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Bi 2 Fe 4 O 9  was synthesized using a polyol-mediated method. X-ray powder diffraction (XRPD) revealed that the as-synthesized sample is nano-crystalline. During heating, the X-ray amorphous powder transformed into a rhombohedral perovskite-type bismuth ferrate followed by a second transformation into mullite-type Bi 2 Fe 4 O 9  at higher temperatures. This transformation was studied at  in-situ  conditions by temperature-dependent XRPD and  57 Fe Mössbauer spectroscopy. The  57 Fe Mössbauer spectra indicate the existence of two Fe 3+  species at two different octahedrally coordinated sites leading to the conclusion that the as-synthesized powder of the polyol synthesis possesses a disordered (Bi 1– x  Fe  x  )FeO 3  perovskite structure. Rietveld refinements have unambiguously supported this observation and this results suggest that one third of the Bi 3+  sites are substituted by Fe 3+  representing the initial chemical composition. This study has shown that as-synthesized nano-materials are not always similar to the respective micro-crystalline ones.

Bi 2 Fe 4 O 9 : Structural changes from nano- to micro-crystalline state