In this work, Si-Ti oxycarbide glasses have been prepared through a process of pyrolysis of preceramic materials in inert atmosphere. The starting reagents were TEOS, TBOT and PDMS, in which the final Ti content was of 0% and 7%. The pyrolysis process has been studied by TGA, FT-IR, RMN-Si29. It has been observed that the most important changes occur in the redistribution reactions during the pyrolysis process. These changes are due to the different thermal stability of the starting pre-ceramic materials and, above all, the presence of Ti.