Synthesis of Reduced Graphene Oxide with Adjustable Microstructure Using Regioselective Reduction in the Melt of Boric Acid: Relationship Between Structural Properties and Electrochemical Performance

The melt of H₃BO₃ was used to reach a controllable reduced graphene oxide (rGO) synthesis protocol using a graphene oxide (GO) precursor. Thermogravimetric analysis and differential scanning calorimetry (TG/DSC) investigation and scanning electron microscopy (SEM) images have shown that different from GO powder, reduction of GO in the melt of H₃BO₃ leads to the formation of less disordered structure of basal graphene planes. Threefold coordinated boron atom acts as a scavenger of oxygen atoms during the process of GO reduction. Fourier-transform infrared (FTIR) spectra of synthesized products have shown that the complex of glycerol and H₃BO₃ acts as a regioselective catalyst in epoxide ring-opening reaction and suppress the formation of ketone C=O functional groups at vacancy sites. Thermal treatment at 800 °C leads to the increased concentration of point defects in the backbone structure of rGO. Synthesized materials were tested electrochemically. The electrochemical performance of these materials essentially differs depending on the preparation protocol. The highest charge/discharge rate and double-layer capacitance were found for a sample synthesized in the melt of H₃BO₃ in the presence of glycerol and treated at 800 °C. The effect of optimal porosity and high electrical conductivity on the electrochemical performance of prepared materials also were studied.