Internal stresses and stability of the tetragonal phase in zirconia thin layers deposited by OMCVD

Zirconia thin films were deposited by OMCVD (organo-metallic chemical vapour deposition) at various temperatures and oxygen partial pressures on a AISI 301 stainless steel substrate with Zr(thd)4 as precursor. The as deposited 250 nm thin zirconia films presented a structure consisting of two phases: the expected monoclinic one and also an unexpected tetragonal phase. According to the literature, the stabilization of the tetragonal phase (metastable in massive zirconia) can be related to the crystallite size and/or to the generated internal compressive stresses. To analyze the effect of internal and external stresses on the thin film behaviour, in-situ tensile experiments were performed at room temperature and at high temperature (500 °C). Depending on the process parameters, phase transformations and damage evolution of the films were observed. Our results, associated to XRD (X-ray diffraction) analyses, used to determine phase ratios and residual stresses within the films, before and after the mechanical experiments, are discussed with respect to their microstructural changes.