The synthesis of SiO 2 core-TiO 2 shell composites from a titanium dioxide sol and a suspension of microspherical silicon dioxide is described. The main factors ensuring the formation of a composite with a preset morphology are the size and charge of the TiO 2 sol particles (10–45 nm) and silicon dioxide core particles (300–700 nm), the pH values of the suspensions of the starting components and the resulting composite, and the proportions and way of mixing of the siliconand titanium-containing components. The SiO 2 core-TiO 2 shell composites show high photocatalytic activity in the degradation of Rhodamine FL-BM dye (rate constant of k = 0.0813 min −1 ) and are much more active than precipitated TiO 2 powder ( k = 0.0022 min −1 ). The activity of the composite is determined by the calcination temperature (700–800°C), by the proportion and accessibility of the active component (TiO 2 ), and by the presence of a dopant (P 2 O 5 ).