Ultra-dispersed catalysts give an improvement over the main reactions activity by having a low deactivation rate. They provide as well other advantages like a diminution in the catalysts metal concentration, a reduction in contaminants and also these catalysts can be used in almost every area where heterogeneous catalysts are used. Catalysts synthesis optimization is important to improve process recovery, especially in hydrocracking/hydrotreating processes, where feedstock is vacuum residue. Here, we have evaluated the catalytic performance of two molybdenum-nickel catalysts prepared using different emulsion formulation, named E-T (base catalyst) and AT-48 (new catalyst). Our results showed that, the percentage of converted products for VR 500 degrees C*, asphaltenes and microcarbon are comparable for both E-T and AT-48 catalysts, despite the fact that for the latter a lower molybdenum concentration was used. In addition, post-catalytic particles analyses using SEM and TEM techniques demonstrated that AT-48 catalyst showed a non-aggregated and homogeneous narrower distribution of metallic particles than E-T one. The lower average particle size distribution is related to the improvement of the liquid product yields for the hydroconversion of Mery/Mesa VR using the AT-48 catalyst. (C) 2012 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.