The aim of this work is to evaluate the influence of glycine fuel used in a stoichiometric proportion and with a 10% and 20% excess of this fuel in the preparation of NiAl2O4 catalyst by combustion reaction. The powders were characterized by XRD, textural analysis by the BET nitrogen adsorption method, particle size distribution, and FTIR. The results show the presence of NiAl2O4 as a major phase and traces of NiO and Ni in all the catalysts studied here. The crystallite sizes were 22 nm in the stoichiometric composition and 18 and 9 nm, respectively, in the composition containing 10% and 20% excess glycine. The powder obtained from all the compositions presented morphological characteristics with irregular plate-shaped agglomerates. The increase in excess glycine caused the particle size in the three compositions to decrease to 59, 54 and 38 nm and the agglomerate size to increase to 7,8 and 12 mu m, respectively. (C) 2011 Elsevier Ltd. All rights reserved.