The present work demonstrates a simple and low-cost method to produce bulk quantities of graphene material through the thermal treatment of graphite oxide (GO). GO of a high oxidation degree was synthesized by electrochemical overoxidation of natural graphite in 11 M H₂SO₄ using linear sweep voltammetry (LSV) technique. The thus synthesized GO was thermally exfoliated-reduced at 500 °C in air, giving the final product – thermally reduced graphite oxide (TRGO). It should be emphasized that the process of TRGO formation from electrochemically obtained GO is for the first time described in the present work. Due to shock treatment, the BET specific surface area of TRGO increased from 4 to 455 m² g⁻¹. Additionally, a decrease in the concentration of oxygen functionalities was also observed. Thermal stability of electrochemically synthesized GO was investigated by thermogravimetric analysis (TGA). In order to characterize the synthesized TRGO, investigations by X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) were performed.

In the present work we demonstrate a simple and effective way to produce bulk quantities of graphene material. For the first time, graphite oxide (GO), synthesized by electrochemical treatment of natural graphite in HClO₄ aqueous solution, was used to obtain thermally exfoliated-reduced graphite oxide (TRGO). Herein, GO was thermally exfoliated and reduced at 500 °C in air, giving the final product of TRGO. Due to shock treatment, the volume of the synthesized TRGO drastically increased compared to the starting GO. Furthermore, the exfoliation process resulted in a significant decrease in the concentration of oxygen functionalities. The choice of GO exfoliation temperature was preceded by thermogravimetric analysis (TGA). TRGO was characterized using X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and atomic force microscopy (AFM) analysis.