Novel ZnSe/NiO heterostructure nanocompos-ites were successfully prepared by one-step hydrothermal method.The ZnSe/NiO-based sensor exhibits a response of ~ 96.47% to 8 × 10-6 NO2 at 140 ℃,which is sig-nificantly higher than those of intrinsic ZnSe-based (no response) and NiO-based (~ 19.65%) sensors.The theo-retical detection limit (LOD) of the sensor is calculated to be 8.91 × 10-9,indicating that the sensor can be applied to detect the ultralow concentrations of NO2.The effect of NiO content on the gas-sensing performance of the nanocomposites was investigated in detail.The optimal NiO content in the nanocomposite is determined to be 15.16% to achieve the highest response.The as-fabricated sensor also presents an excellent selectivity to several possible interferents such as methanol,ethanol,acetone,benzene,ammonia and formaldehyde.The enhanced sensing performance can be attributed to the formation of p-p heterostructures between ZnSe and NiO,which indu-ces the charge transfer across the interfaces and yields more active sites.