Ce 0.5 M 0.5 O 2 (M = Ti, Zr, Hf) nanoparticles have been successfully synthesized by microwave irradiation in the ionic liquid [C 4 mim][Tf 2 N] (1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)amide). The morphology, crystallinity, and chemical composition of the obtained materials were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX), Raman spectroscopy, and N 2 -adsorption measurements. XRD and Raman spectroscopy analyses confirmed the formation of solid solutions with cubic fluorite structure. The catalytic activities of the Ce 0.5 M 0.5 O 2 (M = Ti, Zr, Hf) nanoparticles were investigated in the low-temperature oxidation of CO. Ce 0.5 Zr 0.5 O 2 nanospheres exhibit the best performance (100% conversion at 350 1C), followed by Ce 0.5 Hf 0.5 O 2 (55% conversion at 360 1C) and Ce 0.5 Ti 0.5 O 2 (11% conversion at 350 1C). Heating the as-prepared Ce 0.5 Zr 0.5 O 2 to 600 1C for extended time leads to a decrease in surface area and, as expected decreased catalytic activity. Depending on the ionic liquid the obtained Ce 0.5 Zr 0.5 O 2 exhibits different morphologies, varying from nano-spheres in [C 4 mim][Tf 2 N] and [P 66614 ][Tf 2 N] (P 66614 = trishexyltetradecylphosphonium) to sheet-like assemblies in [C 3 mimOH][Tf 2 N] (C 3 mimOH = 1-(3-hydroxypropyl)-3methylimidazolium). The microwave synthesis superiority to other heating methods like sonochemical synthesis and conventional heating was proven by comparative experiments where the catalytic activity of Ce 0.5 Zr 0.5 O 2 obtained by alternate methods such as conventional heating was found to be poorer than that of the microwave-synthesised material.