xTiO2-ySiO2 system photocatalysts were developed by sol-gel method based on the change of production parameters, and their structure of crystallization and the specific surface area were measured. Considering the efficiency of the ethanol and phenol degradation using the catalyst, the conclusions were obtained as follows: By means of X-ray analysis of xTiO2-ySiO2 powder that is obtained from Titanium and Silicon alkoxide by sol-gel process, it is shown that crystal structure of anatase type is a dominating structure and, on the other hand, the structure of rutile also partly exists. The increase of SiO2 contents causes the decrease of the degree of crystallization of the gel, whereas the specific surface area preferentially increases. It is shown that more than 90% of ethanol and phenol are degraded when reaction time is about three and an hours, and the maximum degradation rate of ethanol and phenol is shown in 60TiO2-40SiO2 catalyst.