A novel process was attempted to prepare nano-scale Cu2Sb alloy powders as anode materials for Li-ion batteries. The preparation started with chemical reduction of Cu2Sb in an aqueous solution with sodium citrate as a complexing agent and KBH4 as a reducer. The analysis of scanning electron microscopy and X-ray diffraction showed that as-prepared nano-scale Cu2Sb powders presented tetragonal structure with particle size of 50–70nm. Cycling between 0 and 1.2V, the nano-scale Cu2Sb alloy showed good cyclability with a stable specific capacity of 200mAhg−1 within 25 cycles.