Study of the evolution of stresses and associated mechanisms in zirconia growing at high temperature on Zircaloy-4 by use of synchrotron radiation

The present work studied the evolution of stresses and associated mechanisms, related to viscoplastic behavior during relaxation, in the zirconia layer formed during the oxidation of Zircaloy-4 under a He/O2 mixture, at temperatures of 700 °C, 800 °C and 900 °C. Measurements by X-ray diffraction are performed in-situ under synchrotron radiation during oxidation to determine the evolutions of phases and stresses in the oxide layer with time. The results show that the zirconia formed contains a mixture of monoclinic and tetragonal phases. The proportion of the tetragonal phase depends on the oxidation temperature and decreases during oxidation. In order to better understand the influence of this evolution and localize the tetragonal phase, measurements by Raman spectroscopy have also been performed. These two phases are subjected to compressive stresses in directions perpendicular to the oxide layer growth direction. These stresses depend on temperature and relax during oxidation. Two mechanical models either considering the zirconia phases independently or considering an equivalent homogeneous oxide are proposed to describe the evolution of these stresses, considering that it is due to oxide viscoplasticity. The model parameters are analysed to discuss the mechanisms of viscoplastic flow in the oxide. Numerical values for the viscoplastic parameters of the model as well as for the corresponding activation energy are therefore provided. •Identification of the relative position of both monoclinic and quadratic phases has been performed by Raman spectroscopy.•X-ray diffraction analysis have been performed to extract the residual stresses in the zirconia layer during oxidation.•Different models are proposed to describe the stress evolution at long oxidation times, accounting for viscoplasticity.•Identification of mechanical parameters for relaxation phenomena are given.•Activation energy are provided and related to diffusion mechanisms in the oxide layer.