Cd(1-x)Ni(x)S/rGO Composites were synthesized through reflux method. The prepared composite materials were subjected to study the structural, functional groups and transformation of GO to rGO by X- ray diffractometer (XRD), Fourier transform infrared (FTIR) and Raman spectrometer. The presence of elements, binding energies and the transformation were studied by X- ray photoelectron spectroscopy. Thermal properties of as synthesized materials were analyzed by thermogravimetric analysis. An introduction of Ni ions into CdS/rGO composites results increase in integral area and current, which is analyzed by cyclic voltammetry. This composite will be useful in future optoelectronics and energy storage applications. © 2016, Sphinx Knowledge House. All rights reserved.