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Herein, a facile fabrication process of ZnO-ZnFe₂O₄ hollow nanofibers through one-needle syringe electrospinning and the following calcination process is presented. The various compositions of the ZnO-ZnFe₂O₄ nanofibers are simply created by controlling the metal precursor ratios of Zn and Fe. Moreover, the different diffusion rates of the metal oxides and metal precursors generate a hollow nanostructure during calcination. The hollow structure of the ZnO-ZnFe₂O₄ enables an enlarged surface area and increased gas sensing sites. In addition, the interface of ZnO and ZnFe₂O₄ forms a p-n junction to improve gas response and to lower operation temperature. The optimized ZnO-ZnFe₂O₄ has shown good H₂S gas sensing properties of 84.5 (S = R_a/R_g) at 10 ppm at 250 °C with excellent selectivity. This study shows the good potential of p-n junction ZnO-ZnFe₂O₄ on H₂S detection and affords a promising sensor design for a high-performance gas sensor.