Nanosized Co powders were prepared by a chemical reduction method with and without CTAB (cetyltrimethylammonium bromide,C19H42BrN) and carbon-coating heat treatment at 700°C for 1 h, and the electrochemical properties of the prepared nanosized Co powders were examined to evaluate their suitability as an anode material of Li-ion batteries. Nanosized amorphous Co-based powders could be synthesized by a chemical reduction method in which a reducing agent is added to a Co ion-dissolved aqueous solution. When the prepared nanosized Co-based powders were subjected to carbon-coating heat treatment at 700°C for 1 h, the amorphous phase was crystallized, and a Co single phase could be obtained. The Co-based powder prepared by chemical reduction with CTAB and carbon-coating heat treatment had a smaller first discharge capacity (about 557 mAh/g) than the Co-based powder prepared by chemical reduction without CTAB and carbon-coating heat treatment (about 628 mAh/g). However, the former had a better cycling performance than the latter from the third cycle. The carbon-coated layers are believed to have led to quite good cycling performances of the prepared Co-based powders from the third cycle.