Nickel-decorated mesoporous cerium-iron oxide composites were synthesized by a combination of incipient wetness impregnation and template-assisted hydrothermal techniques. The effects of the Fe/Ce ratio and the calcination temperature of cerium-iron oxides on the phase composition, texture, structure, and redox properties of the composites were studied by a combination of N physisorption, XRD, high-resolution transmission electron microscopy, SEM, Mössbauer, Raman, XPS, ultraviolet-visible and FTIR spectroscopies, H-temperature-programmed reduction, and total oxidation of ethyl acetate as a catalytic test. The combined physicochemical characterization and FTIR investigation of methanol decomposition was used for a proper understanding of the microstructure of the Ni/FeCe oxide composites and the mechanism of the reaction occurring on them.
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