This paper is devoted to the characterisation of Ni/alumina reforming catalysts. A special attention was paid to the control of the catalytic properties by the synthesis route of bulk and supported catalysts. In this sense it was shown that the massive formation of NiAl2O4 phase, associated with low NiO/NiAl2O4 molar ratios on the catalyst surface, due to a calcination step at high temperatures was notably beneficial for obtaining highly dispersed nickel catalysts (with a Ni crystallite size of 6 nm) after severe reduction at 850 degrees C. This activation procedure did not affect textural and acidic properties to a large extent. Thus, among the investigated nickel catalysts the 70%NiAl2O4/Al2O3 sample exhibited the best performance in the steam reforming of methane. (C) 2013 Elsevier B.V. All rights reserved.