In this study, we examined the electrochemical synthesis, optical properties and morphology of a novel ZnO/Poly(N-phenylmaleimide-co-hydroxyethyl methacrylate) nanocomposite (ZnO/Poly(N-PhMI-co-HEMA). The formation of ZnO in presence of the copolymer was studied by cyclic voltammetry. The nanocomposite was synthesized by the electrodeposition of Zn2+ at controlled potential (-1.1 V) in presence of the Poly(N-PhMI-co-HEMA). Spherical ZnO nanoparticles, with a diameter ranging between 20 and 50 nm, were observed by transmission electron microscopy (TEM). The overall morphology of the nanocomposite was determined by scanning electron microscopy (SEM) and atomic force microscopy (AFM) from which a grain shape structure, with sizes ranging from 100 to 200 inn, was observed. The presence of the polymeric matrix provoked a slightly increase in the band gap of ZnO as was already determined by UV-Vis. The prepared material can be suitable in the design of electronic devices, in addition to its potential application as biomaterial.