To avoid the formation of hollow spheres during spray pyrolysis, NH3 was employed to change the mechanism of forming NiFe2O4 from aerosols, containing Ni(II) and Fe(III) nitrates in the required stoichiometric ratio. Nearly spherical, solid submicron NiFe2O4 particles with narrow size distribution were produced in one step using a dilute aqueous solution at pyrolysis temperatures as low as 823 K. However, higher pyrolysis temperatures (≥1023 K) reduced the oxides to metallic alloy of Ni and Fe due to dissociation of NH3. The forming steps and possible reaction mechanisms for aerosol droplets involved in the process were discussed.
