The combination of two highly versatile materials as reduced graphene oxide (rGO) and molybdenum disulfide (MoS₂ forms the layered rGO-MoS₂ hybrids that have great potential for sensing applications. In this paper, we developed a cost-effective, time-saving, and efficient microwave-assisted method to exfoliate rGO and MoS₂ nanosheets in a powder mixture for the formation of rGO-MoS₂ hybrids. The formation of hybrids with a combination of organic and inorganic 2-D layered materials offers new possibilities for the development of gas sensitive materials. The applied microwave treatment is a simple and fast process for the large-scale synthesis of rGO-MoS₂ hybrids. The synthesized rGO-MoS₂ hybrids were characterized by X-ray diffraction, scanning electron microscope, energy dispersive X-ray spectroscopy, Raman, X-ray photoelectron spectroscopy, and thermogravimetric analyses to determine the phase structure, surface morphology, defect formation, binding energy, thermal stability and so on. The synthesized rGO-MoS₂ hybrids were tested for sensing application and showed the good performance to detect gases such as O₂, N₂, and NH₃ at room temperature.