A nanosheets containing chitosan (CS) and bioactive P2O5:SiO2/Al2O3 were prepared by the sol–gel method. The nanosheets were characterized by XRD, FE-SEM, FT-IR and optical studies. FE-SEM displayed a nano-clustering and dense structure with promising morphology. The optical results reveal that the incorporation of Al2O3 nanoparticles within the phosphosilicate/chitosan system was successfully cross-linked and create a change in the internal electronic structure. The optical band gap increased from 3.6 to 3.8 eV with increasing Al2O3 content. The antimicrobial effectiveness for chitosan/phosphosilicate/(0.6, 0.9 mol.%)Al2O3 nanosheets exhibited remarkable enhancement in the antimicrobial activities that candidates it for spectroscopic and bio-applications.