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High-Speed in Situ X-ray Scattering of Carbon Nanotube Film Nucleation and Self-Organization
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    High-Speed in Situ X-ray Scattering of Carbon Nanotube Film Nucleation and Self-Organization
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    Mechanosynthesis Group, Department of Mechanical Engineering, University of Michigan, 2350 Hayward Street, Ann Arbor, Michigan 48109, United States
    Stanford Synchrotron Radiation Lightsource, SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, California 94025, United States
    § Department of Chemical Engineering, Stanford University, Stanford, California 94305, United States
    Cornell High Energy Synchrotron Source (CHESS), Cornell University, Route 366 & Pine Tree Road, Ithaca, New York 14853, United States
    Laboratory of Atomic and Solid State Physics, Department of Physics, Cornell University, Ithaca, New York 14853, United States
    *Address correspondence to [email protected]
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    ACS Nano

    Cite this: ACS Nano 2012, 6, 6, 5091–5101
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    https://doi.org/10.1021/nn300758f
    Published May 9, 2012
    Copyright © 2012 American Chemical Society

    Abstract

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    The production of high-performance carbon nanotube (CNT) materials demands understanding of the growth behavior of individual CNTs as well as collective effects among CNTs. We demonstrate the first use of grazing incidence small-angle X-ray scattering to monitor in real time the synthesis of CNT films by chemical vapor deposition. We use a custom-built cold-wall reactor along with a high-speed pixel array detector resulting in a time resolution of 10 msec. Quantitative models applied to time-resolved X-ray scattering patterns reveal that the Fe catalyst film first rapidly dewets into well-defined hemispherical particles during heating in a reducing atmosphere, and then the particles coarsen slowly upon continued annealing. After introduction of the carbon source, the initial CNT diameter distribution closely matches that of the catalyst particles. However, significant changes in CNT diameter can occur quickly during the subsequent CNT self-organization process. Correlation of time-resolved orientation data to X-ray scattering intensity and height kinetics suggests that the rate of self-organization is driven by both the CNT growth rate and density, and vertical CNT growth begins abruptly when CNT alignment reaches a critical threshold. The dynamics of CNT size evolution and self-organization vary according to the catalyst annealing conditions and substrate temperature. Knowledge of these intrinsically rapid processes is vital to improve control of CNT structure and to enable efficient manufacturing of high-density arrays of long, straight CNTs.

    Copyright © 2012 American Chemical Society

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    Supporting Information

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    Mathematical model for SAXS of CNTs, mass spectrometry data, AFM images of annealed catalyst films, SEM of CNTs, additional data and fitting parameters for in situ experiments, as well as videos of real-time X-ray images during catalyst annealing, CNT nucleation, and CNT self-organization. This material is available free of charge via the Internet at http://pubs.acs.org.

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    Cited By

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    ACS Nano

    Cite this: ACS Nano 2012, 6, 6, 5091–5101
    Click to copy citationCitation copied!
    https://doi.org/10.1021/nn300758f
    Published May 9, 2012
    Copyright © 2012 American Chemical Society

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