As the electrodes of secondary battery are made with sulfide composite powders, excellent electrode system of environmental non-toxicity and with high specific energy density and low material cost can be obtained. In this study, the (Fe, M)S2 composite powders was synthesized by mechanochemical processes (MCP) in order to improve of the cycle life in bettery. The formation of pyrite phase appreared at the case which adds nickel, but it was not observed in the case where the transition metal was does not add but the transition metal such as cobalt, molybdenum was added in stead. From charge-discharge test results, the initial discharge capasity of (Fe, Ni)S2 electrode was 845 mAh/g. The initial discharge capasity of (Fe, Co)S2 electrode was 500mAh/g, but it showed a better cycle perfoemance than the case where the diffrent transition metal was added.