In this study nickel particles were prepared by spray pyrolysis of NiSO4·6H2O solution with hydrogen and/or other additives such as urea, ammonia.For each method of preparation we investigated the properties of the particles produced by varying process variables such as the furnace set temperature, residence time, initial salt concentration and additives molar ratio.Addition of additives helps the particles reduction with spherical morphology and particle size.Even without hydrogen additives could produce solid nickel particles, though under stricter condition.