A new electrochemical route for the synthesis of a hybrid thin film of endohedral metallofullerene (Dy@C-82 is used here) and polythiophene is presented, which exploits the unique, compatible redox properties of the couple. The electrochemical response of the resulting Dy@C-82/polythiophene film resembles that of Dy@C-82 in organic solvents except for the potential peak shifts, but is markedly different from that of a pure metallofullerene solid film. Both the polythiophene backbones and the Dy@C-82 moieties appear to retain their individual electrochemical properties in the hybrid film. The film was characterized by UV-visible and Fourier transform infrared absorption spectroscopy, time-of-flight secondary ion mass spectrometry, and scanning electron microscopy. The data suggest that the DY@C-82 molecules have been uniformly dispersed in the polythiophene matrix, forming a compact film. The formation and the electrochemical response of the hybrid film have been systematically studied, refining the viable strategy for the encapsulation of metallofullerenes into conducting polymers. (c) 2004 Elsevier B.V All rights reserved.