Composition modulation in copper/cobalt (copper) multilayers grown by a pulse train based deposition technique has been studied using grazing angle X-ray diffraction and X-ray photoelectron spectroscopy techniques. Higher pulse frequency employed during Pulse electrodeposition, has been shown to yield a mixed copper/cobalt phase. Formation of coherent multilayers exhibiting antiphase oscillation of the Cu/Co composition profile has been demonstrated using pulse frequency (duty cycles) of 200 Hz (50%) and 400 Hz (80%) for copper and cobalt electrodeposition, respectively. (c) 2006 Elsevier B.V. All rights reserved.