As the electrodes of secondary battery are made with sulfur compounds, excellent electrode system of environmental non-toxicity, high specific energy density and low material cost can be obtained. In this study, the FeS_2 fine compound powders for active material in the battery were synthesized by mechanical alloying. Fine Fe-53.5 wt.%S powders of 450 nm of mean size were fabricated by mechanical alloying for 60 hours at the horizontal attritor. As the mechanical alloying time increases, particle size of Fe-53.5 wt.%S was decreased and steady state of Fe-53.5 wt.%S compound powders was obtained at 30 hours. Fe-53.5 wt.%S cathode shows the excellent discharge capacity (1011 mAh/g).