Mesostructured Y2O3:Eu3+ phosphor particles were fabricated by a pyrolytic conversion from a pertinent metal–organic framework (MOF), namely, MOF-76(Y):Eu with 1,3,5-benzenetricarboxylic acid ligands, aiming at luminescence sensing of H2O2. Large rod-like MOF-76(Y):Eu particles 301 ± 150 μm in average length were initially obtained by a reaction at 80 °C for 24 h. They were converted to rod-like Y2O3:Eu3+ particles 122 ± 34 μm in average length after heating at 500 °C. The Y2O3:Eu3+ particles actually consisted of primary nanoparticles 7.55 ± 1.43 nm in average size and had a mesoporous structure with a high specific surface area of 80.8 m2 g−1. The photoluminescence intensity of the Y2O3:Eu3+ particles decreased after treating with an aqueous H2O2 solution, which was recognized as H2O2-responsive turn-off luminescence. Three other kinds of Y2O3:Eu3+ particles, including those obtained from other MOF particles synthesized at room temperature, were also prepared and the effects of the microstructure on the degree of turn-off luminescence were examined. It was then observed that the H2O2-sensitivity was enhanced more effectively by using the MOF-derived Y2O3:Eu3+ particles having the higher specific surface area.
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