In this study, with the help of grinding and sonication, the bulk state of molybdenum disulfide was transformed into a two-dimensional sheet, and composite nanofiber consisting of molybdenum disulfide MoS2/polyvinyl alcohol (PVA) has been successfully developed via electrospinning process. X-ray diffraction (XRD) pattern showed the preferred orientation along the (002) plan of The MoS2 nanosheet. Rietveld refinement was applied to obtain the microstructure parameters of the MoS2. The formation of S-S and Mo-S bonds in MoS2 was confirmed by the Fourier-transform infrared spectroscopy (FTIR). FE-SEM images reveal the surface morphology of MoS2 nanosheets, which typically exhibit a flat and layered structure resembling stacked atomic layers of MoS2 two-dimensional nature.In contrast, the MoS2/PVA fibers display a uniform, interconnected nanofiber network with a distinct random formation. Also, Atomic Force Microscopy (AFM) images show the formation of the uniform MoS2/PVA nanofibers, and the evaluated root mean square (RMS) roughness values for PVA and MoS2/PVA fibers are 250 nm and 277 nm, respectively. To elucidate the elemental composition of the MoS2 nanofibers, Energy Dispersive X-ray Spectroscopy (EDX) analysis was performed, confirming the presence of molybdenum and sulfur in the compound. Finally, diffuse reflectance spectroscopy (DRS) was applied to study the optical properties of the MoS2/PVA composite. In addition, the measurement of the contact angle shows that the surface of the nanofibers is hydrophilic, and the amount of hydrophilicity decreases by adding MoS2 nanosheets.