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Nanocomposite coatings via simultaneous organic–inorganic photo‐induced polymerization: synthesis,structural investigation and mechanical characterization
Authors:Cindy Belon  Abraham Chemtob  Céline Croutxé‐Barghorn  Séverinne Rigolet  Marjorie Schmitt  Sophie Bistac  Vincent Le Houérou  Christian Gauthier
Affiliation:1. Département de Photochimie Générale, CNRS, ENSCMu, University of Haute‐Alsace, 3 rue Alfred Werner, 68093 Mulhouse Cedex, France;2. Institut de Sciences des Matériaux de Mulhouse, CNRS, LRC 7228, University of Haute‐Alsace, 3 rue Alfred Werner, 68093 Mulhouse Cedex, France;3. Laboratoire de Chimie Organique Bioorganique et Macromoléculaire, CNRS, ENSCMu, University of Haute‐Alsace, 3 rue Alfred Werner, 68093 Mulhouse Cedex, France;4. Institut Charles Sadron, CNRS, UPR 22, University of Strasbourg, 23 Rue du Loess, BP 84047, 67034 Strasbourg Cedex 2, France
Abstract:Hybrid sol–gel films were prepared via a simultaneous organic‐inorganic UV‐curing process using a diaryliodonium salt as a superacid photogenerator. In this single‐step procedure, an epoxy functionalized reactive resin mixed with a variable amount of either of two epoxy trialkoxysilane precursors was UV‐irradiated, causing both the initiation of epoxy ring‐opening copolymerization and the catalysis of trialkoxysilyl sol–gel reactions. The concomitant photo‐induced sol–gel process was found to have a significant effect on the two related propagation mechanisms in competition for the oxirane ring‐opening—the active chain‐end and the activated monomer mechanisms—as proved by a systematic examination of the hybrid material microstructure through 29Si and 13C solid‐state NMR spectroscopy. The effect of the oxo‐silica network generation on the epoxy reaction kinetics was also evaluated using real‐time Fourier transform infrared spectroscopy upon varying the epoxysilane structure and its concentration. Thermal and dynamic mechanical analyses were systematically performed on these hybrids, by studying thoroughly their structure–property interdependence. Other mechanical characterizations through tribological and scratch tests suggested that the present photopolymer–silica hybrid material provides a powerful tool to tailor mechanical property profiles. Copyright © 2010 Society of Chemical Industry
Keywords:sol–  gel  cationic photopolymerization  hybrid  solid‐state NMR
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