent and deionized water. The preparation method is short in period, adopts ambient pressure drying, and is simple in technology, easy in control of conditions and low in preparation cost; the prepared aerogel is stable in pore structure, large in specific surface area and smaller in particle size.

Application Domain

Tin oxides

Technology Topic

Antimony dopingOrganic solvent +4

Image

Examples

Experimental program(4)

Example Embodiment

[0038] Example 1

[0039] (1) Weigh 30g of crystalline tin tetrachloride, 4.2g of antimony trichloride (doping amount is 12%), 500g of absolute ethanol, 40g of deionized water, 15g of propylene oxide, and use FA and PEG6000 as additives. They are 5g and 2g respectively. The crystalline tin tetrachloride is dissolved in a mixed solution of absolute ethanol and deionized water and stirred evenly to obtain a mixed solution a.

[0040] (2) Add antimony trichloride to solution a and stir evenly to obtain turbid white solution b.

[0041] (3) During the stirring process, 3 g of propylene oxide solution was added dropwise to the turbid white solution b, and after the colorless and clear solution c was obtained, the dropwise addition of propylene oxide was stopped.

[0042] (4) During the stirring process, add the admixtures FA and PEG6000 to the colorless and clear solution c, and wait until it is evenly stirred to obtain a mixed solution d.

[0043] (5) During the stirring process, continue to add the remaining propylene oxide solution dropwise. After the dropwise addition is completed, continue to stir the solution and stir for 10 minutes to obtain the milky white solution f, which is now the antimony-doped tin dioxide sol.

[0044] (6) Stop stirring, and seal solution f and let it stand for 3 hours to obtain a white wet gel.

[0045] (7) Pour the n-hexane solution into the white wet gel and place it in a 45°C dry box for replacement. The replacement period is 3 days. The n-hexane solution is replaced every day to complete the replacement.

[0046] (8) After the replacement is completed, the material is placed in a 65°C drying oven under normal pressure for drying, and the drying time is 24h.

[0047] (9) After the drying is completed, the material is placed in an electric furnace, and the temperature is raised to 550°C at 2°C/min for 1 hour to obtain antimony-doped tin dioxide aerogel.

[0048] Specific surface area = 315m 2 /g, bulk density 0.15g/cm 3 、The average pore diameter is 10nm, the pore volume is 1.7cm 3 /g.

Example Embodiment

[0049] Example 2

[0050] (1) Weigh 50g crystalline tin tetrachloride, 7.5g antimony trichloride (doping amount is 15%), 800g isopropanol, 60g deionized water, 30g propylene oxide, and select FA and CATB as additives. They are 8g and 1.5g respectively. The crystalline tin tetrachloride is dissolved in a mixed solution of isopropanol and deionized water and stirred evenly to obtain a mixed solution a.

[0051] (2) Add antimony trichloride to solution a and stir evenly to obtain turbid white solution b.

[0052] (3) During the stirring process, 6 g of propylene oxide solution was added dropwise to the turbid white solution b, and the dropwise addition of propylene oxide was stopped after the colorless and clear solution c was obtained.

[0053] (4) During the stirring process, add the admixtures FA and CATB to the colorless and clear solution c, and wait until it is evenly stirred to obtain a mixed solution d.

[0054] (5) During the stirring process, continue to drip the remaining propylene oxide solution. After the dripping is completed, continue to stir the solution and stir for 20 minutes to obtain a milky white solution f, which is now the antimony doped tin dioxide sol.

[0055] (6) Stop stirring, seal the solution f and let it stand for 5 hours to obtain a white wet gel.

[0056] (7) Pour the n-hexane solution into the white wet gel and place it in a 45°C dry box for replacement. The replacement period is 3 days. The n-hexane solution is replaced every day to complete the replacement.

[0057] (8) After the replacement is completed, the material is placed in a 65°C drying oven under normal pressure for drying, and the drying time is 24h.

[0058] (9) After the drying is completed, the material is placed in an electric furnace, and the temperature is raised to 600° C. for 1 hour at 2° C./min to obtain antimony-doped tin dioxide aerogel.

[0059] Performance index: specific surface area = 215m 2 /g, bulk density 0.21g/cm 3 、The average pore diameter is 18nm, the pore volume is 1.52cm 3 /g.

Example Embodiment

[0060] Example 3

[0061] (1) Weigh 30g of crystalline tin tetrachloride, 4.5g of antimony trichloride (doping amount is 15%), 600g of absolute ethanol, 200g of n-butanol, 50g of deionized water, 30g of propylene oxide, and optional additives The masses of PEG10000 and CATB are 6g and 1.5g respectively. The crystalline tin tetrachloride is dissolved in a mixed solution of absolute ethanol, n-butanol and deionized water and stirred evenly to obtain a mixed solution a.

[0062] (2) Add antimony trichloride to solution a and stir evenly to obtain turbid white solution b.

[0063] (3) During the stirring process, 5 g of propylene oxide solution was added dropwise to the turbid white solution b, and after the colorless and clear solution c was obtained, the propylene oxide dropwise addition was stopped.

[0064] (4) During the stirring process, add the admixtures PEG10000 and CATB to the colorless and clear solution c, and wait until it is evenly stirred to obtain a mixed solution d.

[0065] (5) During the stirring process, continue to drip the remaining propylene oxide solution. After the dripping is completed, continue to stir the solution and stir for 12 minutes to obtain a milky white solution f, which is now the antimony-doped tin dioxide sol.

[0066] (6) Stop stirring, seal the solution f and let it stand for 5 hours to obtain a white wet gel.

[0067] (7) Pour the n-hexane solution into the white wet gel and place it in a 45°C dry box for replacement. The replacement period is 3 days. The n-hexane solution is replaced every day to complete the replacement.

[0068] (8) After the replacement is completed, the material is placed in a 65°C drying oven under normal pressure for drying, and the drying time is 24h.

[0069] (9) After the drying is completed, the material is placed in an electric furnace, and the temperature is raised to 600° C. for 1 hour at 2° C./min to obtain antimony-doped tin dioxide aerogel.

[0070] Performance index: specific surface area = 260m 2 /g, volume density 0.19g/cm 3 、The average pore diameter is 35nm, the pore volume is 1.65cm 3 /g.

PUM

Property	Measurement	Unit
Specific surface area	315.0	m²/g
Bulk density	0.15	g/cm³
Average pore size	10.0	nm

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Classification and recommendation of technical efficacy words

Short cycle
Simple process

Antimony-doped tin oxide aerogel and preparation method thereof

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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