In this paper, well-crystalline Ag2O/ZnO and ZnO/Ag2O nanocomposites were prepared by a facile chemical method. Structural, morphological and optical properties of the nanocomposite were studied using various advanced characterization techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FTIR), UV-Visible (UVVis) and photoluminescence (PL) spectroscopy. The Ag2O and ZnO were clearly identified in the composite from SEM and TEM. Significant shifting observed in the both UV-Vis and PL spectroscopy. In addition, electrocatalytic activity of the Ag2O/ZnO and ZnO/Ag2O nanocomposites studied by an electrochemical workstation. The ZnO/Ag2O nanocomposites showed better optical and electrochemical properties due to decorating the low-band gap Ag2O on the surface of hexagonal structure ZnO nanoparticles.