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Fe nanoparticles and branched nanostructures of iron oxide were synthesized by chemical reduction in aqueous phase. The mechanism of formation of iron oxides as a function of the amount of surfactant employed during the synthesis process was studied. Specifically Fe, Fe₂O₃, and Fe₃O₄ nanoparticles were obtained. The oxidation of Fe to Fe₃O₄ and finally to Fe₂O₃ was carried out by oxidative etching process, decreasing the amount of stabilizer agent. The structures obtained were characterized by high resolution (HRTEM) and scanning/transmission (STEM) electron microcopies, energy dispersive spectroscopy (EDS), and optical spectroscopy (UV‐Vis and IR).