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Hempflower-like Fe2O3 microspheres were synthesised by a simple method and its structure was determined by the scanning electron microscopy, X-ray diffraction patterns and Fourier transform infrared spectrum. The effect of reaction temperature and time on the formation and size of hempflower-like Fe2O3 microspheres was further investigated in detail. These results show that the formation of Fe2O3 microspheres with hempflower-like structure strongly depends on the reaction temperature and that the size (ca. 2-10--m) of hempflower-like Fe2O3 microspheres can be easily controlled by adjusting the reaction time. Moreover, the synthesised hempflower-like Fe2O3 microspheres were used as water treatment for the water containing with Cu(II). The adsorption capacity of Fe2O3 microspheres was as high as 35.4 mg/g. The hempflower-like Fe2O3 microspheres was expected to apply in water treatment.