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ABSTRACT In this study, Nafion® NR 40 beads with polyethylene oxide (PEO) are fabricated into a nanofiber membrane using electrospinning. In particular, Nafion® beads in non-toxic mixed solvent (EtOH and H2O) were blended with the carrier polymer PEO, which is the minor component in the solution responsible for the solution spinnability. The highest content of Nafion® in the nanofiber is 98.04%. To investigate the factors influencing the nanofiber diameter during electrospinning, an orthogonal design method was adopted. These factors include the carrier polymer content, distance between the syringe needle and roller collector, flow rate of the electrospinning solution, and the roller rotation speed. After obtaining the significant factors and optimal test level, an additional optimization experiment is conducted under the best conditions. The resulting nanofibers have a diameter of ∼150 nm. Moreover, the obtained Nafion® nanofiber membrane has strong potential for applications in polymer electrolyte membrane fuel cells (PEMFC), the chlor-alkali industry, catalysts, and metal ion removal. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015, 132, 41755. [ABSTRACT FROM AUTHOR]