A commercial polycarbosilane was modified with various metallic alkoxides to get mixed ceramic precursors in the Si-M-C-O systems (M=Ti, Zr Al). Pyrolysis under ammonia leads to the formation of various ceramic materials depending on the nature of M : Si3N4/TiN, Si3N4/ZrO2 or β′-SiAlON phases.
The polymer-to-ceramics conversion have been studied by MAS-NMR (29 Si, 27Al) and X-ray absorption (Ti K-edge). This paper will show how these two complementary spectroscopic techniques can be used to follow the nitridation process by probing local environments of different elements. In addition, it will be pointed out how X-ray absorption can be a powerful tool for the detection of the crystallization of nitride cubic phases.