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Crystalline Sb doped tin oxide (ATO) , cassiterite structure , is a wide band gap n2type semiconductor. Because of its optical property (transparent for visible light and reflective for IR) and electroconductibility , good chemical and mechanical stability , it has many applications , such as transparent conductive electrodes , photovoltaic devices , photosensors , catalyst , antistatic coatings and electrochromic materials[1- 4 ] . A variety of techniques have been used to prepare ATO superfine powders , some involve dry processes , others are based on wet chemical processes , including chemical coprecipitation[5] , sol-gelrelated process[6] , emulsion method[7 ] . Compared with dry process , wet chemical process is a low-cost method to fabricate superfine powders. However , the process suffers the disadvantage of producing hard agglomerate during drying and calcining procedures due to the high surface tension stress , physically adsorbed and / or chemically coordinated H2O molecule , and hydroxyl group on hydrate particles surface. The key issue to decrease the agglomeration has been considered to decrease the tension stress and to remove the residual H2O molecule with maximum limit by proper dehydrating process[7 , 8 ] . The dehydrating methods adopted currently include refrigeration drying[9 ] , supercritical drying[10 ] , organic solvent washing and heterogeneous azeotropic distillating[11 ] . The former two kinds of methods which needs specialized equipments , are not used as widespread as the latter two , which are simple and easy to operate. The method of organic solvent washing mainly uses ethanol , isopropanol and acetone to substitute for H2O molecules remained in the gels , but this substitution is limited and the agglomeration can not be completely eliminated. Compared with organic solvent washing method , heterogeneous azeotropic distillation is a more effective anti-agglomeration method. But , up to now , the solvent used in heterogeneous azeotropic distillation mainly is n2butanol . No any other solvents are found to be utilized in the process , and also the report on the preparation of free agglomerate nanometer2sized powder with organic dehydrating agent are not found.. In the present study , nanometer-sized ATO powders are prepared through hydrolysis of metal alkoxides. In order to eliminate the agglomerate , an improved heterogeneous azeotropic distillation process , n-butanol/ xylene mixed solvent heterogeneous azeotropic distillation , and a kind of organic dehydrating agent are used in dehydrating procedure. This paper discusses the effect of the two dehydrating process , compared with other processes , on theproperties of ATO superfine powders. It is found that the n2butanol/ xylene mixed solvent heterogeneous azeotropic distillation process and organic dehydrating agent can effectively dehydrate , and obtain high performance nanoscaled ATO powders. |
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