Ni/Co bimetallic nano-cluters have been prepared from the aqueous solution by reducing their corresponding metal salts under suitable conditions. The experimental conditions including the type and concentration of protective agent, feeding order and the pH of the solution that influence the average particle size have been studied in detail. Transmission electron microscopy (TEM) indicates that the shape of those bimetallic nano-cluster particles is spheroid. The alloy structure has been shown by X-ray powder diffraction (XRD). The X-ray photoelectron spectroscopic (XPS) data have confirmed that the nickel and cobalt in the bimetallic nano-clusters are in the zero-valence state. Ni / Co bimetallic nano-cluters have been prepared from the aqueous solution by reducing their corresponding metal salts under suitable conditions. The experimental conditions include the type and concentration of protective agent, feeding order and the pH of the solution that influence that average particle size Transmission electron microscopy (TEM) indicates that the shape of those bimetallic nano-cluster particles is spheroid. The alloy structure has been shown by X-ray powder diffraction (XRD). The X-ray photoelectron spectroscopy ) data have confirmed that the nickel and cobalt in the bimetallic nano-clusters are in the zero-valence state.