In this paper, the possibility of mechano-chemical synthesis, as a single step process for preparation of nanostructured nickel aluminate spinel powder from NiO/Al2O3 spent catalyst was investigated. Powder samples were characterized in terms of composition, morphology, structure, particle size and surface area using complementary techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM). differential thermal analysis (DTA) and volumetric adsorption of nitrogen. It was found that formation of spinel was possible after 60 h of milling with no heat treatment. Additionally, influence of mechanical activation on the heat treatment temperature was discussed. It was observed that heat treatment of 15 h milled sample at 1100 degrees C is enough to produce nickel aluminate spinel. A product of direct mechanical milling showed higher value of surface area (42.3 m(2)/g) and smaller crystallite size (12 nm) as compared to the heat treated product. (C) 2011 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.