Nano-scaled MNb2O6(M = Mn, Zn) was successfully synthesized via a two-step hydrothermal method. It is important to control the exact pH of the reaction solution in order to obtain pure products. The as-prepared samples both crystallize in the columbite structure. Interestingly, the products possess a flower-like morphology in a pseudo-six-fold symmetry, which is in fact arrayed by two-dimensional nanosheets. Their surface areas (51 m(2)/g for MnNb2O6 and 103 m(2)/g for ZnNb2O6) are about 25-50 times of those prepared by solid state reaction. UV-vis diffuse reflectance spectra show the nano-scaled sample has a stronger absorption and a narrower band gap than its bulk form. The estimated band gap energies are 2.70 eV (MnNb2O6) and 3.77 eV (ZnNb2O6), respectively. The nano-scaled ZnNb2O6 exhibits a double enhancement of photocatalytic activity in the decolorization of methylene blue than bulk ZnNb2O6. (C) 2013 Elsevier Ltd. All rights reserved.