Abstract. In this research, the mechanical activation method is proposed as an alternative process of preparation of the (BiFeO 3 ) 1-x -(BaTiO 3 ) x solid solutions with various concentrations of barium titanate (x = 0.1÷0.9). However, mechanical milling itself does not allow obtaining the desired products and additional thermal treatment is needed to complete the solid-state reaction. In the present studies, X-ray diffraction and 57 Fe Mössbauer spectroscopy were applied as complementary methods in order to study the structural and magnetic properties of materials. The investigations revealed that an increase of BaTiO 3 concentration causes changes in the crystalline and hyperfi ne magnetic structure of the studied (BiFeO 3 ) 1-x -(BaTiO 3 ) x system.