Tin-based alloy/carbonaceous composite materials are attractions for Li-ion rechargeable batteries because of their high capacity. A novel Ni-Sn-P mesocarbon microbead (MCMB) composite material for lithium-ion batteries was prepared by an electroless plating method. On the basis of X-ray color mapping analysis by electron probe microanalyzer, the nanosize Ni-Sn-P was precipitated not only on the surface but in the interior of MCMB powders. The Ni-Sn-P/MCMB composite anode exhibited large capacity (418 mAh/g in the tenth cycle) and the coulombic efficiency of the Ni-Sn-P/MCMB anode is as high as 98% even after the twenty-fifth cycle. In addition, the Ni-Sn-P/MCMB composite anode showed a significant improvement in electrochemical performance. Therefore, the Ni-Sn-P/MCMB provides a new type of anode material for lithium-ion batteries with an enhanced capacity. (c) 2006 The Electrochemical Society.