Wet-chemical process to prepare the ZnO nanoparticles, and this were then incorporated in different proportions of weight to a poly (methyl methacrylate) (PMMA) matrix. Bulk ZnO particles were also embedded in PMMA for comparison. The structural and vibrational properties of the composites were investigated using X-ray diffraction (XRD), Fingerprint Raman spectroscopy (RS), and high-resolution transmission electron microscopy (HRTEM). ZnO's pure phase has been confirmed by XRD analysis. Compared to bulk ZnO and other composites, the crystallite size of ZnO nanoparticles and their nanocomposite films (0.1 wt%) dropped by 52% and 50%, respectively. The presence of ZnO nanoparticles was further verified by the technique of Raman spectroscopy. Higher magnifications with HRTEM images revealed uniform spherical nanoparticles, whereas lower magnifications revealed well-crystalline spherical and disc-like morphologies with sizes ranging from ~5 to 50 nm. Further, two pathogenic studies, specifically E. coli and S. aureus, at the ambient condition were used in the biological activity studies of antibacterial data. The well-diffusion method was adopted, and the inhibition zones of E. coli (12-15 mm) and S. aureus (9-12 mm) were observed for PMMA/ZnO nanocomposites (0.1–0.2 wt.%). The synthesized nanocomposite (NC) films exhibit great potential for use in sensors, solar cells, and the medical field.