Structural characterization and high-temperature behavior of silicon oxycarbide glasses prepared from sol-gel precursors containing Si-H bonds

Silicon oxycarbide glasses have been synthesized by inert atmosphere pyrolysis at 1000°C of gel precursors obtained by cohydrolysis of triethoxysilane, HSi(OEt)3, and methyl-diethoxysilane, HMeSi(OEt)2. The oxycarbide structures have been carefully characterized by means of different techniques such as 29Si magic angle spinning nuclear magnetic resonance (MAS-NMR) and Raman spectroscopies, X-ray diffraction (XRD), and chemical analysis. Experimental results clearly indicate that, depending on the composition of the starting gels, the resulting oxycarbide glass either is formed by a pure oxycarbide phase or contains an extra carbon or silicon phase. By increasing the temperature up to 1500°C, the oxycarbide glasses display compositional and weight stability; however, the amorphous network undergoes structural rearrangements that lead to the precipitation of nano-sized β-SiC crystallites into amorphous silica. Crystallization of metallic silicon is also clearly observed at 1500°C for the samples in which the presence of Si-Si bonds was postulated at 1000°C.