AbstractThe stoichiometry and thickness of TiNxOyfilms has been determined by electron microprobe and nuclear microanalysis. The difficulty arising in the electron microprobe from the interference between NKα and TiLI lines has been overcome by using a suitable Monte Carlo computing scheme. This procedure takes into account the SiKα intensity which was found to be sensitive to composition and thickness of the overlying TiNxOyfilm. The good agreement between electron microprobe and nuclear microanalysis results indicate the validity of the metho