In this paper, MoO 3 /MoSe 2 n-n heterostructure was constructed for fabricating trimethylamine (TMA) gas sensor by an improved hydrothermal and spin-coating method. The surface morphology and microstructure of the prepared materials were analyzed by XRD, XPS, SEM and TEM characterization methods. The microstructural characterization results demonstrated that the MoO 3 /MoSe 2 heterostructure had been successfully synthesized, in which the MoSe 2 had a ower-shaped structure, and MoO 3 had a rod-shaped structure. At the same time, the MoSe 2 surface exhibited periodic honeycomb structure. The gas-sensitivity experimental results showed that the proposed MoO 3 /MoSe 2 sensor had excellent TMA sensing performance at room temperature, including high response capability, low detection limit (20 ppb), short response/recovery time (12 s/19 s), long-term stability, good repeatability and outstanding selectivity. The heterostructure of MoO 3 /MoSe 2 had made outstanding contributions to the enhanced TMA gas sensing performance at room temperature.