Nano-sized ZrO 2 /MnO 2 /carbon clusters composite materials has been successfully obtained by the calcination of a Zr(acac) 4 /Mn(acac) 3 /epoxy resin complex under an oxygen atmosphere. The compositions of the resulting composite materials were determined using inductively coupled plasma (ICP) spectroscopy, elemental analysis and surface characterization by X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy (TEM). The ultraviolet–visible (UV–VIS), X-ray photoelectron spectra (XPS) and electron spin resonance (ESR) spectra of the composites were also measured. ESR spectral examinations suggest the possibility of an electron transfer in the process of MnO 2 →carbon clusters→ZrO 2 . The visible light-responsive oxidation–reduction ability of the calcined material was also investigated.