Electrospun ZnO nanofibers were obtained by calcinating PVA/Zinc Acetate composite fibers at various temperatures. Atomic Force Microscopy (AFM) revealed that the ZnO fibers have diameters in the range of 100-200 nm. The fibers were characterized by FT-IR, TGA-DTA, and XRD studies. The XRD results showed that the crystal structure and the morphology of the fibers were largely dependent on the calcination temperature.