Cu-Se compound powders are synthesized by hydrothermal co-reduction from CuSO4•5H2O and SeO2 in deionized water at 120～200 °C. The phases and morphology of the products were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM) respectively. Experimental results show that, the CuSe phase can be synthesized at 120,150,180 and 200 °C, however, the purity phases become more with the temperature decreasing. It indicates that the reaction is more incomplete at lower temperature. Hexagonal flakes with side length 100～400 nm can be observed in the products at 150,180 and 200 °C, among which only the product prepared at 180 °C has the hexagonal flakes with good dispersity and homogeneous size with 200 nm length.