Syndiotactic Polystyrene based composites have recently shown wide applications in optoelectronic, magnetic, and memory-based devices. In the present work, we have first reported Polystyrene coated fine FeS Nanocomposites using the low-cost Sol-Gel route. These Nanocomposites were characterized for structural properties through XRD, Molecular properties through FT-IR spectroscopy, and morphology through Scanning Electron Microscope (SEM) techniques. XRD peak shows the high crystallinity in the material with the formation of FeS pyrite structure. Polystyrene (PS), which has amorphous nature, turns into crystallite composites with FeS Nanocomposites. Composites also exhibit excellent photoluminescence behavior.