In this part of the investigation, mixed raw materials’ solution was subjected to aerosolization to obtain NiFe2O4 powder. The final product was found to be hollow spheres. Depending on the pyrolysis temperature, the degree of crystallinity of NiFe2O4, changes from non-crystalline (T<753 K) to fully crystalline (T>933 K). In addition, increasing the pyrolysis temperature was found to increase the average particle size, and lower the specific surface area and the average bulk density. The results also indicate that the concentration of the starting solution has an appreciable effect on the product characteristics, i.e. decomposition efficiency, average particle size, particle size distribution and amount of product.