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Materials 2022, 15, 4639 3 of 15 at lower temperatures for minimal environmental impact. In detail, we present the elec- trochemical exfoliation of graphene oxide, where anodic pretreatment based on NaOH is exploited to distance the atomic layers in the graphite rods and facilitate exfoliation (Figure1b). Wequalitativelydiscussthisswellingprocessandwhethertheproposedproto- col can be promoted to the up-scaling level, highlighting the effective yield. We characterize the produced GO powder with several techniques and study its functionalities. Finally, we thermally reduce the obtained powder to decrease the functional groups and compare the powder conductivity with respect to what is usually produced via the Hummers methods. Our final product maintains its properties throughput different volumina, confirming the upscalability of the process, which quantitatively performed well as it produced 20 g of GO per hour, outperforming the most recent works in this field [32,33]. Figure 1. (a) Front (left) and top (right) sides of the electrochemical exfoliation set-up. The lateral view shows the cooling system and the power supply while the top view pictures the electrodes’ position in the electrochemical reactor. The dimensions refer to a 1600 mL reactor. (b) Production protocol for the up-scaling process with anodic pretreatment in 1 M NaOH. (c) Cyclic voltammetry applied to a graphite rod in 1 M NaOH (scan rate 10 mV/s; 6 cycles: dark green to light green). (d) Cyclic voltammetry applied to a graphite rod in 1 M H2SO4 (scan rate 10 mV/s; 6 cycles: dark color to light color). Red indicates an untreated graphite rod and blue a graphite rod pretreated anodically in 1 M NaOH for 10 min.PDF Image | Electrochemical Production Thermal Reduction Graphene Oxide
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