Europium-doped zirconium oxide (ZrO2:Eu3+) nanofibers were prepared via electrospinning, in which a mixture of zirconium chloride oxide octahydrate, europium nitrate hexahydrate, poly(vinyl pyrrolidone), dimethylformamide, and ethanol were electrospun at atmospheric conditions. Subsequent calcination to produce ZrO2:Eu3+ nanofibers with diameters around 300 nm. The crystal structure and photoluminescence of the ZrO2:Eu3+ nanofibers were studied as a function of dopant concentration and heating temperature. At a dopant concentration of 5 mol %, tetragonal phase crystals were observed. Photoluminescence spectra revealed several emission bands in the red region corresponding to the transition of 5D0 → 7FJ (J = 1; 2; 3; 4). Two most intense emission bands were observed at wavelengths of 606 and 591nm due to the forced electric dipole (5D0 → 7F2) and magnetic dipole (5D0 → 7F1) transitions, respectively. This work demonstrates that one-dimensional photoluminescent materials can be generated by a two step electrospinning and calcination process.