In the recent years, fuel cells have been considered as In the present research, firstly poly(vinyl alcohol)/titanium oxide (PVA/TiO2) nanofibers were produced from appropriate dispersions of titanium oxide nanoparticles (with different weight percentages) in PVA aqueous solutions by electrospinning technique. Morphological studies of PVA/TiO2 nanofibers performed with optical microscopy and scanning electron microscopy and proved uniform bead-free structure for nanofibers containing TiO2 nanoparticles. The average fiber diameter increased whith increasing the content of TiO2 nanoparticles as a result of nearly constant solution conductivity and increased solution viscosity. In the next stage glutaraldehyde (GA) was used as a crosslinking agent in order to improve chemical, dimensional and thermal stabilities of electrospun nanofiber membranes to make them suitable for solid polymer electrolytes in alkaline direct ethanol fuel cells (ADEFCs). As a result of increasing GA solution concentration and crosslinking reaction time, the degree of swelling, weight loss and dimensional changes in water decreased, due to increase in the degree of crosslink for all samples. The crosslinked membranes characterized in connection with their anionic conductivities in alkaline solutions with different concentrations at 25? by means of electrochemical impedance spectroscopy method. The results showed an increasing trend in anionic conductivity of membranes in the presence of more TiO2 and a diminishing trend with increasing the GA concentration or crosslinking reaction time in each media. Furthermore the anionic conductivity of each electrospun nanofiber membrane in alkaline solutions increased with increasing the concentration of alkaline solutions. According to the X-ray diffraction (XRD) studies the percentage of amorphous regions increased in PVA electrospun membrane with incorporation of the TiO2 nanoparticles. Also XRD patterns showed nearly constant percentage of amorphous regions in higher concentrations of GA solutions and longer crosslinking reaction times. Thermogravimetric analysis showed the improved thermal stability due to the effect of TiO2 nanoparticles and the chemical crosslinking reaction between GA and PVA. Fourier Transform Infrared Spectroscopy was used to characterize the presence of specific chemical groups in the utilized materials. This study indicates that these membranes have suitable ionic conductivities, chemical, dimensional and thermal stabilities suggesting that they can be used as alkaline anion exchange membranes in direct alcohol fuel cells applications.