Abstract. Vanadium pentoxide (V2O5) nanosheets are successfully synthesized by a hydrothermal method, followed by a high-temperature sintering treatment. Several advanced techniques are used to characterize the morphology and composition of the nanostructures, such as transmission electron microscope (TEM), high-resolution TEM (HRTEM), scanning electron microscope (SEM), and X-ray diffraction (XRD). The HRTEM image and selected area electron diffraction (SAED) indicate the crystalline grows along [010] direction. The gas sensing performance of the V2O5 nanosheets was evaluated toward several volatile organic compounds (VOCs), such as ethanol, acetone, pyridine, and formaldehyde. The results show that the nanosheets exhibits superior sensing response and selectivity toward acetone to that of commercial V2O5 particles at optimum working temperature of ~300°C. this work will help explore vanadium oxides as sensing materials towards VOCs with high performance.