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Direct Observation of Graphene Growth and Associated Copper Substrate Dynamics by in Situ Scanning Electron Microscopy

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Fritz Haber Institute of the Max Planck Society, D-14195 Berlin-Dahlem, Germany
Institute of Low Temperature and Structure Research, Polish Academy of Sciences, 52-422 Wroclaw, Poland
§ Laboratory for Molecular Physics, Ruđer Bošković Institute, 10000 Zagreb, Croatia
Institute of Functional Nano & Soft Materials (FUNSOM), Collaborative Innovation Center of Suzhou Nano Science and Technology, Soochow University, Suzhou 215123, Jiangsu, China
*Address correspondence to [email protected]
Cite this: ACS Nano 2015, 9, 2, 1506–1519
Publication Date (Web):January 13, 2015
Copyright © 2015 American Chemical Society

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    Abstract Image

    This work highlights the importance of in situ experiments for an improved understanding of graphene growth on copper via metal-catalyzed chemical vapor deposition (CVD). Graphene growth inside the chamber of a modified environmental scanning electron microscope under relevant low-pressure CVD conditions allows visualizing structural dynamics of the active catalyst simultaneously with graphene nucleation and growth in an unparalleled way. It enables the observation of a complete CVD process from substrate annealing through graphene nucleation and growth and, finally, substrate cooling in real time and nanometer-scale resolution without the need of sample transfer. A strong dependence of surface dynamics such as sublimation and surface premelting on grain orientation is demonstrated, and the influence of substrate dynamics on graphene nucleation and growth is presented. Insights on the growth mechanism are provided by a simultaneous observation of the growth front propagation and nucleation rate. Furthermore, the role of trace amounts of oxygen during growth is discussed and related to graphene-induced surface reconstructions during cooling. Above all, this work demonstrates the potential of the method for in situ studies of surface dynamics on active metal catalysts.

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    ESEM movies showing the copper surface during annealing in hydrogen, the metal-catalyzed CVD growth of graphene on a copper surface at 1000 °C, and copper surface reconstruction during cooling. AFM movies recorded after growth. EDX characterization of silica particles. Raman and STM characterization of the grown graphene. Supporting figures. This material is available free of charge via the Internet at

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