Nickel powders were synthesized by the reduction of hydrazine of nickel salts from diethanolamine (DEA) solution, and the morphological characteristics of nickel powders were investigated with various process conditions such as the addition of hydrazine, reaction temperature, the composition of mixed solvents. The addition of hydrazine in DEA solution largely affected the size control of nickel powders. Under N2H4/Ni2+molar ratio= 1.5 and 2.0 conditions, spherical nickel powders in the submicron range were obtained owing to higher the reduction rate. An increase of temperature increased the size of nickel particles. At 220°C for 40min, the nickel powders were composed of polyhedral particles with a high crystalline in the submicron range. The mixed volume ratio of TEA to DEA solvent improved the inhibition of agglomerate between particles.