Hybrid organic/inorganic membranes that include a functionalized (‐SO3H), interconnected silica network, a non‐porogenic organic matrix, and a ‐SO3H‐functionalized terpolymer are synthesized through a sol–gel‐based strategy. The use of a novel crosslinkable poly(vinylidene fluoride‐ter‐perfluoro(4‐methyl‐3,6‐dioxaoct‐7‐ene sulfonyl fluoride)‐ter‐vinyltriethoxysilane) (poly(VDF‐ter‐PFSVE‐ter‐VTEOS)) terpolymer allows a multiple tuning of the different interfaces to produce original hybrid membranes with improved properties. The synthesized terpolymer and the composite membranes are characterized, and the proton conductivity of a hybrid membrane in the absence of the terpolymer is promising, since 8 mS cm−1 is reached at room temperature, immersed in water, with an experimental ion‐exchange‐capacity (IECexp) value of 0.4 meq g−1. Furthermore, when the composite membranes contain the interfaced terpolymer, they exhibit both a higher proton conductivity (43 mS cm−1 at 65 °C under 100% relative humidity) and better stability than the standard hybrid membrane, arising from the occurrence of a better interface between the inorganic silica and the poly[(vinylidene fluoride)‐co‐hexafluoropropylene] (poly(VDF‐co‐HFP)) copolymer network. Accordingly, the hybrid SiO2‐SO3H/terpolymer/poly(VDF‐co‐HFP) copolymer membrane has potential use as an electrolyte in a polymer‐electrolyte‐membrane fuel cell operating at intermediate temperatures.
The synthesis and characterization of an original class of linear poly(alkyl aryl) ethers containing 1,2,3-triazolyl and fluorinated moieties based on oligo(tetrafluoroethylene) telomer are presented. These polymers were prepared, from R,ω-dipropargyl ether bisphenol AF and 1,10-diazido-1H,1H,2H,2H,9H,9H, 10H,10H-perfluorodecane, in 62% overall yields via the azide/alkyne "click" reaction and/or oxidative coupling of acetylenes (Hay reaction). The latter reactant was produced from the ethylene end-capping of oligo-(tetrafluoroethylene) followed by a nucleophilic substitution with sodium azide. A simple tuning of the reaction conditions allowed us to direct the originally favored "click" reaction toward a competitive homocoupling of the terminal alkynes, thus leading to copolymers with drastically different structures, as evidenced by size exclusion chromatography, DSC, Raman, and UV-vis spectroscopy. Hence, original poly(alkyl aryl) ether copolymers with a high thermal stability (higher than 300 °C) that exhibit alternating statistic or block microstructures were obtained.
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