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Composite Bi@Bi2O3 microspheres have been synthesized via a microwave-assisted solvothermal route. The Bi@Bi2O3 microspheres had a narrow size distribution in the range 1.2-2.8 mm. Glucose was selected as the reductant, BiCl3 as the bismuth source, and ethylene glycol (EG) as the solvent in the synthesis system. The as-synthesized sample was characterized by X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), particle diameter distribution, energy dispersive X-ray spectroscopy (EDS), ultraviolet-visible (UV-vis) spectroscopy, and photoluminescence (PL) spectroscopy. The photocatalytic activities of the Bi@Bi2O3 microspheres were evaluated by the photodegradation of rhodamine B (RhB) and methyl orange (MO) dyes under UV light irradiation. The degradation reached ~96.6% for RhB and 100% for MO after 4 h reaction in the presence of the as-synthesized Bi@Bi2O3 microspheres.
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