Triethylamine (TEA) poses severe safety hazards to industrial production and human health. To accurately detect TEA concentrations and rapidly warn of leakage, a simple reflux condensation method was deployed to successfully incorporate Zn2+ in situ into Mo-MOFs precursor in a green, safe, and time-efficient synthesis condition. Subsequently, through calcination, MoO3/ZnMoO4-X (MMZ-X) were prepared, which exhibited an increased number of defects and enriched porosity, facilitating the access and interaction of TEA with adsorption sites. Simultaneously, rationally built in situ MoO3/ZnMoO4 heterostructures accelerated carrier migration and induced a drastic resistive change. MMZ-2 demonstrated outstanding TEA sensing performance, exhibiting extremely high sensitivity (R = 572.3, 100 ppm), along with superior selectivity, repeatability and stability, rapid response and recovery times, and a low detection limit. Moreover, the key intrinsic parameters of the heterostructure on the atomic scale were determined by density functional theory (DFT) calculations, providing a detailed elucidation of the sensing enhancement mechanism of the MoO3/ZnMoO4 heterostructure. The simple and efficient synthesis method and the related mechanistic analysis pave a new path for designing high-performance TEA gas sensors with practical applications.
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