The aim of this study was to prepare poly(styrene sulfonic acid-co-maleic acid) (PSSA-MA)/polyvinyl alcohol (PVA) ion-exchange fibers using the electrospinning technique and a post-thermal treatment. First, intermediate PSSA-MA/PVA fibers were prepared from solutions of PSSA-MA/PVA combined at ratios of 0.2/1 to 1/1; the fibers were subsequently crosslinked at 80-150 A degrees C for 0.25-7 h. The effect of the crosslinking time, the temperature and the PSSA-MA/PVA ratio on various properties of the obtained ion-exchange fibers was investigated. When the PSSA-MA/PVA ratios were greater than 0.4/1, bead formation was observed. Thus, only smooth fibers without beads prepared from PSSA-MA/PVA mixed in ratios up to 0.4/1 were subjected to the thermal crosslinking treatment. When the crosslinking time and temperature were increased, the degree of crosslinking increased, which caused a decrease in the water solubilization and water uptake and an increase in the Young's modulus. These parameters also appeared to significantly affect the ion-exchange capacity value. The temperature and time for successful crosslinking were 120-140 A degrees C and 1-7 h, respectively.