In this work, we report a simple one-pot approach to prepare hollow BaF2 microcubes employing the reaction of Ba(NO3)2 and NaBF4 under hydrothermal conditions. X-Ray diffraction, scanning electron microscopy, electron diffraction, transmission electron microscopy, and photoluminescence spectra were used to characterize the samples. Contrast experiments indicated that the triblock copolymer of EO20PO70EO20 (P123) and the complex of citrate both played important roles for the formation of hollow BaF2 cubes. Furthermore, the use of NaBF4 as fluoride source is indispensable for obtaining the microstructures. For the first time, we demonstrate that microcubes of BaF2 with hollow interiors can be synthesized via a combination of soft-templating mechanism and oriented attachment process. Additionally, the near-infrared luminescence of lanthanide ions (Er, Nd, and Yb) doped BaF2 hollow microcubes were discussed in detail.
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