Spherical particles of several iron oxides have been obtained by pyrolysis of an aerosol generated by ultrahigh frequency spraying of a solution. Two different precursor solutions were used to produce the aerosol: Fe(NO3)3 · 9H2O and FeC6H5O7 · 4H2O. The iron nitrate decomposition leads to the formation of α-Fe2O3, while the organic precursor pyrolysis leads to magnetic particles of either γ–Fe2O3 or Fe3O4. Structural phase, particle size, texture, and homogeneity of the products so obtained can be controlled as a function of some synthesis conditions such as precursor solution, temperature, solution concentration, and surrounding atmosphere.