Titanium dioxide-cadmium oxide (TiO2/CdO) nanofibers were prepared by the electrospinning technique followed by a single-step calcination from a solution of titanium isopropoxide and cadmium acetate dihydrate. Scanning electron microscopy, transmission electron microscopy, and the Brunauer-Emmett-Teller technique were employed to characterize the as-spun nanofibers as well as the calcined product. The specific surface area of the calcined product was calculated to be 65.3067 m(2) g(-1). X-ray powder diffractometry analysis was conducted on the samples to study their chemical composition as well as their crystallographic structure. The results obtained indicated that the prepared nanostructure product can eliminate all of the methyl orange dye within about 75 min, whereas the pristine titanium dioxide nanofibers could not eliminate more than 50% even after 180 min.