Temperature Effects on the HOPG Intercalation Process

Graphite intercalation via chemical strategies is a common procedure to delaminate stratified crystals and obtain a suspension of graphene flakes. The intercalation mechanism at the molecular level is still under investigation in view of enhancing graphene production and reducing damage to the original pristine crystal. The latter, in particular, can undergo surface detriment due to both blister evolution and carbon dissolution. The role of the electrolyte temperature in this process has never been investigated. Here, by using an in-situ atomic force microscopy (AFM) apparatus, we explore surface morphology changes after the application of fast cyclic-voltammetries at 343 K, in view of de-coupling the crystal swelling phenomenon from the other electrochemical processes. We find that blisters do not evolve as a consequence of the increasing temperature, while the quality of the graphite surface becomes significantly worse, due to the formation of some adsorbates on possible defect sites of the electrode surface. Our results suggest that the chemical baths used in graphite delamination must be carefully monitored in temperature for avoiding undesired electrode detriment