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Graphene oxide finds applications in different fields of science, includingenergy conversion. Electrochemical reduction of graphene oxide (GO)significantly improves its conductivity. However, the kinetics of this processdepends on the solvent, supporting electrolyte, pH, and numerous other factors.Most studies report the macroscopic views and ex-situ properties of reduced GO.To expand the knowledge about GO reduction, in this study, we used cyclicvoltammetry (CV), simultaneous 2 points and 4 points resistance measurement(s24), conductive atomic force microscopy (AFM), and theoretical calculations.Using CV, we demonstrated that the choice of supporting electrolyte (KCl orLiCl) influences the potential range in which electrochemical GO reductionoccurs. The activation energy of this process was estimated to be below 30 kJmol-1 in both electrolytes, being significantly lower than that required forthermal reduction of GO. Simultaneous in situ s24 resistance measurementssuggest that GO films reach a highly conductive state at deep negativepotentials, with an abrupt, irreversible switch from non-conductive to theconductive state. However, conductive AFM presents a more exact picture of thisprocess: the reduction of GO films starts locally while the formed conductiveislands grow during the reduction. This mechanism was confirmed by theoreticalcalculations indicating that the reduction starts on isolated oxygen-functionalgroups over the GO basal plane, while clustered OH groups are more difficult toreduce. The presented results can help in tailoring reduced GO for a particularelectrochemical application by precisely controlling the reduction degree andpercentage of the conductive area of the reduced GO films.

Electrochemical reduction of thin graphene-oxide films in aqueous solutions: restoration of conductivity