Ceria-based materials have the potential to be used as catalysts in electrochemical devices, especially ceramic fuel cells. Their incorporation into nickel-based catalysts promotes metallic dispersion, minimises particle agglomeration, and enhances metal-support interaction at the anode site of proton ceramic fuel cells (PCFCs). In this study, a methodical approach to investigate and analyse the effect of calcination temperature on the crystallographic structure and chemical properties of a nanostructured NiO-CeO2 powder that will be used as catalysts at the anode site of proton ceramic fuel cells (PCFCs) for cleaner power generation. The calcination temperature profile of the was varied from 300 °C to 600 °C. XRD and FTIR were used to investigate crystallinity and chemical properties of the prepared NiO-CeO2 powder. The XRD investigation results show that such increasing calcination temperature may increase the size of nanoparticles powder and phase purity. Following that, the FTIR analysis shows that the absorption bands formed at less than 800 cm−1 represent the metal-oxygen stretching (Ce-O and Ni-O stretch) which confirms the existence of NiO-CeO2 particles, thus, confirms the purity of NiO and CeO2 composite particles and suitable materials for PCFC anodes.
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