Nowadays, HOPG has focused an increasing interest in electrochemistry due to its layered structure, from which graphene sheets can be extracted. In view of industrial implementation, large-scale production and quality enhancement of graphene flakes should be combined to a reduction of the production cost. In these perspectives, electrochemical strategies are successful and graphene is obtained by anion intercalation inside the graphite crystal at specific electrochemical potentials, producing a delaminating effect. Most of the works analyze the graphene products and good results are reported in the literature1. However, it has been recently noted that there is an unjustified lack of knowledge regarding the evolution of the immersed graphite, which could limit the graphene sheet sizes2. To overcome this bottleneck, in this talk we discuss the potentiality offered by a combined high resolution study of the surface evolution by electrochemical atomic force and scanning tunneling microscopy (EC-AFM and EC-STM, respectively) together with a traditional cyclic-voltammetry (CV) and a normal pulse-voltammetry (NPV) analysis. The latter allows revealing the kinetics of the different electrochemical processes3.
In this research, we investigate the behavior in different electrolytes (nominally, sulfuric, perchloric, phosphoric and hydrochloric acids) and we proved that the graphite basal plane undergoes carbon dissolution phenomena, as soon as a high EC potential is applied4,5. This represents a clear detriment in view of graphene production. Furthermore, the electrode is damaged by blisters, well before the acid intercalation process, which suggests a re-examination of the existing interpretative model6.
 C. T. J. Low et al. Carbon 54 (2013) 1-21; V. Nicolosi et al. Science 340 (2013) 1226419.
 Z. Y. Xia et al. Adv. Funct. Mater. 23 (2013) 4684-4693.
 R. Yivlialin et al. Phys. Chem. Chem. Phys. 19 (2017) 13855.
 G. Bussetti et al. J. Phys. Chem. C 120 (2016) 6088-6093.
 R. Yivlialin et al. Beilstein J. Nanotechnol. 7 (2016) 1878-1884.
 K. W. Hathcock et al. Anal. Chem. 67 (1995) 2201-2206.