In this study, by using nickel chloride solution as a raw material, a nano-sized nickel oxide powder with an average particle size below 50 nm was produced by spray pyrolysis reaction. A spray pyrolysis system was specially designed and built for this study. The influence of nozzle tip size on the properties of the produced powder was examined. When the nozzle tip size was 1 mm, the particle size distribution was more uniform than when other nozzle tip sizes were used and the average particle size of the powder was about 15 nm. When the nozzle tip size increases to 2 mm, the average particle size increases to roughly 20 nm, and the particle size distribution becomes more uneven. When the tip size increases to 3 mm, particles with an average size of 25 nm and equal to or less than 10 nm coexist and the particle size distribution becomes much more uneven. When the tip size increases to 5 mm, large particles with average size of 50 nm partially exist, mostly consisting of minute particles with average sizes in the range of 15~25 nm. When the tip size increases from 1 mm to 2 mm, the XRD peak intensities greatly increase while the specific surface area decreases. When the tip size increases to 3 mm, the XRD peak intensities decrease while the specific surface area increases. When the tip size increases to 5 mm, the XRD peak intensities increase again while the specific surface area decreases.