In view of large-scale applications, electrochemical exfoliation of graphite for the production of graphene sheets must follow chemical processes that ensure high quality of the products -wide-size graphene foils, single- or few-layer thickness, and low level of defectivity -in order to guarantee high electrical transport and good mechanical properties. Understanding the exfoliation process of graphite at the atomic scale, that is, the intercalation of graphene layers in the electrolyte solution, is fundamental to really be able to control and optimize such processes. This can be obtained, for instance, by investigation of the exfoliated graphite -the surface of the original crystal left behind in the chemical solution- and by real-time monitoring of graphite surface morphological and structural modifications during the exfoliation process. Here, we monitor graphite surface changes as a function of the electrochemical potential by both electrochemical (EC) atomic force microscopy and EC scanning tunneling microscopy coupled with cyclic voltammetry. Following this strategy, we disclose the surface modifications encountered during the early stages of anion intercalation, for different electrolytes: surface faceting, step erosion, terrace damages, and nanoprotrusions, all affecting the graphite surface and therefore the exfoliation process. Our results represent a key step toward a full investigation of the intercalation process in graphite. Within the current debate on the exfoliation of layered crystals, these data potentially represent important information for investigation of the intercalation process in graphite and, on the other hand, for further optimization of the electrochemical protocol for graphene production

We report on a combined X-ray and UV photoemission spectroscopy study (XPS and UPS) of organicinorganic perovskites prepared from a solution of lead chloride (PbCl 2 ) and methylammonium iodide (CH 3 NH 3 I). The XPS intensities are consistent with a pure iodide perovskite (CH 3 NH 3 PbI 3 ), with no detectable chloride left. However, we found that the elimination of chloride results in residual methylamine molecules (CH 3 NH 2 ) trapped within the perovskite crystal lattice. Furthermore, we show that vacuum annealing or sputtering induce the formation of a thin PbI 2 layer at the crystal surface which acts as a surface barrier blocking electron transfer from the underlying perovskite film.

In the currently accepted picture, when graphite is immersed and polarized in a diluted sulfuric acid electrolyte, the surface undergoes an invasive process due to the intercalation of solvated sulphate anions inside the crystal. The following evolution of CO, CO and O promotes the surface swelling and the growth of blisters. Here, we give evidence that the appearance of blisters affects the graphite surface as soon as the oxygen potential is reached, i.e. before the traditionally accepted anion intercalation stage, which instead is demonstrated slowing the blister development. These results suggest a new picture of the solvated anion intercalation in graphite with respect to the current interpretative model.

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Driven by the perspective of large-scale, high-quality graphene production via chemical routes, the investigation of electrochemical anion intercalation between the basal graphite planes has seen a renewed interest among the scientific community. At relatively high electrochemical potentials, when oxidation occurs,\ud graphite electrodes undergo significant anion intercalation processes. The latter swell the uppermost graphite layers (i.e., graphene sheets), reduce the interplane interaction and favor the graphite delamination\ud in liquid. Different intercalation stages are observed in a perchloric acid electrolyte, which are usually interpreted in terms of different perchlorate penetration depths. Nonetheless, the understanding of the morphological changes occurring at the electrode surface during the different intercalation stages is still not\ud completely clear. We combine different microscopy techniques including optical, scanning electron and electrochemical atomic force microscopies to analyze the morphological evolution of the graphite surface at different length scales as a function of the applied electrochemical potential. Whereas both carbon dissolution and blisters affect the surface on the micrometer scale as soon as intercalation starts, we find that the graphite surface is cracked on the sub-millimeter scale only when intercalation at a higher potential is reached, inducing a significant aging of the electrode surface