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Nickel oxides (NiO) nano- and submicron particles were synthesized by a low-pressure spray pyrolysis system. Conversion of micrometer droplets into particles in the gas phase using NiO synthesis as a model was studied. Different types of precursors (aqueous Ni(NO₃)₂·6H₂O, NiCl₂, and Ni(HCO₂)₂·2H₂O) and temperatures from 400 to 900°C have great influences on controlling the size and morphology of final particles. The results show that operation of a low-pressure system leads to substantial changes in size and morphology of particles, and that the NiO particles having size around 20nm can be generated under a limited of conditions.