CdS-OH/polyacrylonitrile (PAN) hybrid nanofibers with strong photoluminescence and photocatalytic hydrogen production efficiency were synthesized by one-step co-electrospinning for the first time. The suspension of CdS-OH nanoparticles (size: 5 nm) in N,N-dimethylformamide (DMF) was mixed with PAN/DMF solutions to make spinning solutions, followed by electrospinning to make CdS-OH/PAN hybrid nanofibers. Their morphology and structure were characterized by SEM, TEM, XRD and fluorescence spectrophotometer. TEM and XRD measurements proved that the crystallographic structure of CdS-OH nanoparticles is identical to that of CdS. The CdS-OH nanoparticles were evenly distributed in PAN nanofibers of 320 nm in diameter. Thermogravimetrical analysis demonstrated that hybrid nanofibers were more thermally stable than neat PAN nanofibers. The hybrid nanofibers displayed excellent photoluminescent property. Additionally, they showed good photocatalytic hydrogen production efficiency with a rate of 13.5 mu mol/h g fiber containing 60 mg of CdS-OH nanoparticles. (c) 2012 Elsevier Ltd. All rights reserved.