In this study, nano-sized powder of Ni-ferrite was fabricated by spray pyrolysis process using the Fe-Ni complex waste acid solution generated during the shadow mask processing. The average particle size of the produced powder was below 100 nm. The effects of the reaction temperature, the inlet speed of solution and the air pressure on the properties of powder were studied. As the reaction temperature increased from 80$0^{circ}C$ to 110$0^{circ}C$, the average particle size of the powder increased from 40 nm to 100 nm, the fraction of the Ni-ferrite phase was also on the rise, and the surface area of the powder was greatly reduced. As the inlet speed of solution increased from 2 cc/min. to 10 cc/min., the average particle size of the powder greatly increased, and the fraction of the Ni-ferrite phase was on the rise. As the inlet speed of solution increased to 100 cc/min., the average particle size of the powder decreased slightly and the distribution of the particle size appeared more irregular. Along with the increase of the inlet speed of solution more than 10 cc/min., the fraction of the Ni-ferrite phase was decreased. As the air pressure increased up to 1 $kg/cm^2, the average particle size of the powder and the fraction of the Ni-ferrite phase was almost constant. In case of 3 $kg/cm^2 air pressure, the average particle size of the powder and the fraction of the Ni-ferrite phase remarkably decreased.