The objective of this work is to develop an environmentally friendly method for preparation of ZnO nanocomposites. ZnO nanocomposites were prepared by three natural fibers such as coir, sawdust, and chitosan using aqueous solution of zinc chloride and sodium hydroxide. The functional groups of ZnO, C=O for polysaccharide, and N-H bending vibration of amine were confirmed by FTIR spectroscopy. A new high intensity absorption band has been observed at 424 cm⁻¹ which corresponds to the E₂ mode of hexagonal ZnO. The crystallinity and phase formation of coir, chitosan, and sawdust combined ZnO nanocomposites were confirmed by X-ray diffraction patterns. XRD patterns revealed the polycrystalline nature of ZnO composites belonging to the hexagonal phase with (101) preferential lattice orientation. The microstructural parameters were calculated for coir, chitosan, and saw wood combined ZnO composites. Also texture coefficients were estimated for all the diffraction lines of ZnO based nanocomposites. SEM and TEM analyses confirmed evenly distributed nanosized grains in the ZnO composites. The UV-Vis absorption spectra were observed where the blue shift absorption peak was at 334 nm. The optical band gap values were estimated in the range of 3.18–3.26 eV. The emission peak was observed at ~388 nm and ~463 nm by photoluminescence spectroscopy.