Al2O3, MgO and MgAl2O4 nanocrystalline and mesoporous materials were prepared by simple solution combustion synthesis using urea and metal nitrates and the effect of metal nitrate/urea ratio was investigated. The metal oxides that were found suitable for catalytic purposes were tested in catalytic partial oxidation of methane (CPOM). It was observed that the oxidizer/fuel ratio could affect the structure phase, crystallinity and morphology of the synthesized materials. gamma-Al2O3 was obtained when the equivalence ratio was 2, and at lower ratios, the obtained phase was alpha-Al2O3. The cubic MgO phase was obtained at each ratio but the material yield was low below the equivalence ratio of 4. Highly crystalline MgAl2O4 was obtained at fuel-rich conditions only. 10% (wt.) Ni loaded MgAl2O4-2 and MgO-4 showed high activity (>90% CH4 conversion) and product selectivity (>98% H-2 and CO selectivity) at 800 degrees C under 157,5001 kg(-1) h(-1). (C) 2019 Elsevier B.V. All rights reserved.