The ZnS particles were immobilized on the surface of poly(vinylidene difluoride) (PVDF) mixing methacrylic acid (MAA)-trifluoroethyl acrylate (TFA) copolymer electrospun nanofibers. The PVDF and MAATFA copolymer nanofibers were prepared by electrospinning. Zinc ions were introduced onto the surface of nanofibers by coordinating with the carboxyls of MAA, and then sulfide ions were added to react with zinc ions to form ZnS particles under hydrothermal condition. The size and the amount of ZnS particles increased with the reaction time prolonging. The Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) results reveal that a chemical interaction exists between ZnS and fluoropolymer fibers. The degradation rate of methylene blue in ZnS-fluoropolymer nanocomposite system was considerably higher than in that of ZnS powders system under UV irradiation. There may be an ad sorption-migration-photodegradation process during the degradation of methylene blue by using ZnS-fluoropolymer nanocomposites as photocatalyst. The photocatalytic activity of ZnS-fluoropolymer nanocomposites changes indistinctively after 10 times repeating tests. (C) 2009 Elsevier Ltd. All rights reserved.