Cobalt/copper multilayer formation was analysed over different substrates in order to control the bilayer thickness and quality of coatings. Using a sulphate-citrate bath, at pH 4.7, clectrodeposition conditions were optimised to prepare good alternate Cu/Co layers with high efficiency, by minimising the oxidation of cobalt layers during copper deposition. For multilayers with cobalt and copper layers of several nanometers, direct observation by scanning electron microscopy (SEM) or tapping mode-atomic force microscopy (TMAFM) gives layer thickness in agreement with the value calculated from deposition charges. Therefore, this calculation has been used to estimate the thickness of the thinner layers for which direct observation was difficult or impossible. A relation between the response of different characterisation methods was found. When the thickness of each layer in Cu/Co multilayers is > 1.8-2 run, potentiodynamic stripping experiments show separate peaks related to cobalt and copper oxidation. In these conditions, magnetoresistance of the coating is low. For thinner layers, the stripping response shows overlapping peaks or even a single oxidation peak. In these conditions the magnetoresistance begin to increase.