The nano-composite photocatalyst with Fe-doped anatase TiO2 nanoparticles (5-10 nm in size) coupling with TiO2(B)- an uncommon synthetical polymorph of titanium oxide with monoclinic structure nanobelts (30-100 nm in width, 10-30 nm in thickness, and several micrometers in length) was fabricated via a two-step procedure: hydrothermal synthesis of the TiO2(B) nanobelts followed by co-deposition of the Fe-doped anatase TiO2 nanoparticles on the nanobelts. The microstructure and photocatalysis of the samples were systematically studied by TEM, HRTEM, EDS, XRD, UV-vis and BET techniques. The purpose of the coupling of different TiO2 polymorphs is to accelerate the separation of photogenerated charges and improve the photon quantum efficiency. The Fe doping endows the TiO2 based nano-composite with visible light photocatalytic activity. An efficient photodegradation of the methyl orange aqueous solution was achieved under visible light (lambda > 420 nm) irradiation, revealing the potential applicability of such nano-composite in some industrial fields, such as air and water purifications. (C) 2010 Elsevier B.V. All rights reserved.