Intercalated nanocomposite based on Mg, Al layered double hydroxide (LDH) and poly(vinyl alcohol) (PVA) was prepared using exfoliation-adsorption technique, and characterized by X-ray diffraction and thermal gravimetric analysis. The results suggest that the intercalated species are formed via the re-aggregation of the delaminated LDH lamellar with the interlayer spacing 14.5 Angstrom, and the thermal stability of the nanocomposite improved compared with the original PVA. (C) 2003 Elsevier Ltd. All rights reserved.