Stiffness and mechanical manipulation of blisters grown on electrochemically intercalated graphite

Electrochemical anion intercalation of highly oriented pyrolytic graphite in mineral acids (such as sulfuric, perchloric, etc.) represents a model system to study (i) the intercalation process of chemical compounds in stratified crystals; (ii) the evolution of gases at the surface and inside the sample and (iii) the evolution of swollen regions of graphite, called blisters. Although the explanation of the blister evolution mechanism can be dated back to the nineties of the last century, many chemical and physical properties have been explored only very recently. In particular, the mechanical properties of blisters on graphite are not widely discussed in the literature. Here, we employ in-situ atomic force microscopy (AFM) to characterize the blister stiffness. The same AFM tip is used to move mechanically the blister on the basal plane or even cut it. As a consequence of this operation, the entrapped gases (namely, CO, CO2 and O2) can deflate and the swollen graphite layers lay down to recompose the graphite basal plane.