Temperature-dependent deoxygenation during sulfonation for graphene oxide reduction

The objective of this study was to elucidate the sulfonation behaviour of graphene oxide (GO) across a temperature range of 50 °C, 100 °C, and 150 °C under a nitrogen atmosphere. Analysis revealed a significant reduction in –OH, C-O, and O-C-O functional groups, facilitating a substantial conversion from sp3 to sp2 carbon hybridization. Specifically, the sp2 carbon content increased from 37.43 ± 2.0 % in GO to 50.32 ± 2.5 % in GO-SO3H50, 43.72 ± 3.0 % in GO-SO3H100, and 47.92 ± 2.8 % in GO-SO3H150. At higher temperatures, deoxygenation led to a decrease in C-S density due to the pronounced removal of oxygen moieties, which constrained the availability of functional groups for −SO3H binding. SEM imaging corroborated that sulfonated GO retained its disordered stacked layer configuration, consistent with the precursor. These results affirm that sulfonation is a viable alternative for synthesizing reduced graphene oxide (rGO), with enhanced sp2 carbon content and modified structural characteristics.

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