NiO nanosheets are synthesized in situ on gas sensor chips using a facile solvothermal method. These NiO nanosheets are then used as gas sensors to analyze allyl mercaptan (AM) gas, an exhaled biomarker of psychological stress. Additionally, MnO 2 nanosheets are synthesized onto the surfaces of the NiO nanosheets to enhance the gas-sensing performance. The gas-sensing response of the NiO nanosheet sensor is higher than that of the MnO 2 @NiO nanosheet sensor. The response value can reach 56.69, when the NiO nanosheet sensor detects 40 ppm AM gas. Interestingly, a faster response time (115 s) is obtained when the MnO 2 @NiO nanosheet sensor is exposed to 40 ppm of AM gas. Moreover, the selectivity toward AM gas is about 17-37 times greater than those toward confounders. The mechanism of gas sensing and the factors contributing to the enhance gas response of the NiO and MnO 2 @NiO nanosheets are discussed. The products of AM gas oxidized by the gas sensor are identified by gas chromatography-mass spectrometry (GC/MS). AM gas detection is an unprecedented application for semiconductor metal oxides. From a broader perspective, the developed sensors represent a new platform for the identification and monitoring of gases released by humans under psychological stress, which is increasing in modern life.