This paper focuses on the preparation of ZnIn(2)S(4)/fluoropolymer fiber composites and their performance for H(2) evolution from splitting of water using Xe lamp irradiation. Hexafluorobutyl acrylate-co-methacrylic acid (poly(HFBA-co-MAA)) is synthesized by a solution polymerization. Next, the fluoropolymer fibers, which have around 100 nm in average diameter, of poly(HFBA-co-MAA) and polyvinylidene fluoride (PVDF) mixtures are obtained by electrospinning. Then, zinc and indium ions are introduced onto the fiber surface by coordinating with carboxyls of MAA. After that, sulfide ions are incorporated to react with zinc and indium ions by a hydrothermal synthesis. Thus, ZnIn(2)S(4) particles of around 800 nm in average size, are obtained and well loaded on the fiber surface. The absorption edge of ZnIn(2)S(4)/fluoropolymer fiber composites is at 510 nm within the visible-light region. Photocatalytic H(2) evolution from water was investigated using Xe lamp. It was found that the average rate of H(2) evolution of ZnIn(2)S(4) powders gradually decreased, while the average rate of H(2) evolution of ZnIn(2)S(4)/fluoropolymer fiber composites increased from the first to the third run. The average rate of H(2) evolution using the ZnIn(2)S(4)/fluoropolymer fiber composites as the catalyst achieved 9.1 mL/h in the third run. (C) 2010 Professor T. Nejat Veziroglu. Published by Elsevier Ltd. All rights reserved.