Crystallography of magnetron sputtered TiN coatings on steel substrates

Structure formation processes in TiN coatings deposited by reactive CFUBMS on steel substrates have been investigated by X-ray diffraction experiments in symmetric Bragg-Brentano (B-B) and grazing incidence asymmetric Bragg diffraction (GIABD) modes and by SEM. The results show that the deposits with thicknesses of 500 and 4000 nm are built-up of polycrystalline stoichiometric TiN, in addition to which, some negligible amount of Ti-O and Ti-N-O phases have also been observed predominantly at their surfaces. In the thinner 500 nm films only columnar crystallites with {1 1 1}, {2 0 0} and {2 2 0} crystallographic planes parallel to the surface were formed. The share of the micro-volumes belonging to the 〈1 1 1〉 out-of-plane texture component varied between 70% and 80% depending on the target current (I_d) used (4 or 8 A in the present experiments). During the more advanced stages of growth the 〈1 1 1〉 texture weakens and new texture components appear; the process being more pronounced when the application has been performed at higher I_d values. The obtained crystallographic texture results for the thinner films and their changes during the more advanced stages of the coatings formation are discussed with particular consideration of the crystallography of the TiN lattice and the anisotropy of its elastic parameters. Based on a precise estimation of the interplanar distances, d_{〈u v w〉}, corresponding to the main texture components of the investigated films in the direction along the surface macro-normal, it has been revealed that the elastic strain, ε_{〈u v w〉}, caused by the compressive residual macro-stresses acting parallel to the film surfaces and the corresponding elastic stored energy, U_{〈u v w〉}, values obey the following relationships: ε_{〈1 1 1〉}>ε_{〈2 2 0〉}> ε_{〈2 0 0〉} and U_{〈1 1 1〉}>U_{〈2 2 0〉}>U_{〈2 0 0〉}, respectively. The observed ε_{〈u v w〉} and U_{〈u v w〉} anisotropy is found to be more pronounced in the thinner coatings and is such that, at more advanced stages of growth, it would be expected to favour the transition from 〈1 1 1〉 to 〈2 0 0〉 out-of-plane preferred orientation. However, the experimental results do not confirm this expectation, which points out that the texture-formation at these stages is not governed solely by the minimization of the stored elastic energy, but is a rather complicated process depending on a larger number of factors, some of which are discussed in the paper.