Polyimide/gamma-Fe(2)O(3) nanocomposite films with superparamagnetic behavior have been prepared by thermal curing of the magnetite (Fe(2)O(3)) nanoparticles-containing poly(amic acid) (PAA) derived from pyromellitic dianhydride (PMDA) and 4,4'-oxydianiline (4,4'-ODA) in NNdimethylacetamide (DMAc). To improve the dispersion ofthe doped nanoparticles, the amine-functionalized Fe(2)O(3) nanoparticles reacted with the PMDA dianhydride in DMAc firstly, and then polymerization was carried out by adding 4,4'-ODA and then PMDA to form the PAA-grafted magnetic particles. Thermal treatment of the Fe(2)O(3)-doped precursor film converted the PAA into its final polyimide form with concomitant transformation of Fe(2)O(3) into gamma-Fe(2)O(3), yielding a polyimide film with superparamagnetic behavior. The distribution of nanoparticles in the polymer matrix was investigated by transmission electron microscopy and field emission scanning electron microscopy. The nanoparticles and composite films were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, magnetic and mechanical measurement. (c) 2007 Elsevier B.V. All rights reserved.