Cu/ZnO in nanosizes have been synthesized using ethylene glycol at various conditions. The effects of reaction temperature, extent of reduction, various precursors such as CuX2·nH2O, ZnX2·nH2O (X = Cl−, NO3−, CH3CO2−), the addition of water and the removal of volatile compounds including water were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), and dynamic light scattering (DLS). Cu/ZnO powders with an average diameter of as low as 50 nm was obtained with a very low polydispersity in the absence of a protective polymer. Ethylene glycol oxidation products were also identified by Fourier transform infrared (FTIR) spectroscopy. The morphology of Cu/ZnO powders and the yield of powders are found to be strongly dependent on the synthesis conditions.