Double layered hydroxide (LDH) nanomaterials were prepared by the co-precipitation method and characterized by X-ray diffraction. The XRD pattern of LDH showed a rhombohedra phase with a hexagonal lattice. After blending polyvinyl alcohol/polyethylene oxide (PVA/PEO) by casting method, the as-prepared LDH was loaded to the polymer blend in different amounts; 0, 1, 3, 5, 7, 8, and 10 wt.%. The results of the XRD revealed a significant change in the crystallinity of the polymer nanocomposite films. Energy-dispersive X-ray spectroscopy (EDX) was used to characterize the LDH nanomaterials. The ratio of Zn and Fe (4:1) in LDH nanopowder is confirmed. Field-emission scanning electron microscopy (FE-SEM) was used to test the morphology of the LDH nanopowder and polymer nanocomposites. A homogenous rough surface in the form of paper-like layers was observed in LDH nanoparticles. Fourier transform infrared (FTIR) reflectance spectra were measured at room temperature in the wavenumber range 400 – 4000 cm−1. It was noted that there are no interactions between PVA/PEO blend and LDH nanoparticles. The UV–vis spectra of the nanocomposite films were discussed to determine different optical parameters to look for the applications of the studied nanocomposite films if any.