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CryoSEM: Revealing Microstructure Development in Drying Coatings

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Protective Coatings

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Abstract

This chapter provides a brief overview of cryogenic scanning electron microscopy (cryoSEM) and how it can be used to characterize wet coating microstructure and its development. As one of the few tools capable of studying wet coating microstructure, cryoSEM reveals transient states in the microstructure that develop as the coating dries. In this chapter, the basic concepts of cryoSEM sample preparation are reviewed including sample vitrification, cryo-fracture, and sublimation. Additionally, several possible artifacts of cryoSEM sample preparation are highlighted and the challenges of image interpretation are discussed. Lastly, several case studies are presented where cryoSEM was used to characterize the microstructure of wet coatings. The examples include: drying-induced gradients in particle concentration, understanding the origin of dry film microstructure from the microstructure of the initial dispersions, and understanding the fundamentals of drying-induced stress development in hard particle coatings.

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Acknowledgments

The authors would like to gratefully acknowledge support from the National Science Foundation under Award No. CBET 0967348, and the industrial supporters of the Coating Process Fundamentals Program (CPFP), part of the industrial partnership IPrime at the University of Minnesota. Parts of this work were carried out in the Characterization Facility, University of Minnesota, which receives partial support from NSF through the MRSEC program. Acknowledgments also go to Chris Frethem for all of his contributions to the work presented here. The authors are also grateful to the late Professors L. E. Scriven and H. T. Davis and the past graduate student researchers in CPFP for their pioneering work in developing cryoSEM techniques for coatings characterization.

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Authors and Affiliations

  1. Department of Chemical Engineering and Materials Science, University of Minnesota, Minneapolis, MN, USA

    Kyle Price, Alon V. McCormick & Lorraine F. Francis

  2. Axalta Coating Systems, Coatings Technology Center, Wilmington, DE, USA

    Kyle Price

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  1. Kyle Price
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  2. Alon V. McCormick
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Correspondence to Kyle Price .

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Editors and Affiliations

  1. Axalta Coating Systems, Coatings Technology Center, Wilmington, Delaware, USA

    Mei Wen

  2. Institute of Macromolecular Chemistry, Academy of Sciences of the Czech Republic, Prague, Czech Republic

    Karel Dušek

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Price, K., McCormick, A.V., Francis, L.F. (2017). CryoSEM: Revealing Microstructure Development in Drying Coatings. In: Wen, M., Dušek, K. (eds) Protective Coatings. Springer, Cham. https://doi.org/10.1007/978-3-319-51627-1_6

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