The good adhesion of electrodeposited Ni clusters on carbon supports was demonstrated; the metallic clusters were deposited on recompressed graphite (Papyex) and PAN-based fibres (Toray T300) by electrodeposition technique. For both substrates, the process parameters were optimized in order to obtain a uniform and dense spatial distribution of the Ni clusters with narrow size distribution peaked around 50 nm. The morphology of the Ni clusters was characterized by SEM and AFM. The cluster adhesion to the substrates was tested with several experiments: Ni coated carbon substrates were dipped into different liquids, processed with a variety of treatments (immersion, magnetic stirring, centrifugation and ultrasonic bath) and then observed with SEM. Moreover, nano-scratch tests were performed on Ni coated supports by means of an AFM equipped with a diamond tip. (c) 2005 Elsevier B.V. All rights reserved.