A series of CeO 2 –TiO 2 composites were synthesized using sol-gel method, and the structures were investigated by HR TEM, XRD, TG-DSC-MS, N 2 adsorption-desorption isotherms. The titania coating layer consisting of fine crystallites contributes to properties of the CeO 2 @TiO 2 nanocomposite. The development of the fast, simple, and facile route for the synthesis of novel CeO 2 @TiO 2 core-shell nanocomposite particles was suggested. An approach to increase the shell thickness of titania is to increase the concentration of the precursor of titania, but it also observed the formation of a small amount of independent titania clusters. It is shown that an increase in the titania content leads to the formation of a larger proportion of the rutile phase and a decrease in the proportion of metastable anatase and brookite, while reducing the particle size of the initial ceria core and the specific surface area due to the contact of titania shells, caused by the closer connections between nanoparticles.