This paper describes the effect of drying process on the preparation of TiO2-SiO2 nano-hybrid particles. The hybrid sol was prepared by sol-gel process with controlled chemical modification (CCM) to attain the TiO2 nano-coating on the SiO2 nano-sphere. The hydrolysis reaction of titanium alkoxide was controlled by R-A ([CH3COOH)/[Ti]), and R-W ([H2O]/[Ti]). The hybrid particles were dried by under the super critical drying to suppress the hard agglomeration of the as-prepared nano-hybrid sol. As a result, the hard agglomeration of the primary particles was successfully suppressed to obtain TiO2-SiO2 nano-hybrid particles with controlled chemical modification of titanium alkoxide. The quantum size effect of nano-hybrid particles was confirmed by the band gap energy shift, using ultraviolet-visible spectroscopy (UV-vis). (C) 2008 Elsevier B.V. All rights reserved.