Nanofibers, which have high surface area to volume ratio and better mechanical properties, are nanomaterials that both industry and scientists have started to show great attention in the last two decades. They are used in many areas such as life and filtration sciences, sensors, and composite reinforcement etc. The purpose of this study is to electrospin polystyrene/butyl rubber blends and to investigate the effects of electrospinning parameters on the fibers produced. In this study, polystyrene/butyl rubber blends were electrospun by changing the applied voltage, the tip- to-collector distance, the flowrate, and the butyl rubber content in the fiber. Finally, morphology of electrospun fibers was characterized by SEM.