Cu/Co-Ni-Cu films have been electrochemically synthesized in a single bath using a pulse deposition technique. The results of cyclic voltammetry investigation of the electrodeposition process have been used to optimise bath composition and pulse deposition parameters. The results of in-situ examination of the surface morphology using Atomic Force Microscopy (AFM) have been presented to show reduction in surface roughness following pulse deposition. Pulse plated multilayers of Cu/Co-Ni-Cu have also been characterised using Glancing Angle X-ray Diffraction (GAXRD) studies. (C) 2004 Kluwer Academic Publishers.