Nano-sized ceria particles were prepared from the aqueous solution containing the polymeric precursors by ultrasonic spray pyrolysis at the severe preparation conditions such as high flow rate of carrier gas and short residence time. The key idea to produce nanoparticles was to prepare hollow ceria particles which are easily turned to aggregates of nano-sized primary particles during the post-thermal treatment and thereafter disintegrate such aggregates to nano-sized particles by a simple ball milling process. It was found that using the polymeric precursor strongly influences the crystallization characteristics and morphological changes of the as-prepared particles during the post-thermal treatment. The as-prepared particles prepared from the polymeric precursor solution had non-spherical shape and fractured structure with a thin shell, whereas the as-prepared and calcined ceria particles obtained from the aqueous solution had spherical shape and hollow morphology with a thick shell. Also, nano-sized ceria particles prepared from the polymeric precursor solution had less aggregated structure than those prepared from the aqueous solution. For the ceria particles prepared from the polymeric precursor solution, the degree of aggregation between the primary particles was reduced as increasing the calcination temperature. As a result, aggregation-free nano-sized ceria particles were obtained above 1200 degrees C without a milling process. The mean size of the primary particles increased from several tens nanometer to submicrometer size as the calcination temperature changed from 800 to 1300 degrees C. (c) 2005 Elsevier B.V. All rights reserved.