The preparation of ceria powders via a sol-gel process using cerium glycolate complex as precursor has been investigated to study the hydrolysis and condensation of cerium glycolate precursor. The gelation was followed by FT-IR spectroscopy and the evolution of the Ce-O-C and Ce-O-Ce bands of the cerium glycolate molecule was analyzed. The intensity of these bands decreased with the hydrolysis time. Monitoring the evolution of gelation within 5-110 min time regime was achieved. X-ray diffraction (XRD), nitrogen adsorption (BET specific surface area) and scanning electron microscopy (SEM) techniques have been applied to characterize the texture and structure of ceria systems prepared by the sol-gel method containing different hydrolysis ratios and thermal treated at temperatures between 400 and 1100 degrees C. Crystallization was observed after thermal treatment at above 400 degrees C. The thermal stability of ceria system was confirmed, and moderate surface areas were obtained even after the high temperature of calcination. (c) 2005 Elsevier B.V. All rights reserved.