Incipient Anion Intercalation of Highly Oriented Pyrolytic Graphite Close to the Oxygen Evolution Potential: A Combined X-ray Photoemission and Raman Spectroscopy Study

In the present work we used two different electrochemical (EC) techniques, namely cyclic voltammetry (CV) and normal pulsed voltammetry (NPV), applied to a highly oriented pyrolytic graphite (HOPG) electrode for anion intercalation in two different aqueous electrolytes (i.e. perchloric and sulphuric acid). We performed comparative X-ray photoemission (XPS) and Raman spectroscopy studies at various EC potentials. The chemical analysis obtained by XPS and Raman, the latter applied in-situ and in real-time during the electrochemical processes, indicates that at oxygen evolution potential (i.e. before reaching the well-known intercalation stage potentials) the HOPG intercalation process is already active. These results suggest that the intercalated compound is efficiently obtained before reaching higher potentials, which usually cause a detriment of the graphite crystal.