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Synthesis, formulation, and characterization of siloxane–polyurethane coatings for underwater marine applications using combinatorial high-throughput experimentation

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Abstract

Crosslinked siloxane–polyurethane coatings were designed, synthesized, formulated, applied, and characterized using combinatorial high-throughput experimentation and eight coatings were selected as candidates for further characterization. First, 72 novel hydroxyalkyl carbamate and dihydroxyalkyl carbamate-terminated poly(dimethylsiloxane) (PDMS) oligomers and their carbamate-linked block copolymers with poly(ε-caprolactone) (PCL) were synthesized using a high-throughput synthesis system. These PDMS oligomers and block copolymers were characterized for their molecular weight using high-throughput Gel Permeation Chromatography (Rapid-GPC). The 72 oligomers were then incorporated into siloxane–polyurethane formulations at four different levels resulting in 288 coatings. After initial screening of these 288 coatings, eight coatings were selected for further characterization. Differential scanning calorimetry, dynamic mechanical analysis, X-ray photoelectron spectroscopy and surface energy analysis demonstrate the presence of PDMS on the surface with a polyurethane underlayer. Pseudo-barnacle adhesion and the attachment strength of reattached live barnacles (Balanus amphitrite) were in good agreement. Out of the eight coatings that were down-selected, two coatings performed well in algal (Ulva), bacterial (Cytophaga lytica, Halomonas pacifica), and barnacle (Balanus amphitrite) laboratory screening assays and are potential candidates for ocean testing.

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Acknowledgments

The authors would like to thank David A. Christianson for his assistance with the use of combinatorial high-throughput instruments and the Office of Naval Research for supporting this research under Grants N00014-04-1-0597 and N00014-05-1-0822. We also thank John H. Thomas, III, from the University of Minnesota IT Characterization Facility for his assistance with XPS measurements and analysis.

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Authors and Affiliations

  1. Department of Coatings and Polymeric Materials, North Dakota State University, Fargo, ND, 58105, USA

    Abdullah Ekin & Dean C. Webster

  2. Center for Nanoscale Science and Engineering, North Dakota State University, Fargo, ND, 58102, USA

    Justin W. Daniels & Shane J. Stafslien

  3. School of Biosciences, The University of Birmingham, Birmingham, B15 2TT, UK

    Franck Cassé, James A. Callow & Maureen E. Callow

Authors
  1. Abdullah Ekin
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  2. Dean C. Webster
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  3. Justin W. Daniels
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  4. Shane J. Stafslien
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  5. Franck Cassé
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  6. James A. Callow
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  7. Maureen E. Callow
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Corresponding author

Correspondence to Dean C. Webster.

Additional information

This paper was awarded Second Place in the 2006 Roon Awards competition, held as part of the FutureCoat! conference, sponsored by the Federation of Societies for Coatings Technology, in New Orleans, LA, on November 1-3, 2006.

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Ekin, A., Webster, D.C., Daniels, J.W. et al. Synthesis, formulation, and characterization of siloxane–polyurethane coatings for underwater marine applications using combinatorial high-throughput experimentation. J Coat Technol Res 4, 435–451 (2007). https://doi.org/10.1007/s11998-007-9039-7

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