Nano-particles of NiAl2O4 were prepared by co-precipitation and their bulk and surface were characterized by XRD, Raman spectroscopy, N-2-adsorption-desorption analysis, SEMEDS and XPS. The reducibility was studied by TPR and HTXRD techniques under H-2 atmosphere. The synthetized catalyst was made of NiAl2O4 spinel oxide as main phase and of NiO (10%) free oxide. Interestingly, it was shown that the surface was richer in Al species. The catalytic performances in methane dry reforming were evaluated without H2 pretreatment of catalyst. A very high activity was observed with conversion of methane and CO2 at 750 degrees C of 84 and 90 mol%, respectively and high H-2/CO ratio. The amount of coke deposited during the reaction on this spinel was similar to 3.6%. The physico-chemical properties of the catalyst on their behavior in the dry reforming of methane are discussed. (C) 2017 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.