Titania (TiO2)-coated silica (SiO2) particles were prepared by controlled hydrolysis of titanium alkoxide precursors. First, monodisperse spherical silica particles were prepared by the sol-precipitation method. During sol-precipitation, the silica particle size was affected by the reaction conditions, such as the TEOS and ammonia concentrations. The morphology of the titania-coated silica particles was strongly dependent upon the HPC concentration and the ultrasonic dispersion. Without HPC, the titania was coated on the aggregated silica particles. Isolated SiO2/tiO2 core/shell particles having uniform titania coating layer of 8 to 10 nm thickness were obtained only when titania was coated in the presence of HPC, followed by ultrasonic dispersion. Ultrasonic dispersion effectively removed the second-phase titania particles grown on the coating layer. The titania-coated silica particles were characterized using FE-SEM, TEM, N2 adsorption, electrophoresis, and XRD.