In this study, Fe2O3.Al2O3/polyethylene composites were prepared using a two-step process. In the first step, PE is synthesized using titanium based metallocene catalyst system. While the synthesized PE was subsequently purified, hydrated alumina filled PE (MHFP) composites was formed by the hydrolysis of methylaluminoxane (MAO). In the second step, Fe2O3.Al2O3/PE was prepared via thermal decomposition of ferric formate in a high temperature solution of MHFP composite. The structure, morphology, and thermal properties of the composites were characterized using the XRD, FTIR, SEM-EDX, TGA, and DSC analytical techniques. Results showed that the incorporation of a suitable amount of Fe2O3.Al2O3 into the composites enhances the thermal stability. (c) 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011