BiFeO microtetrahedra, microcubes and microspheres were successfully synthesized by a simple hydrothermal process and by adding different additive agents. The formation mechanism of BiFeO microcrystals was proposed; the additive agents had important influences on the morphology and facet exposure of the products. The catalytic activity of these materials was evaluated by the degradation of RhB in a heterogeneous photo-Fenton process. The BiFeO microcubes showed enhanced photo-Fenton catalytic activity, which can be attributed to an exposed {001} facet with the active O atoms. The hydroxyl radicals are the main active group in the heterogeneous photo-Fenton catalytic degradation. This study may provide a new method to design and synthesize novel nanoscale and microscope functional materials.
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