Copper Indium diselenide (CISe) layers have been synthesized via two stage processes; electrodeposition of Copper-Indium (Cu-In) and selenization. The effect of complexing agent, citric acid (CA) was studied on the growth of Cu, In and Cu-In layers. Polycrystalline Cu-In layers were electrodeposited from aqueous bath at ? 0.85 V versus Ag/AgCl reference electrode. The structural, optical, morphological, compositional, photo-elctrochemical and optoelectronic properties for Cu-In layer and selenized Cu-In layers are studied. Three prominent reflections of tetragonal crystal structure of CISe, (112), (204/220) and (312/116) were exhibited in selenized layers. Nearly uniform, void-free surface morphology was observed in selenized samples. Upon selenization of Cu-In layers prepared with 0.1 M CA produced stoichiometric CISe thin films. The energy band-gap values are estimated between 1.05 eV to 1.18 eV. Photoelectrochemical cell measurement revealed the growth of p-type and n-type conductivity of CISe thin films. The peaks related to chalcopyrite CISe and ordered defect compound are observed in Raman analyses. The superstrate solar cell structure prepared with selenized Cu-In layer deposited in presence of 0.1 M CA measured 4.05% efficiency. The values of R-s, 7.42 omega-cm(2), 0.94 omega-cm(2) and G, 1.01 mS/cm(2) 10.25 mS/cm(2) were calculated under dark and illuminated condition, respectively. We believe that the measured efficiency is low; however the further improvement is possible by optimizing the surface treatment conditions.