The effects of the SAR (14 and 38) and of the methodology of introduction of nickel ( wetness impregnation and ion exchange) on catalyst activation were investigated in Ni/USY model catalysts submitted to two activation treatments: reduction ( A) and reduction/calcination/reduction, successively ( B). For the catalysts prepared by wetness impregnation, a marked increase in the catalytic activity after treatment B was observed. On the basis of the catalyst efficiency toward ethane hydrogenolysis, the lower SAR catalyst presents a threefold higher activity. On the contrary, the catalysts prepared by ion exchange, as well as a model catalyst prepared by wetness impregnation over a USY exhaustively exchanged with nickel ions, do not present measurable increasing of the catalytic activity under the same activation conditions. Monitoring the catalyst activation by EXAFS indicates the formation of nickel clusters in the impregnated catalysts after activation treatment B, which should be responsible for the high catalytic activity. However, TEM images reveal a bimodal particle size distribution, with large (ca. 20 nm) and small nickel particles. Temperature-programmed reduction performed under the same conditions of catalyst activation suggests that only the small nickel particles are activated under the experimental conditions adopted in this work.