Potentialities of Raman Imaging for the Analysis of Oxide Scales Formed on Zircaloy-4 and M5® in Air at High Temperature

Micro-Raman imaging was used to investigate oxide scales formed on Zircaloy-4 and M5® alloys in air, in the 800–1,000 °C temperature range. To create the 2D spectral images, the data were processed by different ways. The results clearly show that a microscopic picture of the scales in terms of microstructure and internal stresses can be developed from Raman spectral maps at the micron scale. Data on the microstructure, crystallography, and composition, are presented. They confirm that the crystallographic phases observed for the Zircaloy-4 and M5® alloys are different, since, for Zircaloy-4, we clearly observed additional Raman signatures which most probably track the presence of nitrogen in the layers well before the occurrence of the kinetic transition. In particular, they show the presence of cubic zirconia in the layers, and strongly suggest the presence of zirconium nitride and oxynitride. Results also suggest the presence of strong stress gradients in the oxide scales.