Sb-doped SnO2 （ATO） nanometer powders were synthesized by hydrolysis of alkoxides, using SnCl4·5H2O and SbCl3 as raw materials. Some dehydrating processes, such as n-butanol/xylene mixed solvent heterogeneous azeotropic distillation, organic dehydrating agent and other dehydrating processes, were used to treat the wet colloids for preparing nonagglomerated ATO nanoparticles. The influences of dehydrating processes on the particle size, agglomeration and resistance were investigated using X-ray diffraction （XRD）, transmission electron microscopy （TEM） and Brunauer-Emmet-Teller （BET）. It is indicated that the dehydrating methods have great influences on the products properties, and that n-butanol/xylene mixed solvent heterogeneous azeotropic distillation processing and organic dehydrating agent can effectively remove the residual H2O molecules in wet colloids, and be used to prepare powders with high surface areas, about 85.32 m2/g, low agglomeration and good conductivity.
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