Nickel powders were synthesized by the hydrazine reduction of nickel chloride solution containing ammonia in DEA solutions. The size distribution of nickel powders were investigated as a function of ammonia concentration, hydrazine concentration and the mixed composition ratio of diethanolammine (DEA) and triethanolammine (TEA). Nickel powders with the size in submicron range were obtained at for 45 minutes by hydrazine reduction of nickel chloride solution in DEA solutions. The hydrazine concentrations showed significant effects on the particle size and shape distribution of nickel powders under molar ratio of 2.0 condition. As the mixed volume ratio of TEA and DEA increased, nickel powders with relatively larger particle size and low agglomeration were obtained. Nickel powders with particle size in the ranged from 0.4 to were obtained at the 50 of TEA.