The partial pyrolysis of poly(dimethyl siloxane) is reported. Pyrolysis is completed in a two step process, inert pyrolysis in a nitrogen atmosphere followed by oxidative pyrolysis in air. Treatment temperatures were from 300-400 degrees C for the inert processing and 260-300 degrees C for oxidative treatment. This thermal processing required no solvents or bulky catalysts, whose transport into the matrix is diffusion controlled and thus limit product uniformity. Therefore, high sample uniformity was achieved. Hybrid materials with reduced carbon and hydrogen content and an increased oxygen/silicon ratio resulted. These composites were shown to be stronger than composites reported in the literature with similar elemental compositions, but prepared in such a way as to achieve only limited interphase interaction. At high oxidation temperatures, microporosity developed in the materials.