In particular, gas sensors require characteristics such as high speed, sensitivity, and selectivity. In this study, we fabricated a NOX gas sensor by using a multi-walled carbon nanotube (MWCNT)/zinc oxide (ZnO) composite film. The fabricated MWCNT/ZnO gas sensor was then treated by a 450℃ temperature process to increase its detection sensitivity for NOx gas. We compared the detection characteristics of a ZnO film gas sensor, MWCNT film gas sensor, and the MWCNT/ZnO composited film gas sensor with and without the heat-treatment process. The fabricated gas sensors were used to detect NOX gas at different concentrations. The gas sensor absorbed NOX gas molecules, exhibiting increased sensitivity. The sensitivity of the gas sensor was increased by increasing the gas concentration. Additionally, while changing the temperature inside the chamber for the MWCNT/ZnO composite film gas sensor, we obtained its sensitivity for detecting NOX gas. Compared with ZnO, the MWCNT film gas sensor is excellent for detecting NOX gas. From the experimental results, we confirmed the enhanced gas sensor sensing mechanism. The increased effect by electronic interaction between the MWCNT and ZnO films contributes to the improved sensor performance.