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ECS Journal of Solid State Science and Technology, 2020 9 093013 Figure 2. A timeline of events in the graphene history.84,91 potential of +10 V for 10 min. The yield of this process was about 60% and the product obtained has 1–3 layers. Based on the results of the above research, sulfuric acid is an electrolyte suitable for electrochemical intercalation and graphite exfoliation process. The size of the sulfate ions (0.46 nm) which is similar to the graphite interlayer distance (0.335 nm) may contribute to the intercalation process. In addition, electrolysis of sulfate ions and co-intercalated water causes the formation of gases such as SO2, O2 and H2.157,158 The use of acid electrolyte caused graphite to be flaking during the intercalation process. This process produce graphene with several layers while the expected product was one layer.15,130,159,160,161 Parvez et al., (2014) proposed a general concept for electrochemical stripping of graphite in inorganic salts as shown in Fig. 7.162 Graphite electrodes were immersed in ammonium sulfate solution [(NH4)2SO4, H2O] and applied potential was set to +10V (Fig. 7a). At this potential, water reduction occurs at the cathode and produces hydroxyl (OH–) ions as strong nucleophiles. Nucleophiles attack the edges and boundaries of the graphite grains, resulting in oxidation reactions and intercalation of sulfate ions in the graphite layer (Fig. 7b). Oxidation reactions induce the depolarization and expansion of the graphite layer (Fig. 7c). During this process, the water molecules act as a co-intercalation with SO42− ions. Oxidized water molecules and SO42− ion reduction produce gas species (SO2, O2,PDF Image | Progress in Graphene Synthesis
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