Diameter-controlled tin oxide nanofibers have been successfully prepared using electrospinning and a subsequent calcination process; their diameters, morphologies, and crystal structures have been characterized. The diameters of the as-spun nanofibers can be decreased by lowering the concentration of a polymer and a tin precursor in the electrospinning solution because of the decrease in the solution viscosity. The crystal structure of the nanofibers calcined at various temperatures from 200˚C to 800˚C has been proved to be the tetragonal rutile of tin oxide; crystallinity is improved by increasing the temperature. However, nanofibers with lower concentrations of tin precursor do not maintain their fibrous structures after calcination at high temperatures. In this study, the effect of the relationship between the precursor concentration and the calcination temperature on the diameter and the morphology of the tin oxide nanofiber has been systematically investigated and discussed.