Chitosan/poly(vinyl alcohol) (PVA) nanofibrous mats were prepared by the electrospinning method. The morphology and structure of electrospun nanofibers were investigated by scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR) spectroscopy. SEM images showed that the uniform and bead-free fibers were obtained at concentrations greater than 8 wt%. Chitosan/PVA mats were irradiated with different doses (50-200 kGy) of (60)Co gamma rays. The effect of irradiation dose on the mechanical and thermal properties of these films was also investigated. Increasing the irradiation dose led to a decrease in tensile strength. FT-IR and DSC demonstrated that there were strong intermolecular hydrogen bonds between the chitosan and PVA molecules. (C) 2009 The Korean Society of Industrial and Engineering Chemistry. Published by Elsevier B.V. All rights reserved.