Bi 2 MoO 6 nanosheets were synthesized by a hydrothermal method. Morphology and structure of the Bi 2 MoO 6 nanosheets were analyzed by SEM, XRD, N 2 adsorption techniques and XPS. Gassensing properties of the as-prepared Bi 2 MoO 6 sensors were also systematically investigated. The results showed the reaction temperature greatly affected the morphology and structure of as-prepared Bi 2 MoO 6 nanosheets. When the reaction temperature reached 170 ºC, the morphology of the Bi 2 MoO 6 nanosheets tended to regular, and pure Bi 2 MoO 6 nanosheets were obtained. The operating temperature determined the gas-sensing properties of the Bi 2 MoO 6 sensor. At this optimal operating temperature of 300 ºC, the sensitivity of the Bi 2 MoO 6 sensor towards 20 ppm nitrogen oxide (NO) reached a maximum of 3.13. With the increase of the nitrogen oxide (NO) concentration, the sensitivity of the Bi 2 MoO 6 sensor also rapidly increased, and displayed an almost linear relationship between them. Additionally, the Bi 2 MoO 6 sensor demonstrated excellent selectivity with respect to several typical interfering gases.