Inorganic-organic hybrid membranes consisting of an aliphatic main-chain polymer and trisiloxane bond were synthesized using a simple, one-pot process from a trisiloxane derivative, phosphonic acid acrylate, and vinylbenzotriazole. 1,5-Divinyl-3-phenylpentamethyltrisiloxane (DPPMTS) was copolymerized with 2-hydroxyethyl methacrylate acid phosphate (HEMAP), and N-vinylbenzotriazole (VBT), yielding inorganic-organic hybrid composites. The formation of the inorganic-organic hybrid structure was confirmed by IR, 13C, and 29Si NMR spectroscopy. The membranes exhibited good thermal stabilities up to 200 °C. The aliphatic chains of the methacrylate derivative copolymerized with trisiloxane in the hybrid membranes improved the mechanical properties of the membranes. The tensile modulus of the VBT/HEMAP/DPPMTS membrane with a composition of 1:9:5 was 1.19 GPa. The conductivities of the 1:9:5 membranes were 5.3 × 10−2 S cm−1 and 4.1 × 10−4 S cm−1 at 100 and 19.3% relative humidity (RH), respectively, and 130 °C. The membrane electrode assembly (MEA) using the hybrid membrane exhibited a peak power of 7.8 mW cm−2 at 140 °C and 30% RH.
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