Abstract. X-ray diffraction and Mössbauer spectroscopy techniques were used to study the structure and hyperfi ne interactions of multiferroic Aurivillius compounds Bi m+1 Ti 3 Fe m-3 O 3m+3 . Samples were synthesized by two methods, that is, the solid-state sintering at various temperatures and mechanical activation in a high-energy ball mill. The compounds were obtained from a mixture of three polycrystalline powder oxides, that is, TiO 2 , Fe 2 O 3 and Bi 2 O 3 . At room temperature, the Aurivillius compounds are paramagnetic materials with orthorhombic crystal structure. The c lattice parameter of the unit cell depends linearly on the m − number of layers with perovskite--like structure. Based on the Mössbauer studies, it is concluded that the hyperfi ne interactions parameters do not change with m number.