Origin and development of residual stresses in the NiNiO system: in-situ studies at high temperature by X-ray diffraction

TLDR: In this article, two high temperature chambers for X-ray diffraction were designed, allowing us to determine the stresses in both the oxide and the substrate with the sin2 ϕ technique, at high temperatures or room temperature and during heating-cooling sequences.

Abstract: In order to characterize the respective importance of the growth stresses, thermal stresses and stress relaxation developed in oxide scales, two high temperature chambers for X-ray diffraction were designed, allowing us to determine the stresses in both the oxide and the substrate with the sin2 ϕ technique, at high temperatures or room temperature and during heating-cooling sequences. It was applied to NiNiO. At room temperature after oxidation, NiO is subjected to compressive stresses whose level depends on the substrate thickness and on the oxidation time and temperature. In the substrate, compressive stresses are mainly due to internal oxidation. During oxidation at 900 °C, the oxide scale is subjected to slight tensile stresses which can be due partially to anionic diffusion, internal oxidation or the heating process. During heating-cooling sequences, the stresses in the scale decrease with increasing temperature and become negligible when the oxidation temperature is reached. The reversibility of the stress-temperature curve indicates that no stress relaxation occurs. The stresses found at room temperature are due only to thermal stresses and fit well the theoretical calculation of thermal stresses in NiO scale based on the newly determined thermal expansion coefficients of Ni and NiO. All these results show that the stresses found at room temperature are mainly generated during cooling and that the effect of the Pilling-Bedworth ratio or of factors playing a role during isothermal growth is negligible.