Electrospun nanofibrous scaffolds have great potential for many biomedical applications. In the present study, we fabricated and characterized chitosan/polyvinyl alcohol (Chi/PVA) nanofibrous scaffolds through electrospinning. Cross-linking was performed using chemically with 5 % glutaraldehyde vapor. The morphology and chemical banding of the electrospun nanofibers before and after cross-linking were evaluated using scanning electron microscopy (SEM) and Attenuated Total Reflectance Fourier Transform InfraRed (ATR-FTIR) spectroscopy. SEM micrographs and FTIR spectra showed that the cross-linking process was accomplished successfully. With the biocompatibility and non-toxicity of chitosan and PVA, it is expected that this electrospun nanofibrous scaffold could be an excellent candidate for biomedical applications.