AbstractThis study investigates the effects of Multistage Heat Treatment (MSHT) on the development of an oxide-scale layer on the surface of FeCrAl sintered-metal-fibers. The oxide-scale layer was developed using an MSHT cycle at 930 °C for 1 h, followed by 960 °C for 1 h, and finally at 990 °C for 2 h. In this study, three samples were considered: Sample 1 was kept without thermal oxidation, while Samples 2 and 3 were exposed to one and eighteen MSHT cycles. Thermo-gravimetric analyses show that the weight gain of the heat-treated sample slows with time, confirming the growth of the protective oxide-scale layer. Scanning electron microscope images, after one MSHT cycle, reveal nonuniform oxide-scale growth with platelet-like on the surface. After eighteen MSHT cycles, however, clumped particles formed on the surface of the fibers. Atomic force microscopy was utilized to study the surface topography of the fibers. The results show that MSHT increases the surface roughness, where the surface roughness of one and eighteen MSHT cycles are the same. The x-ray diffraction analyses of the baseline sample and the sample with one MSHT cycle show pattern peaks of crystalline Fe2CrAl. In contrast, the results of eighteen MSHT cycles displayed diffraction pattern peaks of crystalline Cr and stable α-Al2O3. In summary, the results of this study reveal the changing nature of the oxide-scale layer. The findings of this study form the foundation for new techniques to protect and prepare the FeCrAl fibers as a support for catalysts.