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Effect of Backbone Chemistry on the Structure of Polyurea Films Deposited by Molecular Layer Deposition

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    Effect of Backbone Chemistry on the Structure of Polyurea Films Deposited by Molecular Layer Deposition
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    † †Department of Chemical Engineering, ‡Department of Chemistry, #Department of Materials Science and Engineering, Stanford University, Stanford, California 94305, United States
    ∥ SLAC National Accelerator Laboratory, Menlo Park, California 94025, United States
    *E-mail: [email protected]
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    Chemistry of Materials

    Cite this: Chem. Mater. 2017, 29, 3, 1192–1203
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    https://doi.org/10.1021/acs.chemmater.6b04530
    Published January 1, 2017
    Copyright © 2017 American Chemical Society
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    Abstract

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    An experimental investigation into the growth of polyurea films by molecular layer deposition was performed by examining trends in the growth rate, crystallinity, and orientation of chains as a function of backbone flexibility. Growth curves obtained for films containing backbones of aliphatic and phenyl groups indicate that an increase in backbone flexibility leads to a reduction in growth rate from 4 to 1 Å/cycle. Crystallinity measurements collected using grazing incidence X-ray diffraction and Fourier transform infrared spectroscopy suggest that some chains form paracrystalline, out-of-plane stacks of polymer segments with packing distances ranging from 4.4 to 3.7 Å depending on the monomer size. Diffraction intensity is largely a function of the homogeneity of the backbone. Near-edge X-ray absorption fine structure measurements for thin and thick samples show an average chain orientation of ∼25° relative to the substrate across all samples, suggesting that changes in growth rate are not caused by differences in chain angle but instead may be caused by differences in the frequency of chain terminations. These results suggest a model of molecular layer deposition-based chain growth in which films consist of a mixture of upward growing chains and horizontally aligned layers of paracrystalline polymer segments.

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    Supporting Information

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    The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.chemmater.6b04530.

    • MLD deposition conditions, NEXAFS measurement and correction details, AFM and XRR measurements used to verify film thicknesses, complete NEXAFS spectra for all chemistries at the carbon and nitrogen K-edges, graphitic carbon calibration standard, example NEXAFS fit, and peak fit parameters for all NEXAFS spectra (PDF)

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    This article is cited by 61 publications.

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    Cite this: Chem. Mater. 2017, 29, 3, 1192–1203
    Click to copy citationCitation copied!
    https://doi.org/10.1021/acs.chemmater.6b04530
    Published January 1, 2017
    Copyright © 2017 American Chemical Society
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