In situ XRD analysis of the oxide layers formed by oxidation at 743 K on Zircaloy 4 and Zr–1NbO

Abstract Two alloys, having different oxidation behaviour (Zy4 and Zr–1NbO), have been investigated during oxidation at high temperature (743 K) and low oxygen pressure (10 kPa) by in situ X-ray diffraction (XRD). Tetragonal phase content and ‘pseudo-stresses’ on the monoclinic phase have been measured as a function of the oxide layer thickness. The tetragonal phase contents are similar for both alloys and decreased with the oxide layer thickness. Pseudo-stresses were much more compressive on Zr–1NbO alloy, with limited changes at the corrosion kinetics transition. On cooling, the tetragonal fractions do not change, while ‘pseudo-stresses’ decreased in different ways for the two alloys. With respect to stress analysis, no correlation was found between ‘pseudo-stresses’ and tetragonal phase content. In addition, due to the thermoelastic properties of the highly anisotropic phases of the zirconia, large internal thermal stresses are expected to develop during any temperature changes. The orders of magnitude of them are similar to the stresses induced by swelling during oxidation from Zr to ZrO2.