In this study, nanofiber mats consisting of two potential metal oxides were produced by electrospinning technique. An aqueous solution of zinc acetate dihydrate and germanium isopropoxide was mixed with polyvinyl alcohol solution to prepare a sol-gel that was electrospun at 20 kV. The obtained nanofiber mats were dried under a vacuum at 80 degrees C for 24 h and then calcined in air at different temperatures and soaking times. Physiochemical characterizations have affirmed that nanofibers composed of zinc oxide-germanium dioxide (ZnO-GeO2) can be prepared by calcination at different temperatures. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), and the Brunauer-Emmett-Teller (BET) technique were employed to characterize the as-spun nanofibers and the calcined product. The specific surface area of the calcined product decreased with increases in temperature. X-ray powder diffractometery (XRD) analysis was used to study the chemical composition and the crystallographic structure. The optical properties of the as-prepared ZnO-GeO2 nanofibers were also studied.