The thermal reduction behavior of graphite oxide (GO) film in an air atmosphere during a continuous heating process was monitored in situ using temperature-dependent infrared (IR) spectroscopy and synchrotron radiation wide-angle X-ray diffraction (WAXD) techniques. The results show that most of the water adsorbed by the GO sheets is removed by heating them to 130 °C. The dehydration process leads to a slight decrease of the interplane distance of the GO sheets. The IR data suggest that the thermal reduction occurs starting at 160 °C. The synchronous change of the of hydroxyl and carbonyl stretching mode (ν(-OH) and ν(C=C)) bands of GO between 160 and 210 °C suggest that the recovery of conjugated structure is mainly due to the reduction of -OH groups in this temperature region, in which the <i>d</i> spacing has not been affected. When the temperature reaches 210 °C, the rapid reduction of C=O groups together with the removal of the residual -OH and ether (C-O-C) groups leads to the sudden collapse of the GO sheets. Based on these findings, we present a schematic of the thermal stability of GO film in a continuous heating process, in which the thermal-induced chemical and crystallographic structural changes of the GO film have been correlated.

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