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

An electrochemical exfoliation method for the production of graphene oxide and its characterization by electrochemical techniques are presented here. Graphite rods are used as working electrode in a three‐electrode electrochemical cell, and electro‐exfoliation is achieved by applying anodic polarization in a sulfuric acid solution. The electrochemical process involved two steps characterized by an intercalation at lower potential and an exfoliation at higher potential. The electrochemical behavior of the produced GO is studied through cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). X ray Photoelectronic Spectroscopy (XPS), Raman spectroscopy, Transmission Electron Microscopy (TEM), and Atomic Force Microscopy (AFM) are employed to characterize the structural and chemical properties of the exfoliated GO. The results demonstrate that the electrochemical exfoliation method yields GO materials with varying degrees of oxidation, defect density, and crystallite size, depending on the applied potential and acid concentration. The graphene oxide samples exhibited distinct electrochemical properties, including charge transfer resistance, interfacial capacitance, and relaxation times for the charge transfer, as revealed by CV and EIS measurements with a specifically selected redox probe. The comprehensive characterization performed provides valuable insights into the structure‐property relationships of the GO materials synthesized through electrochemical exfoliation of graphite. Between the sheets: The Intercalation‐Exfoliation (I‐E) method was successfully applied to produce graphene oxide (GO) materials with adjustable oxidation levels, defect density, and crystallite size by tuning applied potential and electrolyte concentration. Investigating the electrochemical properties of these GO samples via CV and EIS measurements with a selected redox probe establishes meaningful correlations between their structural features and performance.