The large-scale synthesis of the metal–organic framework Eu(1,3,5–BTC)·6H2O nanocrystallites with delicate morphologies such as sheaflike, butterflylike, and flowerlike superstructures composed of nanowires have been realized via a simple solution phase method at room temperature. Time-dependent experiments indicate that these superstructures were constructed by the splitting crystal growth mechanism, as has been noted in some minerals in nature. The synthetic parameters such as reaction time, concentration and molar ratio of reactants, surfactant, and reaction temperature all affected the morphology of the Eu(1,3,5–BTC)·6H2O architectures. These well-arranged architectures exhibit red emission corresponding to the 5D0 → 7F2 transition of the Eu3+ ions under UV light excitation, and the lifetime is determined to be about 0.22 ms.
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