Nano-sized Sn powder was prepared by pulsed wire evaporation method. The Sn powder and carbon black were charged in jar and ball milled. The milling time was varied with 10 min., 1h, 2h, and 4h, respectively. The milled powders were dried and the shape and size were observed by FE-SEM. Nano-sized Sn powders were plastic-deformed and agglomerated by impact force of balls and heat generated during the SPEX milling. The agglomerated Sn powder also consisted of many nano-sized particles. Initial discharge capacities of milled Sn electrode powders with carbon powder were milled for 10 min., 1h, 2h, and 4h were 787, 829, 827, and 816 mAh/g, respectively. After 5 cycle, discharge capacities of Sn electrode powders with carbon powder milled for 10 min., 1h, 2h, and 4h decreased as 271, 331, 351, and 287 mAh/g, respectively. Because Sn electrode powders milled for 2h constist of uniform and fine size, the cyclability of coin cell made of this powders is better than others.