A new method of synthesis of BiFeO 3 prepared by thermal decomposition of Bi[Fe(CN) 6 ]4H 2 O M. C. Navarro M. C. Lagarrigue J. M. De Paoli R. E. Carbonio M. I. Go ´mez Received: 5 June 2009 / Accepted: 12 August 2009 / Published online: 10 September 2009 Ó Akade ´miai Kiado ´, Budapest, Hungary 2009 Abstract In order to investigate the formation of the multiferroic BiFeO 3 , the thermal decomposition of the inorganic complex Bismuth hexacyanoferrate (III) tetra- hydrate, Bi[Fe(CN) 6 ]4H 2 O has been studied. The starting material and the decomposition products were character- ized by IR spectroscopy, thermal analysis, laboratory powder X-ray diffraction, and microscopic electron scan- ning. The crystal structures of these compounds were refined by Rietveld analysis. BiFeO 3 were synthesized by the decomposition thermal method at temperature as low as 600 °C. There is a clear dependence of the type and amount of impurities that are present in the samples with the time and temperature of preparation. Keywords Bi[Fe(CN) 6 ]4H 2 O  BiFeO 3 synthesis  Thermal decomposition Introduction The study of multiferroic materials is of great interest because they exhibit ferroelectricity and magnetic ordering in the same phase [1]. The application of an electric (magnetic) field to a multiferroic material is expected to control spontaneous magnetization (polarization) by means of magnetoelectric interactions. Therefore, the study of multiferroic materials has been an interesting subject not only from the viewpoint of solid-state physics but also because of their possible applications in electric devices such as electric field induced magnetic memory effects, electro-optic transducer controlled by magnetic fields [2–4], etc. However, ferroelectricity and magnetism hardly coexist due to the structural competition. We can find many examples of these materials in the perovskite oxides fam- ily, e.g., BiFeO 3 , BiMnO 3 , and YMnO 3 [5–9]. BiFeO 3 , one of the very few multiferroics with a simultaneous coexis- tence of ferroelectricity and antiferromagnetic order in perovskite oxides, has attracted much attention for many decades since the 60s. BiFeO 3 has a ferroelectric Curie temperature (T C ) of 1,103 K and antiferromagnetic Ne ´el temperature (T N ) of 634 K [10]. It shows also a well sat- urated ferroelectric hysteresis loop with a large saturated polarization of approximately 24 mC/cm 2 [11]. Owing to this magnetoelectric coupling, BiFeO 3 based systems may be used to develop novel applications [12–16] in the field of radio, television, satellite communications, sensors, memory devices, and digital recording, etc. Several ways for the preparation of BiFeO 3 were informed [17–21]. Most of them try to obtain the highest purity, to be obtained at the lowest possible temperature in order to reduce cost and volatility of Bi, or to obtain nanostructured materials. The most common impurities obtained during synthesis of BiFeO 3 are Bi 2 Fe 4 O 9 and Bi 25 FeO 40 , which are usually leached out by washing with nitric acid, but this is not a convenient procedure since it can change stoichiommetry of BiFeO 3 by selectively dis- solving some of the elements. The synthesis of oxides, particularly perovskites and related compounds from the decomposition of inorganic coordination compounds allows one to lower the reaction temperature and to obtain M. C. Navarro  M. C. Lagarrigue  M. I. Go ´mez (&) Instituto de Quı ´mica Inorga ´nica, Facultad de Bioquı ´mica, Quı ´mica y Farmacia, Universidad Nacional de Tucuma ´n, Ayacucho 471, 4000 San Miguel de Tucuma ´n, Argentina e-mail: mgomez@fbqf.unt.edu.ar J. M. De Paoli  R. E. Carbonio INFIQC-CONICET, Departamento de Fisicoquı ´mica, Facultad de Ciencias Quı ´micas, Universidad Nacional de Co ´rdoba, Ciudad Universitaria, 5000 Co ´rdoba, Argentina 123 J Therm Anal Calorim (2010) 102:655–660 DOI 10.1007/s10973-009-0417-5