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    Rapid Selective Etching of PMMA Residues from Transferred Graphene by Carbon Dioxide
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    † Department of Materials Science and Engineering, The University of Texas at Dallas, Richardson, Texas 75080, United States
    ‡ Department of Mechanical Engineering and the Materials Science and Engineering Program, The University of Texas at Austin, Austin, Texas 78712, United States
    § Texas Instruments Incorporated, Dallas, Texas 75243, United States
    *E-mail: [email protected]. Phone: +1 (972)-883-5751. Fax: +1 (972)-883-5725.
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    The Journal of Physical Chemistry C

    Cite this: J. Phys. Chem. C 2013, 117, 44, 23000–23008
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    https://doi.org/10.1021/jp408429v
    Published October 10, 2013
    Copyright © 2013 American Chemical Society
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    Abstract

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    During chemical-vapor-deposited graphene transfer onto target substrates, a polymer film coating is necessary to provide a mechanical support. However, the remaining polymer residues after organic solvent rinsing cannot be effectively removed by the empirical thermal annealing in vacuum or forming gas. Little progress has been achieved in the past years, for little is known about the chemical evolution of the polymer macromolecules and their interaction with the environment. Through in situ Raman and infrared spectroscopy studies of PMMA transferred graphene annealed in nitrogen, two main processes are uncovered involving the polymer dehydrogenation below 200 °C and a subsequent depolymerization above 200 °C. Polymeric carbons over the monolayer graphitic carbon are found to constitute a fundamental bottleneck for a thorough etching of PMMA residues. The dehydrogenated polymeric chains consist of active C═C bonding sites that are readily attacked by oxidative gases. The combination of Raman spectroscopy, X-ray photoemission spectroscopy, and transmission electron microscopy reveals the largely improved carbon removal by annealing in oxidative atmospheres. CO2 outperforms other oxidative gases (e.g., NO2, O2) because of its moderate oxidative strength to remove polymeric carbons efficiently at 500 °C in a few minutes while preserving the underlying graphene lattice. The strategy and mechanism described here open the way for a significantly improved oxidative cleaning of transferred graphene sheets, which may require optimization tailored to specific applications.

    Copyright © 2013 American Chemical Society

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    Supporting Information

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    The SEM image of suspended graphene on prepatterned holes, the reference hole for TEM imaging, and Raman spectra of the sample prepared by a slightly modified condition for confirming the existence and the same origin of the two new Raman peaks. This material is available free of charge via the Internet at http://pubs.acs.org.

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    Cite this: J. Phys. Chem. C 2013, 117, 44, 23000–23008
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    https://doi.org/10.1021/jp408429v
    Published October 10, 2013
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