Sol-gel technique emphasing the Pechini process has been employed for the preparation of nano-sized ZnTiO3 powders. Results of thermal analysis are given, including both DTA and TG. The decomposition of the precursor proceeded in four major steps, which include dehydration reaction, decomposition, combustion reaction and ZnTiO3 phase formation. The optimum temperature for ZnTiO3 powder calcination is 800 degrees C, which is determined by calculating the intensity and area of XRD peaks. The TEM observation shows that the powders existed in the mode of polycrystalline structure and the average grain size is about 30 nm. Moreover, FT-IR measurement is given for the relationship of the cationic environment in ZnTiO3 structure during the heat-treatment. (C) 2007 Elsevier Ltd. All rights reserved.