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The efficient detection of n-butanol, which is in demand for highly sensitive materials, is essential for multiple applications. A nonaqueous method was applied to prepare NiFe₂O₄ nanoparticles (NPs) using benzyl alcohol as a solvent, which shows a size of 7.9 ± 1.6 nm and a large surface area of 82.23 m²/g. To further improve the sensing performance for n-butanol, Pd/PdO functionalization was sensitized with NiFe₂O₄ NPs. Gas sensing results demonstrate that the Pd/PdO-NiFe₂O₄ exhibits an enhanced response of 36.9 to 300 ppm n-butanol and a fast response and recovery time (18.2/17.6 s) at 260 °C. Furthermore, the Pd/PdO-NiFe₂O₄-based sensor possesses a good linear relationship between responses and the n-butanol concentration from 1 to 1000 ppm, and great selectivity against other volatile organic compounds (VOCs). The excellent sensing enhancement is attributed to the catalytic effects of Pd/PdO, the increase of oxygen vacancies, and the formation of heterojunction between PdO and NiFe₂O₄. Thus, this study offers an effective route for the synthesis of Pd/PdO-functionalized NiFe₂O₄ NPs to achieve n-butanol detection with excellent sensing performance.