Ti-Si mixed oxides with different TiO2 content were prepared by sol-gel one step hydrolysis, using TiCl4 as the precursor. The samples were characterized by BET, FT-IR and XRD. The results indicated that titanium is in fourfold coordination with oxygen in the SiO44- in mixed oxides, form the bond of Ti-O-Si, and the low titania materials are mixed on an atomic scale. The phase of anatase appeared when TiO2 content is up to 80%. The mixed oxides had high specific surface areas up to 681.5 m2/g. 10TiSi is a better support than SiO2 in the reaction of CO oxidation. The samples were characterized by BET, FT-IR and XRD. The results indicates that the titanium is in fourfold coordination with oxygen in the SiO44- in mixed oxides, form the bond of Ti-O-Si, and the low titania materials are mixed on an atomic scale. The phase of anatase appeared when TiO2 content is up to 80%. The mixed oxides had high specific surface Areas up to 681.5 m2 / g. 10TiSi is a better support than SiO2 in the reaction of CO oxidation.