Nano-sized Ni-ferrite powder was fabricated by spray pyrolysis process using the waste solution resulting from shadow mask processing. The average particle size of the powder was below 100 nm. The effects of the concentration of raw material solution, the nozzle tip size and air pressure on the properties of powder were studied. As the concentration increased, the average particle size of the powder gradually increased and its specific surface area decreased, but size distribution was much wider and the fraction of the Ni-ferrite phase greatly increased as the concentration increasing. As the nozzle tip size increased from 1 mm to 2 mm, the average particle size of the powder decreased. In case of 3 mm nozzle tip size, the average particle size of the powder increased slightly. On the other hand, in case of 5 mm nozzle tip size, average particle size of the powder decreased. Size distribution of the powder was unhomogeneous, and the fraction of the Ni-ferrite phase decreased as the nozzle tip size increasing. As air pressure increased up to 1 kg/$cm^2$, the average particle size of the powder decreased slightly, on the other hand, the fraction of the Ni-ferrite phase was almost constant. In case of 3kg/$cm^2$ air pressure, average particle size of the powder and the fraction of the Ni-ferrite phase remarkably decreased, but size distribution was narrow.