In this study, Fe2O3-CeO2 nanoparticles were synthesized by combusting a gel composed of polyvinyl alcohol (PVA) and tartaric acid (TA). Various factors affecting the formation of Fe2O3-CeO2, including solution pH, TA/PVA mole ratio, (Fe/Ce)/(TA/PVA) mole ratio, and calcination temperature, were thoroughly analyzed. The characterization of the Fe2O3-CeO2 particles involved XRD, EDS, SEMtechniques. The results obtained show that Fe2O3-CeO2 oxide particles have a nanometer size of about 50 nm. Subsequently, the photocatalytic performance of the nanostructured Fe2O3-CeO2 under appropriate light conditions was assessed, demonstrating high efficiency in decomposing methylene blue (MB).