Some cobalt antimonides have been prepared and studied as the candidate anode materials for lithium ion batteries. Reversible capacities of 424, 423 and 546 mA@h@g -1 were measured at the first cycle for as-solidified CoSb2, CoSb3 and annealed CoSb3 respectively. A low lithium ions diffusion coefficient in the order of 10-16 m 2@s -1 was estimated from the coulometric titration measurements in the annealed CoSb3 electrode. It was found that the electrochemical properties of fine powders are significantly better than coarse powders. However the SEM picture shows that the nano-sized CoSb3powders gathered to larger granules, which worsens somewhat the capacity retention of the nano-sized materials, although the volume capacities of the annealed and ball milled CoSb3 remain near twice of that of graphite after 50 cycles.