Chemical analysis of graphene oxide films after heat and chemical treatments by X-ray photoelectron and Micro-Raman spectroscopy

Several nanometer-thick graphene oxide films deposited on silicon nitride-on silicon substrates were exposed to nine different heat treatments (three in Argon, three in Argon and Hydrogen, and three in ultra-high vacuum), and also a film was held at 70 °C while being exposed to a vapor from hydrazine monohydrate. The films were characterized with atomic force microscopy to obtain local thickness and variation in thickness over extended regions. X-ray photoelectron spectroscopy was used to measure significant reduction of the oxygen content of the films; heating in ultra-high vacuum was particularly effective. The overtone region of the Raman spectrum was used, for the first time, to provide a “fingerprint” of changing oxygen content.