Electrochemical Exfoliation of Graphene Oxide: Unveiling Structural Properties and Electrochemical Performance

Abstract

An electrochemical exfoliation method for the production ofgraphene oxide and its characterization by electrochemicaltechniques are presented here. Graphite rods are used asworking electrode in a three-electrode electrochemical cell, andelectro-exfoliation is achieved by applying anodic polarizationin a sulfuric acid solution. The electrochemical process involvedtwo steps characterized by an intercalation at lower potentialand an exfoliation at higher potential. The electrochemicalbehavior of the produced GO is studied through cyclicvoltammetry (CV) and electrochemical impedance spectroscopy(EIS). X ray Photoelectronic Spectroscopy (XPS), Raman spectroscopy,Transmission Electron Microscopy (TEM), and AtomicForce Microscopy (AFM) are employed to characterize thestructural and chemical properties of the exfoliated GO. Theresults demonstrate that the electrochemical exfoliation methodyields GO materials with varying degrees of oxidation, defectdensity, and crystallite size, depending on the applied potentialand acid concentration. The graphene oxide samples exhibiteddistinct electrochemical properties, including charge transferresistance, interfacial capacitance, and relaxation times for thecharge transfer, as revealed by CV and EIS measurements with aspecifically selected redox probe. The comprehensive characterizationperformed provides valuable insights into the structurepropertyrelationships of the GO materials synthesized throughelectrochemical exfoliation of graphite.