A series of Co/Fe hydrotalcite-like samples were prepared by the traditional co-precipitation method and treated under microwave irradiation at different temperatures, powers, and for various durations. The resulting samples have been calcined to obtain the nano-oxide catalysts. Characterization by different physicochemical techniques including X-ray diffraction (XRD), scanning electron microscopy (SEM), temperature programmed reduction by hydrogen (H 2 -TPR), and X-ray photoelectron spectrometry (XPS) was carried out. The nanocatalysts