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Glassy carbon is a graphene-rich form of elemental carbon obtained frompyrolysis of polymers, which is composed of three-dimensionally arranged,curved graphene fragments alongside fractions of disordered carbon and voids.Pyrolysis encompasses gradual heating of polymers above 900 degree C underinert atmosphere, followed by cooling to room temperature. Here we report on anexperimental method to perform in situ high-resolution transmission electronmicroscopy (HR-TEM) for the direct visualization of microstructural evolutionin a pyrolyzing polymer in the 500-1200 degree C temperature range. The resultsare compared with the existing microstructural models of glassy carbon.Reported experiments are performed at 80 kV acceleration voltage usingMEMS-based heating chips as sample substrates to minimize any undesiredbeam-damage or sample preparation induced transformations. The outcome suggeststhat the geometry, expansion and atomic arrangement within the resultinggraphene fragments constantly change, and that the intermediate structuresprovide important cues on the evolution of glassy carbon. A completeunderstanding of the pyrolysis process will allow for a general process tuningspecific to the precursor polymer for obtaining glassy carbon with pre-definedproperties.

Evolution of Glassy Carbon Microstructure: In Situ Transmission Electron Microscopy of the Pyrolysis Process