Preparation and characterization of acrylic polymer titania hybrid. A study of organicinorganic interactions in hybrid m
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Preparation and characterization of acrylic polymer titania hybrid. A study of organicinorganic interactions in hybrid materials by micro-hardness Vickers
Van Nhan Nguyen, François Xavier Perrin and Jean-Louis Vernet Laboratoire de Chimie Appliquée-ISITV, Université de Toulon et du Var, BP 132, 83957 La Garde Cedex - FRANCE ABSTRACT Metal-oxide ceramer films have been developed using an acrylic polymer bearing a low amount of methacrylic acid units (ca. 4%mol) as the organic phase with titanium tetrabutoxide as the inorganic sol-gel precursor. The characterisation of free films was realized by various experimental methods. The formation of COOTi bonds prevents large scale phase separation between the organic component and the mineral network. Mechanical properties of the hybrid films have been investigated through dynamic mechanical analysis. The influence of the titania content on the damping peak amplitude suggests that titania is molecularly dispersed in the polymer matrix and that it significantly hinders the segmental motion of the polymer chains. However, the low content in potential carboxylic crosslinking sites explains why the glass transition temperature remains relatively unchanged when titania content increases. Vickers microhardness measurements used in this study allowed us to understand the contribution of the inorganic part (phase TiO2) to the mechanical properties of the polymer. The creep of hybrids has been studied carrying out hardness measurements under various indentation times. The mineral constituent leads to an important increase of the hardness and limits, in a significant way, the creep of polymer. INTRODUCTION In the last decade, an increasing attention has been devoted to the preparation of organic/inorganic hybrid materials [1-3]. Most of these materials are nanoscopic, hence inferring new and peculiar properties when compared to the traditional macroscale composites. So far, the preparation of hybrid materials from acrylic polymers either utilises organic polymers functionalized with trialkoxysilane moieties [4] or hydroxyl groups [5] or simply involves hydrogen bondings between the silanol of the inorganic network and the carbonyl groups on the unfunctionnalized acrylic polymer [6]. Here, we use the first approach considering the potential reactivity of carboxylic acid groups with metal alkoxides [7]. The coordinative bondings between the polymer and titania is demonstrated. Mechanical properties of hybrids are also discussed through dynamic mechanical analysis and hardness measurements.
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EXPERIMENTAL The acrylic terpolymer is a poly(methyl methacrylate-co-n-butyl methacrylate-co-methacrylic acid) obtained from ICI, with a 0.16, 0.80 and 0.04 in molar faction per monomer unit, respectively. The molecular mass of terpolymer is 120.000
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