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Y2O3:Tb3+ hollow microspheres have been successfully prepared on a large scale with polystyrene microspheres as templates followed by subsequent calcination. All X-ray diffraction peaks can be indexed to the pure cubic phase of Y2O3. Transmission electron microscopy and scanning electron microscopy images indicate that the average size of the hollow spheres is ca.1.3 µm and the thickness of the shells is ca. 50 nm. The microspheres show a strong green emission corresponding to the 5D4–7F5 transition of Tb3+ under ultraviolet excitation. The optimum Tb3+ concentration was 3 mol% to obtain the highest photoluminescence intensity. This study indicates that a calcining temperature of 800°C is needed for high luminescence efficiency.
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