Ultrafine fibers were spun from polyacrylonitrile (PAN)/N,N-dimethyl formamide (DMF) Solution as a precursor of carbon nanofibers using a homemade electrospinning set-up. Fibers with diameter ranging from 200 nm to 1200 nm were obtained. Morphology of fibers and distribution of fiber diameter were investigated varying concentration and applied voltage by scanning electric microscopy (SEM). Average fiber diameter and distribution were determined from 100 measurements of the random fibers with an image analyzer (SemAfore 5.0, JEOL). A more systematic understanding of process parameters was obtained and a quantitative relationship between clectrospinning parameters and average fiber diameter was established by response surface methodology (RSM). It was concluded that concentration of solution played an important role to the diameter of fibers and standard deviation of fiber diameter. Applied voltage had no significant impact on fiber diameter and standard deviation of fiber diameter. (c) 2005 Elsevier Ltd. All rights reserved.