Modification and Characterization of Si-Based Nanobuilding Blocks Precursors for Hybrid Materials
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Modification and Characterization of Si-Based Nanobuilding Blocks Precursors for Hybrid Materials Fayna Mammeri 1, Najiba Douja 1, Christian Bonhomme 2, François Ribot 2, Florence Babonneau 2 and Sandra Dirè 1 1 Dipartimento di Ingegneria dei Materiali e Tecnologie Industriali, Università di Trento, Via Mesiano 77, 38050 Trento, Italy 2 Laboratoire de Chimie de la Matière Condensée, UMR-CNRS 7574, Université Pierre et Marie Curie, 4 place Jussieu, 75252 Paris Cedex 05, France ABSTRACT New functional nanobuilding blocks have been successfully synthesized by hydrosilylation of unsaturated alcohols with dimethylsiloxy isobutyl-POSS and further acylation with methacryloylchloride. The solvent influence on the reaction pathway has been studied, and reaction steps and final nano-objects have been characterized using multinuclear NMR and FTIR spectroscopy. The organic spacer chain length between the inorganic cage and the reactive methacrylate function has been changed in order to modify the reactivity of the final functional nanobuilding block in the polymerization process. INTRODUCTION The use of NanoBuilding Blocks (NBBs) to obtain organic-inorganic (O-I) hybrid structures has been developed with various systems such as silsesquioxanes, transition metal-oxo-clusters, organotin-oxo-clusters or functionalized nanosized metal oxide particles [1-4]. NBBs are highly precondensed structures and consequently present a lower reactivity towards hydrolysis or nucleophilic attacks than molecular precursors. Additionally, they are monodispersed and nanometric in size, with perfectly defined structures. They can be capped with polymerizable ligands to allow the preparation of hybrid materials and will keep their initial structure in the final material [1-4]. An emerging class of NBBs is based on Polyhedral Oligomeric SilSesquioxanes (POSS), which have been studied for different applications such as fire-resistant materials or dental restorative materials [5-7]. In order to prepare new functional NBBs, an easy synthetic approach is to start from commercial POSS, which are available with different reactive groups. They can be reacted with organic spacers, and further modified with polymerizable functions. Platinum-catalyzed hydrosilylation is an efficient method to produce new silicon-carbon bonds by the addition of C=C to Si-H bonds. However, when unsaturated alcohols are used as organic spacers, a competitive reaction between Si-H and OH groups can take place [5]. Thus the experimental conditions to enhance the hydrosilylation pathway should be optimized. In this work, we have investigated the hydrosilylation reaction of allylalcohol [CH2=CH-CH2-OH] and 4-penten-1-ol [CH2=CH-(CH2)3-OH] with the -(CH3)2Si-H reactive groups belonging to dimethylsiloxy
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isobutyl-POSS (DMIPOSS). The main aim of this study was to achieve a full hydrosilylation reaction in order to keep the OH functions, which will be further reacted with methacryloylchloride [Cl-COC(CH3)=CH2]. The influence of the organic spacer chain length (CH2=C
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