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Conversion of poly (ethylene-alt-tetrafluoroethylene) copolymers into polytetrafluoroethylene by direct fluorination: A convenient approach to access new properties at the ETFE surface

Year: 2011

Journal: Journal of polymer science part A: Polymer chemistry 2011, 49 (7) pp 1517-1527, 20121211

Authors: Gérard Calleja, Axel Houdayer, Sylvie Etienne-calas, David Bourgogne, Valérie Flaud, Gilles Silly, Sota Shibahara, Atsushi Takahara, Alex Jourdan, André Hamwi, Bruno Ameduri

Organizations: Ingénierie et Architectures Macromoléculaires, Institut Charles Gerhardt-UMR(CNRS) 5253, Ecole Nat Sup de Chimie de Montpellier, 8 Rue de l'Ecole Normale, F-34296 Montpellier Cedex, France; Laboratoire des Matériaux Inorganiques, UMR(CNRS) 6002, Université Blaise Pascal, 24 avenue des Landais, 63177 AUBIERE Cedex, France; Matériaux Hybrides et Nanostructures, Groupe d'Etude des Semiconducteurs-UMR(CNRS) 5650, Université Montpellier 2, place E. Bataillon 34095 Montpellier Cedex 5, France; Institut Charles Gerhardt-UMR(CNRS) 5253, Université Montpellier 2, place E. Bataillon 34095 Montpellier Cedex 5, France; Institute for Materials Chemistry and Engineering, Kyushu University, Nishi-ku, Fukuoka 819-0395, Japan; AREVA NC-BUC/DRD, BP 44-26701 Pierrelatte Cedex, France

Direct fluorination of poly(ethylene-alt-tetrafluoroethylene) copolymer (ETFE) was carried out on commercially available ETFE films with pure fluorine gas at ambient atmosphere. Reaction temperature was either 95 °C or 150 °C and exposure time was 20 hours. Analysis of the fluorinated samples was performed by attenuated total reflection Fourier transform Infrared, confocal micro-Raman and 1H and 19F magic angle spinning nuclear magnetic resonance spectroscopies, scanning electron microscopy, electron diffraction and X-Ray photoelectron spectroscopies, contact angle determination, atomic force microscopy and nanoindentation measurements, and compared to those of the virgin ETFE copolymer. Integrity of the bulk materials was verified by investigating the thermal behavior of the polymers by thermogravimetric analysis and differential scanning calorimetry. Evidence for the formation of a homogeneous layer of polytetrafluoroethylene with a thickness of several microns at the surface of the copolymers with no degradation of the materials was observed.