A Zr-O-Si alkoxide complex was synthesized and its hydrolysis-condensation reaction was studied using small angle X-ray scattering. Transparent and homogeneous Zr-O-Si alkoxide solutions were formed by reacting Zr(OC3H7)4 with Si(OC2H5)4 hydrolyzed with one mole of water per one mole of Si(OC2H5)4 and HCl catalyst, whereas the solutions hydrolyzed with NH4OH catalyst or without any catalyst resulted in precipitation of ZrO2 crystals. Homogeneous Zr-O-Si alkoxide solutions were hydrolyzed with 0 to 8 moles of water to metal alkoxide, whose X-ray scattering curves were analyzed in both power law and Guinier law. The synthesized Zr-O-Si alkoxide consisted of chain like polymers, which were aggregated into three dimensional branched polymers with water content up to 4 moles per 1 mole metal alkoxide and their size increased up to 65Å in the Guinier radius. However, no further changes in size and shape of aggregated polymers were observed with more than 4 moles of water.