In this study, nanofibers of poly (acrylic acid) (PAAc), polyacrylamide (PAAm) and poly (vinyl alcohol) (PVOH) were prepared using the electrospinning technique. Based on the Taguchi DOE (design of experiment) method, the effects of electrospinning parameters, i.e., needle tip to collector distance, polymer solution concentration, applied voltage, polymer solution feed rate and polymer type, on the diameter and morphology of polymer nanofibers were evaluated. Analyses of the experiments for the diameters of the polymer nanofibers showed that the type of polymer was the most significant factor. The optimal combination to obtain the smallest diameters with minimum deviations for electrospun polymer nanofibers was also determined. For this purpose, the appropriate factor levels were determined as follows: polymer PAAm, applied voltage 10 kV, delivery rate 0.1 mL/h, needle tip to collector distance 10 cm, and polymer solution concentration 8%, to obtain the thinnest nanofibers. This combination was further validated by conducting a confirmation experiment, and the average diameter of the polymer nanofibers was found to be close to the optimal conditions estimated by the Taguchi DOE method.