An effective method of carbothermal reduction was employed to prepare spherical microcrystal NiSnx. alloy powders from oxides of Sn and Ni used as anode materials for Li-ion battery. According to XRD, SEM and TEM analysis, the synthesized spherical NiSnx. powders show a loose submicro/micro-sized structure and a multi-phase composition. The prepared NiSnx. alloy composite electrode exhibits a stable discharge capacity of electrode is ca. 380 mAh g(-1) at constant current density of 50 mA g(-1), and can be retained at 350 mAh g(-1) after 25 cycles. Moreover, NiSnx alloys exhibit excellent high rate performance, i.e. stable discharge capacities of 300-310 mAh g(-1) and the coulombic efficiencies of 97.5-99.5% have been obtained at the current density of 500 mA g(-1). The loose submicro-sized particle structural characteristic and the Ni addition in Sn matrix should be responsible for the improvement of cycling stability of NiSnx electrode. The carbothermal reduction method is simple, low-cost and mass-productive, which should be viable to other alloy composite materials system of rechargeable lithium ion batteries. (C) 2009 Elsevier Ltd. All rights reserved.