Spherical silica and zirconia mixed titania and pure titania samples were prepared in presence of cetyltrimethylammonium bromide (CTAB) through controlled hydrolysis of corresponding metal alcoxides. Effect of surfactant amount and calcinations temperature on morphology, surface area and photocatalytic activity is studied using PXRD, SEM, FTIR, Solid state UV-vis spectroscopy and BET surface area. It is well observed that in presence of 2 mol% CTAB, uniform sized spherical oxide particles can be synthesized. However, increasing or decreasing the surfactant amount does not favor the spherical particle formation. Material synthesis in presence of CTAB not only helps in the spherical particle formation but also increases the surface area and visible light absorption. Studies on photocatalytic lead removal with respect to calcination temperature indicate that the calcination at 500 degrees C is most suitable for the best photocatalytic activity. Mixing of zirconia and silica helps in anatase phase stabilization even at 900 degrees C calcination. Accordingly low decrease in surface area even at 900 degrees C calcination is observed. Due to the phase stabilization and higher surface area binary oxide materials showed comparatively better photocatalytic activity even after calcination at 900 degrees C. So it can be concluded that present synthesis approach can produce uniform sized spherical binary oxide materials with better photocatalytic activity in visible light. (C) 2008 Elsevier Inc. All rights reserved.