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Despite the recent developments in Graphene Oxide due to its importance as ahost precursor of Graphene, the detailed electronic structure and its evolutionduring the thermal reduction remain largely unknown, hindering its potentialapplications. We show that a combination of high resolution in situ X-rayphotoemission and X-ray absorption spectroscopies offer a powerful approach tomonitor the deoxygenation process and comprehensively evaluate the electronicstructure of Graphene Oxide thin films at different stages of the thermalreduction process. It is established that the edge plane carboxyl groups arehighly unstable, whereas carbonyl groups are more difficult to remove. Theresults consistently support the formation of phenol groups through reaction ofbasal plane epoxide groups with adjacent hydroxyl groups at moderate degrees ofthermal activation (~400 {\deg}C). The phenol groups are predominant overcarbonyl groups and survive even at a temperature of 1000 {\deg}C. For thefirst time a drastic increase in the density of states (DOS) near the Fermilevel at 600 {\deg}C is observed, suggesting a progressive restoration ofaromatic structure in the thermally reduced graphene oxide

Probing the Thermal Deoxygenation of Graphene Oxide using High Resolution In Situ X-Ray based Spectroscopies