X-ray photoelectron spectroscopy investigations of Si in non-stoichiometric SiNx LPCVD multilayered coatings

Si nanocrystals were formed in the non-stoichiometric Si-enriched SiNx low-pressure chemical vapor deposited (LPCVD) coatings on Si wafers treated by various modes. The coating structure as a function of technological conditions was investigated by ellipsometry and X-ray photoelectron spectroscopy (XPS) depth profiling. It was found that nanocomposites on base of SiNx films enriched by Si have a complex multilayered structure varying in dependence of deposition and annealing parameters. Analysis of the XPS spectra and Si 2s peaks shows the existence and quantity of four chemical structures corresponding to the Si–O, Si–N states, nanocrystalline and amorphous Si. The XPS results show evolution of the chemical structure of silicon nitride and formation of Si nanocrystals. It was found: • The LPCVD technology of nanocrystals formation allows to get enough high concentration of Si nanocrystals on different depths from the sample surface. • The volume fraction of nanocrystalline and amorphous Si is changed with depth; this relation depends from SiNx composition and annealing parameters. • XPS detects these two phase compositions of Si nanoparticles in SiNx and SiO2 layers. The ellipsometry, HR-TEM, and XPS results are in good agreement.