In this study, a series of alpha-Fe2O3-CeO2 nanocomposites containing 5, 15, 30, and 50 % Fe as well as the pure oxides, alpha-Fe2O3 and CeO2, were synthesized by a novel route of auto-combustion method at temperatures lower than those reported previously. The as-synthesized catalysts were characterized by several techniques such as XRD, XRF, N-2 physisorption, DSC/TGA, NH3-TPD, TEM, and EDX. The catalytic activity of the synthesized nanocomposites was examined under ethanol conversion. The results revealed that the solid-solution formation was established for all the Fe-substituted CeO2 samples while maintaining the fluorite structure of ceria. Only a hardly noticeable segregation of alpha-Fe2O3 was appreciated for the catalyst samples with higher iron content (30 and 50 wt% Fe). The results confirmed that the adopted auto-combustion method allowed a good control of the chemical composition of the prepared composites with the proper structural and textural characteristics. The 30 % Fe-Ce sample was the most active and selective catalyst toward ethylene production compared with the other samples under study, owing to the pronounced Bronsted acid sites. The overall data collected through this work revealed that the synthesized nanocomposites are promising candidates for the production of ethylene from ethanol.