Abstract: The preparation of rod-shaped Pd/FeVO4 powder and its gas sensitivity performance investigation experiment is a new experimental course. The rod-shaped Pd/FeVO4 powder was prepared by low temperature hydrothermal-chemical reduction method. The crystal structure, morphology and elemental composition of the samples were characterized. The gas sensing properties of benzyl alcohol gas were also studied. The experimental results show that the gas sensitivity of Pd nanoparticles modified FeVO4 powder has been significantly improved. Practice shows that the experiment covers a wide range of knowledge, comprehensive basic experimental skills such as low temperature chemical preparation, structural characterization and physical properties testing and research of semiconductor materials. It is conducive to cultivating students’ ability to comprehensively apply knowledge and conduct scientific research. It can be used as an exploratory experiment for the innovation class of Physics College of our university.