IntroductionTo generate GO and rGO nanoparticles, high‐temperature thermal reduction and the Hummers' technique were both employed. A GO sample is heated and turned into rGO nanopowder. A MoS2 precursor is then added to make a MoS2/rGO composite structure.ObjectivesThe themes of this research work consist of (1) preparation of molybdenum disulfide (MoS2) powder produced by hydrothermal method and sulfurization reaction; (2) graphene oxide (GO) nanoparticles prepared by Hummers' method, compounded with MoS2 to form molybdenum disulfide/reduced graphene oxide (MoS2/rGO) powder in order to reduce the working temperature of a gas sensing process; (3) evaluation of effects of MoS2 and MoS2/rGO sensing devices for NO and NO2 (NOx) gas detection.Results and conclusionWhen tested under various gas concentration and ambient temperature conditions, the NOx gas concentration is 10 ppm, and the working temperature is 150°C, the response value obtained reaches 14.4. In this study, MoS2; a member of two‐dimensional (2D) transition metal sulfide materials, was applied as the main body of the sensing material, and rGO was used as a functional additive. For creating new gas sensing devices, significant progress has been made in creating and designing NOx gas sensing devices for MoS2/rGO composite materials.