Abstract Two-dimensional transition metal carbides/nitrides, known as MXenes, have been recently receiving attention for gas sensing. However, studies on hybridization of MXenes and 2D transition metal dichalcogenides as gas-sensing materials are relatively rare at this time. Herein, Ti 3 C 2 T x and WSe 2 are selected as model materials for hybridization and implemented toward detection of various volatile organic compounds. The Ti 3 C 2 T x /WSe 2 hybrid sensor exhibits low noise level, ultrafast response/recovery times, and good flexibility for various volatile organic compounds. The sensitivity of the hybrid sensor to ethanol is improved by over 12-fold in comparison with pristine Ti 3 C 2 T x . Moreover, the hybridization process provides an effective strategy against MXene oxidation by restricting the interaction of water molecules from the edges of Ti 3 C 2 T x . An enhancement mechanism for Ti 3 C 2 T x /WSe 2 heterostructured materials is proposed for highly sensitive and selective detection of oxygen-containing volatile organic compounds. The scientific findings of this work could guide future exploration of next-generation field-deployable sensors.