The present study investigates the morphology, chemical composition, and phase constitution of oxide scales formed on the Fe40Al5Cr0.2TiB intermetallic alloy after long-term oxidation at 700 °C for 2000 h in air and water vapor environments. The results demonstrate the formation of an extremely thin oxide scale (≈300 nm), composed predominantly of α-Al2O3, which provides effective protection against further oxidation. The oxide layer exhibits locally heterogeneous morphology, including whisker-like structures and fine crystallites. Due to the very limited thickness of the oxide scale, significant challenges arise in the interpretation of microanalytical data. It is shown that the accelerating voltage strongly influences the effective information depth in SEM-EDS analysis, leading to a substantial contribution from the substrate even at low voltages. Monte Carlo simulations were used to support the interpretation of electron–matter interactions and to explain the observed discrepancies in chemical analysis. The study demonstrates that reliable characterization of ultrathin oxide scales requires careful optimization of SEM parameters and the combined use of complementary techniques, including EDS/WDS, XRD, and EBSD. The findings highlight the importance of methodological considerations in the analysis of thin oxide layers and provide guidance for the correct interpretation of experimental data in similar systems.
Cebulski et al. (Sun,) studied this question.