A modified solution combustion technique was successfully used to synthesize sub-10 nm crystallites of hybrid CeO2-Al2O 3-CeAlO3. The fuel in the solution combustion was tuned to obtain mixed oxides and solid solutions of the compound. The compounds were characterized by X-ray diffraction, transmission electron microscopy and X-ray photoelectron spectroscopy. XRD and TEM analysis showed the substitution of Al3+ ions in the CeO2 matrix when a combination of glycine, urea, hexamine and oxalyl dihydrazide was used as fuel for the synthesis. The compounds showed high activity for CO oxidation and the activity of the compounds was dependent upon the composition of the oxide. © The Royal Society of Chemistry 2011.