Few-layer graphene is synthesized from electrochemically-produced graphite intercalation compounds in aqueous perchloric acid. Although anodic intercalation is more efficient in terms of time, cathodic pre-treatment is preferred to avoid the formation of graphite oxide. The materials are characterized by high resolution transmission electron microscopy and scanning electron microscopy, UV-visible, infrared and Raman spectroscopy. We demonstrate that the method, under the experimental conditions used in this work, does not produce damage to the sp 2 carbon lattice. The synthetic approach using electrochemical-potential control is very promising to obtain, in a controllable manner, graphene with different degrees of oxidation. © 2011 Elsevier Ltd. All rights reserved.