Antimony zinc alloy, Zn4Sb3, was studied as a potential material for negative electrodes of lithium-ion batteries. It was found that the reversible capacity of ball-milled Zn4Sb3 in the first cycle reached 507 mA h g−1 and increased up to 580 mA h g−1 when the alloy was ball-milled with about 11.8 wt.% graphite additives. Ex-situ XRD analyses of the pure Zn4Sb3 electrodes during cycling showed that several lithium-containing compounds such as LiZnSb, Li3Sb and LiZn have been formed successively during the insertion of lithium into Zn4Sb3. It was found that the ball-milled composite, Zn4Sb3/C7, possesses high initial reversible capacity, small voltage hysteresis and good capacity retention, which make this material an interesting potential electrode for lithium-ion batteries.