Various properties of composite materials were studied using Fourier-transform infrared (FTIR) spectral and Raman analysis techniques in this study. These two commonly used methods can quickly provide information about the analyzed materials. Hydroxypropyl methylcellulose (HPMC) has been widely used in anti-corrosion fields such as those related to foods and pharmaceuticals, and especially in the study of tribology-related issues. HPMC is derived from natural materials. However, as a biopolymer, the tribological capability of HPMC is limited. Therefore, biocompatible micro-particles with superior tribological properties, like MoS2, are added to enhance the tribological properties of film materials during application. FTIR spectral and Raman analyses were performed to investigate the characteristics of HPMC and HPMC/MoS2 composite materials, as well as their degradation behaviors in different solutions. The Raman spectral analysis also illustrated the good uniformity of the MoS2 distribution in thin films. Lastly, an X-ray diffraction (XRD) analysis confirmed the influence of the MoS2 addition on the crystallization and surface roughness of the thin films. This study demonstrated that the Raman, FTIR, and XRD techniques can rapidly provide important information about composite materials, making them suitable for in-process, real-time analyses.