This paper reports production of nanofibers with voltage value of 20 kV, different fluid velocities (0.1 ml/h, 0.5 ml/h), different durations (2 min, 5 min), and distance of 7 cm in the electrospin assembly. The morphology of the produced nanofibers was observed before and after heat treatment by scanning electron microscope. The crystal structure of the nanofibers was examined by X-ray diffraction. In addition, thermal analysis/thermal gravimetric analysis of nanofibers was performed. X-ray diffraction measurements showed that the samples were crystalline in barium titanate. It was observed that the diameters of the nanofibers increased when the flow rate and time increased, while the diameters of the nanofibers decreased when the flow rate and time decreased. Scanning electron microscope images showed how the morphology of the samples changed by heat treatment. As a result, characterization results were found to be consistent with the literature.