In this study, a three-dimensional (3D) nano/micropeony-like hierarchical Cu2-xSe has been synthesized by a one-step solvothermal method with ethylenediamine and ethylene glycol as mixed solvents. The 3D copper foam was selected as sacrificial template, and the aqueous solution of mixture Na2SeO3 and Na2Se was chosen as a suitable selenium source for this reaction. Note that 3D Cu2-xSe nano/micro architectures are rarely reported in previous studies. Meanwhile, the 3D template can provide a more stable environment and huge specific surface area, which lead to more stable and regular Cu2-xSe grown in situ. Every nanoflake of the uniform Cu2-xSe hierarchical structures is about 5 mu m in diameter and 50 nm in thickness. These nanoflakes can be used as a Fenton-like catalyst for the degradation of Methylene Blue and Rhodamine B dye solution without any kind of light source and thus obtain good effect. (C) 2013 Elsevier B. V. All rights reserved.