In this study, we report the synthesis of PVA/Mg-Al-OH layered double hydroxide composite film by a sonochemical method under different reaction proceedings. The prepared nanocomposites were characterized by X-ray powder diffraction analysis (XRD), Ultraviolet-visible (UV-Vis) spectroscope, Scanning electron microscope (SEM), Energy-dispersive X-ray spectroscope (EDS), and Fourier transform infrared (FTIR)  spectroscopes to study structural, optical, and morphological properties. The basal spacing of PVA/Mg-Al-OH composite increased from 7.694Å to 8.424 Å and the basal spacing of layered double hydroxide enlarged after PVA attached to the surface effects. The average size of particles was determined 23.4 and 4.48 nm. The decrease of particle size explained by the influence of organic groups on the stability of the structure. The optical band gap of PVA/Mg-Al-OH layered double hydroxide was estimated to be 0.64 eV and 0.9 eV, respectively

doi.org/10.32737/0005-2531-2023-1-141-148