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Preparation of stibium doping stannic oxide nanopowder by hydrothermal method

A technology of tin dioxide and nano-powder, which is applied in the direction of tin oxide, etc., can solve the problems of small control margin and poor stability, and achieve the effects of easy control of reaction conditions, excellent electrical conductivity, and regular powder morphology

Inactive Publication Date: 2008-12-24
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has high requirements on reaction equipment, and strict requirements on process parameters, and the margin of control is small, so the quality (particle size distribution) of powder prepared by this method is less stable.

Method used

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  • Preparation of stibium doping stannic oxide nanopowder by hydrothermal method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] SnCl 4 ·5H 2 O(A.R.) and SbCl 3 (A.R.) were prepared into ethanol solutions of 1mol / L and 0.2mol / L respectively. Take SnCl 4 ·5H 2 O ethanol solution, add SbCl according to the doping ratio Sb / Sn=1:50 (mol / mol) 3 ethanol solution, adding deionized water to dilute the SnCl 4 The concentration is 0.5mol / L, stir and mix evenly, adjust the pH value to 9 with ammonia water, take 80mL of the mixed solution and inject it into a 100mL stainless steel autoclave with a polytetrafluoroethylene lining and electromagnetic stirring, at a hydrothermal temperature of 150°C React with a pressure of 18MPa for 2h. The product was washed with deionized water, dried, ground, and treated at 600° C. for 30 minutes to obtain Sb-doped tin dioxide nanopowder.

Embodiment 2

[0019] SnCl 4 ·5H 2 O(A.R.) and SbCl 3 (A.R.) were prepared into ethanol solutions of 1mol / L and 0.2mol / L respectively. Take SnCl 4 ·5H 2 O ethanol solution, add SbCl according to the doping ratio Sb / Sn=11:100 (mol / mol) 3 ethanol solution, adding deionized water to dilute the SnCl 4 The concentration is 0.5mol / L, stir and mix evenly, adjust the pH value to 9 with ammonia water, take 80mL of the mixed solution and inject it into a 100mL stainless steel autoclave with a polytetrafluoroethylene lining and electromagnetic stirring, at a hydrothermal temperature of 150°C React with a pressure of 18MPa for 2h. The product was washed with deionized water, dried, ground, and treated at 600° C. for 30 minutes to obtain Sb-doped tin dioxide nanopowder.

Embodiment 3

[0021] SnCl 4 ·5H 2 O(A.R.) and SbCl 3 (A.R.) were prepared into ethanol solutions of 1mol / L and 0.2mol / L respectively. Take SnCl 4 ·5H 2 O ethanol solution, add SbCl according to the doping ratio Sb / Sn=9:50 (mol / mol) 3 ethanol solution, adding deionized water to dilute the SnCl 4 The concentration is 0.5mol / L, stir and mix evenly, adjust the pH value to 9 with ammonia water, take 80mL of the mixed solution and inject it into a 100mL stainless steel autoclave with a polytetrafluoroethylene lining and electromagnetic stirring, at a hydrothermal temperature of 150°C React with a pressure of 18MPa for 2h. The product was washed with deionized water, dried, ground, and treated at 600° C. for 30 minutes to obtain Sb-doped tin dioxide nanopowder.

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Abstract

The invention discloses a hydrothermal preparation method of antimony doped tin dioxide nano-powder comprising: respectively preparing a SnCl4 alcohol solution and a SbCl3 alcohol solution, mixing the SnCl4 alcohol solution with the SbCl3 alcohol solution and adding deionized water into the mixture to maintain the concentration of SnCl4 between 0.005 mol / L and 3 mol / L, adjusting the pH value of mixed solution to 8.5-9.5 by ammonia, homogeneously dispersing the mixed solution in a reactor, conducting hydrothermal reaction for 1-2 hours at 100-200 DEG C, centrifugating, washing and drying the products after reaction to obtain powder, heating the powder after the powder is grinded for 0.5-1 hour at 400-700 DEG C, obtaining the antimony doped tin dioxide nano-powder. The powder prepared by the invention has a regular appearance and a narrow granularity distribution. The reaction condition is easy to control for adopting cheap SnCl4.5H2O and SbCl3 as materials, which is suitable for industrial mass production.

Description

technical field [0001] The invention relates to a method for preparing antimony-doped tin dioxide nanometer powder, in particular to a method for preparing antimony-doped tin dioxide nanometer powder by a hydrothermal method. Background technique [0002] Antimony doped tin oxide (ATO) nanopowder has excellent electrical conductivity, optical properties, thermal stability and corrosion resistance, and the raw material is cheap, so it is an ideal transparent conductive material. [0003] There are many methods for preparing ATO nanopowder, such as sol-gel method, co-precipitation method, and hydrothermal method. Compared with sol-gel method and co-precipitation method, hydrothermal method has relatively simple process, easy control of reaction conditions, high production efficiency, easy process scale-up, low cost, uniform product particle size distribution, less agglomeration between particles, and easy preparation of high-purity , various nano-inorganic powders. [0004] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G19/02
Inventor 蔡振云周箭陆宇
Owner ZHEJIANG UNIV
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