Stable metallic Cu/Zn nanoparticles were prepared in the base oil phase by hydrothermal method. The physical properties, such as crystal structure, crystallite size and crystallinity according to synthesis conditions have been investigated by XRD, FT-IR and TEM. In addition, 4-ball test has been performed in order to investigate the frictional wear properties of prepared nanosized Cu/Zn particles. The peaks of the X-ray diffraction pattern indicate that the particle size was very small and crystallinity of Cu/Zn particles was good. The micrographs of TEM showed that nanosized Cu/Zn particles possessed a spherical morphology with a narrow size distribution. The crystallite size of the Cu/Zn particles synthesized in base oils was 23-30 nm. It was found that the antiwear capacity increases with increasing Cu/Zn concentration. When the concentration of Cu/Zn was 5.0 wt%, the wear scar diameters was 0.38 mm.