Magnetic α-Fe₂O₃/Fe₃O₄ heterogeneous nanosheets were successfully fabricated via the hydrothermal and glucose reduction process, they and their precursor were characterized by SEM, TEM, XRD and VSM techniques, and the effect of additive concentration, hydrothermal temperature and hydrothermal time on morphology and properties of them were investigated. Firstly, α-Fe₂O₃ nanosheets were prepared by the hydrothermal approach, the results revealed that the optimized preparation conditions for α-Fe₂O₃ nanosheets were the FeCl₃ concentration of 25 mM, the NaH₂PO₄ concentration of 7.5 mM, the hydrothermal temperature of 220 °C, and the hydrothermal time of 24 h. while, α-Fe₂O₃/Fe₃O₄ heterogeneous nanosheets were constructed by the glucose reduction method with α-Fe₂O₃ nanosheets as the precursor, the results showed that the magnetic α-Fe₂O₃/Fe₃O₄ heterogeneous nanosheets with largest saturation magnetization of 25.1 emu/g were obtained by calcination at 600 °C for 4 h when the mass ratio of α-Fe₂O₃ nanosheets and glucose was 1:12.

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