In recent years, nanostructured materials like compositionally modulated alloys have been widely studied. These materials consist of alternated layers of different metals or alloys with a thickness less than 100 nm. They have very promising properties, which can’t be achieved with bulk materials. Multilayered films have been the subject of numerous recent studies due to their improved physico-mechanical, optical, electrical, magnetic, and magnetic-optic properties compared to traditional alloys [1]. The aim of this study is to investigate the electrodeposition of multilayers from a single bath, and to explore ways to characterize such multilayered systems. The research work was focused on CoW/Cu alternated layers obtained by electrodeposition. Cu/CoW multilayers were produced with a wide range of sublayer thickness by electrodeposition on steel substrates covered with a nickel seed-layer. The electrochemical studies allowed to select the proper current density for achieving an alternated deposition of CoW and Cu sublayers. SEM investigations confirmed the periodical structure in multilayers at bi-layer periods above 200 nm. Hardness of Cu/CoW multilayers depends on the bi-layer period and the electrodeposition parameters. The Cu/CoW multilayers show in most cases an increase in hardness compared to single CoW layers deposited under the same electroplating conditions (fig. 1). In dry sliding fretting tests, Cu/CoW multilayers withstand well the tangential forces at low normal forces, but at high normal forces of 10 N the wear resistance of these coatings depends very strongly on the presence of copper in the electrodeposited layers.figureFig. 1. Nanohardness, measured by continuous multi cycle method for different electrodeposition parameters (see Table 1).TableTable 1. Electrodeposition parameters used to obtain Cu/CoW multilayers