| Summary: | The MXene Ti<sub>3</sub>C<sub>2</sub>T<sub>x</sub> was synthesized using hydrofluoric acid and an improved multilayer method in this study. Subsequently, a Bi<sub>2</sub>O<sub>3</sub>/Ti<sub>3</sub>C2T<sub>x</sub> composite material was produced through hydrothermal synthesis. This composite boasts a unique layered structure, offering a large surface area that provides numerous contact and reaction sites, facilitating the adsorption of ammonia on its surface. The prepared Bi<sub>2</sub>O<sub>3</sub>/Ti<sub>3</sub>C<sub>2</sub>T<sub>x</sub>-based sensor exhibits excellent sensing performance for ammonia gas, including high responsiveness, good repeatability, and rapid response–recovery time. The sensor’s response to 100 ppm ammonia gas is 61%, which is 11.3 times and 1.6 times the response values of the Ti<sub>3</sub>C<sub>2</sub>T<sub>x</sub> gas sensor and Bi<sub>2</sub>O<sub>3</sub> gas sensor, with response/recovery times of 61 s/164 s at room temperature, respectively. Additionally, the gas sensitivity mechanism of the Bi<sub>2</sub>O<sub>3</sub>/Ti<sub>3</sub>C<sub>2</sub>T<sub>x</sub>-based sensor was analyzed, and the gas sensing response mechanism was proposed. This study shows that the sensor can effectively enhance the accuracy and precision of ammonia detection at room temperature and has a wide range of application scenarios.
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