The present research deals with the synthesis of cobalt bimetallic Co/Mo nanocatalysts supported on alumina. The nanocatalysts were prepared by wet impregnation method. The samples were characterized in terms of reducibility, dispersion and particle size using Temperature Programmed Reduction (TPR), Transmission Electron Microscopy (TEM) and BET-surface area analysis. H2-TPR analysis of Co/Al2O3 indicated three temperature regions at 380°C (low temperature), 680°C (medium temperature) and 900°C (high temperature). The incorporation of molybdenum into cobalt nanocatalysts shifted the reduction temperatures towards higher temperature but the percentage of species being reduced at low temperature increased also incorporation of molybdenum reduce the crystallinity but decreased the metal particle size of the catalysts. Increasing metal loading from 5 to 10 wt increased the reducibility of bimetallic nanocatalysts. © 2011 Asian Network for Scientific Information.