In order to prepare fine metal-oxide particles and circulating fluidized particles coated with metal compounds, experimental investigations were carried out to study spray pyrolysis using the superior heat transfer characteristics of a circulating fluidized bed (CFB). Quartz sand particles of three different size ranges were used as circulating fluidized particles in the CFB loop, and a nickel-acetate solution was injected as droplets into the CFB riser, It was recognized that the size distribution of the prepared particles was considerably affected by the size of circulating fluidized particles. Increasing the circulating fluidized particle size was found to lead to larger nickel-oxide particles. It was shown that the concentration of the injected nickel-acetate solution had no influence on the geometric characteristics of the prepared nickel-oxide particles.