A novel two-step method was employed to synthesize gold nanoparticles dispersed on boron-doped diamond (BDD) electrode. It consisted of sputter deposition at ambient temperature of maximum 15 equivalent monolayers of gold, followed by a heat treatment in air at 600 degrees C. Gold nanoparticles with an average diameter between 7 and 30nm could be prepared by this method on polycrystalline BDD film The obtained Au/BDD composite electrode appeared stable under conditions of electrochemical electrode. characterization performed using ferri-/ferrocyanide and benzoquinone/hydroquinone redox couples in acidic medium. The electrochemical behavior of Au/BDD was compared to that of bulk Au and BDD electrodes. Finally, the Au/BDD composite electrode was regarded as an array of Au microelectrodes dispersed on BDD substrate. (C) 2008 Elsevier Ltd. All rights reserved.