This research addressed to prepare a novel type of catalyst from the Cu and Zn metals supported on alumina. To do this, a stable colloidal of Cu and Zn nanoparticle was firstly prepared in W/O microemulsion system. The formulated microemulsion was formed from Cu nitrate and Zn nitrate as a source of metals, cyclohexane as oil phase and the anionic surfactant AOT. Then N2H4 revitalizer was added to introduce microemulsion to change the Cu and Zn ion to its metal form. In order to confirm the formation of Cu and Zn colloidal systems, the UV-vis method have been used. From the DLS result, it was found that the nanoparticles average size for both of the systems were almost 40 nm. Finally, γ-Al2O3 was added to the colloidal systems to make the Cu-Zn/Al2O3 nanocatalyst. The resulted nanocatalyst was characterized by SEM and XRD techniques. The prepared nanocatalysts were tested for hydrogenation reaction of an unsaturated aldehyde.