Study and Comparison of Different Routes to Synthesize Reduced Graphene Oxide

The feasibility of graphene oxide (GO) obtained by both Hummers and Tour method to prepare reduced graphene oxide (rGO) as well as chemically reduction under different experimental conditions were evaluated with the objective of establishing the key items that should be considered when performing the synthesis of GO and rGO. This key items can be supportive to select the most feasible methodology to synthesize GO and rGO depending on the future application. Reduced graphene oxide was prepared by combining chemical and solvothermal as well as combined reduction adding a final thermal annealing step. Obtained GO and rGO were characterized by XRD, Raman spectroscopy, XPS and BET analysis. A higher oxidation degree was achieved for samples from Tour method than those oxidized by Hummers method. On the contrary, lower oxidation degree from Hummers graphene oxide (GO-H) facilitates the subsequent reduction process, leading to a higher reduced rGO. Hence, rGO samples obtained from the Hummers method in the different reduction treatments presented higher C/O atomic ratios than the corresponding Tour method. In addition, the combination of a solvothermal treatment and chemical reduction, including a final annealing stage, increases significantly the value of the C/O ratio as well as it contributes to decrease the defect density and the restoration of π-conjugated structure. Besides, rGO samples obtained from Tour method presented higher SSA and pore volume than those samples obtained from Hummers method. Results from this study suggest the suitability of Tour graphene oxide (GO-T) for chemical functionalization which is very useful for several applications. In addition, GO and rGO coming from Tour method are more appropriate to applications in which high surface area is required. Taking into account the vast possible applications for chemically-exfoliated graphene the findings of this study could help to select the best method for oxidising graphite depending on the intended application.