Samples of TiNx sub-stoichiometric chemical vapour-deposited coatings had been studied by means of high-resolution X-ray emission spectroscopy. It was found that a strong vacancy-induced peak was present in the Ti K-emission band. Its intensity could be correlated to the vacancy concentration deduced from nuclear reaction spectroscopy and X-ray diffraction data. This relationship was linear if the vacancy concentration was between 0 and 0.3. If it was higher than 0.3, an anomalous behaviour occurred which was attributed to microstructural changes. As confirmation, transmission electronic studies of a TiN0.57 layer with a 0.43 vacancy concentration were performed. The most striking result was the observed existence of many stacking faults. These defects were extrinsic, and the stacking-fault energy was about 3.5mJ/m2. Their density seemed to depend upon their distance from the substrate/coating interface.

Transmission Electron Microscopy Analysis of a TiNx Substoichiometric CVD Coating. J.L.Derep, E.Beauprez: Journal of Materials Science, 1993. 28[18], 4957-61