This paper presents the preparation and characterization of a Rh/Pt bilayer electrodeposited on Pt and its behavior for ethanol oxidation in perchloric acid solution. The electrodes were characterized by atomic force microscopy (AFM) and cyclic voltammetry. The ethanol oxidation was studied on a Pt/Rh/Pt bilayer using cyclic voltammetry and chronoamperometry techniques. In this study, an increase of 268% in the current density peak for the ethanol oxidation and a displacement of 100 mV towards more negative values in the beginning of this process on the Pt/Rh/Pt are observed. The ethanol oxidation at constant potential (E = 0.5 V versus reversible hydrogen electrode (RHE)) showed an increase of 10 times in the current density compared to polycrystalline platinum. (c) 2005 Elsevier B.V. All rights reserved.