Ti-Si mixed oxides of various TiO2 contents were prepared via sol-gel one step hydrolysis with economical TiCl4 and tetraethoxy silane (TEOS) as the precursors and characterized by means of N-2-physisortion, FT-IR and XRD. The effects of TiO2 content on the gelation time were studied. The influences of calcination temperature on the mixed oxide of 20 wt.% TiO2 (20TiSi) were also studied. The results indicate that titanium is in four-fold coordination with oxygen in the SiO44- structure and Ti-O-Si band is observed by FT-IR. The mixed oxides with large TiO2 content exist on the pattern of amorphous material but not anatase. The composites have high specific surface areas, up to 681.5 m(2)/g, and a narrow pore size distribution. The ratio of the micropore declines with the increase of TiO2 content. 20TiSi has good thermal stability and still possesses 11 m(2)/g after calcination at 1100 degreesC. Within the range of tested calcination temperature, Ti-O-Si band does not break. TiO2 is well dispersed as the form of amorphous in 20TiSi calcined at 1100 degreesC. (C) 2004 Elsevier B.V. All rights reserved.