A new method is reported for obtaining microspirals of iron-based compounds by interfacial interaction. A thin film of Fe(OH)₃ is obtained as a result of interaction between an aqueous solution of iron salts and gaseous ammonia. Upon drying, it is transformed into Fe(OH)₃ microspirals with a diameter of up to 10 µm. These microspirals can be transformed into Fe₂O₃ microspirals by annealing in air. As a result of hydrogen reduction, Fe microspirals are formed. Both the annealing in air and that in hydrogen allow the retaining of the morphology. The material synthesized is characterized by electronic microscopy methods, X-ray diffraction, diffuse reflectance Fourier transform infrared, and Mössbauer and photoelectron spectroscopies. The electrocatalytic properties of the electrode based on Fe₂O₃ microspirals as a catalyst of hydrogen evolution and the magnetic properties of Fe microspirals are tested. A hypothesis is proposed on the formation of microspirals by the gas–solution interface technique.