The reaction of PVF<sub>2</sub> films in aqueous NaOH with the use of tetrabutylammonium hydrogen sulfate as phase transfer catalyst results in surface dehydrofluorination. Subsequent examination of the PVF<sub>2</sub> surface using ATR FT-IR affords evidence as to the structure of dehydrofluorinated PVF<sub>2</sub>. It is found that the infrared bands at 1402, 1225, 1194, and 882 cm<sup>−1</sup> are sensitive to the surface treatment. The origin and behavior of these bands are discussed. It is observed that upon dehydrofluorination the FT-IR spectra of the PVF<sub>2</sub> surface exhibit two infrared bands at 1613 cm<sup>−1</sup> and 1717 cm<sup>−1</sup> which arise from the formation of carbon-carbon double bonds. The band at 1613 cm<sup>−1</sup> is due to conjugated -(-CH=CF-)- units, whereas the 1717 cm<sup>−1</sup> band is assigned to the -(-CF=CF-)- units which arise from resonance at structural head-to-head and tail-to-tail defects.
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