Morphological characteristics and electrochemical behaviour of nickel- Polyvinylchloride (Ni-PVC) composite were studied in alkaline solutions, It was found that prolonged cathodic polarization and continue potential cycling on samples seriously alters the surface morphology, surface composition and adsorption properties of the composite samples. This was confirmed by SEM, EDS, IR spectroscopy and osmometry. Oxygen evolution reaction (oer) was also studied on fresh and pre-activated samples by stationary polarization curves.