A series of NH4Y3F10 sub-microcrystals had been prepared by a one-step hydrothermal route. The morphological and structural properties of the sub-microcrystals were studied by scanning electron microscopy (SEM) and powder X-ray diffraction (XRD). The results of SEM and XRD suggested that NH4Y3F10 sub-microcrystals have irregular shapes with their sizes varying from 100nm to 500nm and the structures of obtained NH4Y3F10 sub-microcrystals are cubic phase. Additionally, the down-converting(DC) phenomenon have been observed under UV excitation in (Yb3+, Nd3+) co-doped NH4Y3F10. It is found that luminescent efficiency of 10%Yb, 1%Nd co-doped NH4Y3F10 sub-microcrystals is stronger than that of 10%Yb, 5%Nd co-doped NH4Y3F10 sub-microcrystals. The energy transfer mechanism of the emission spectra of (Yb3+, Nd3+) co-doped NH4Y3F10 is discussed.
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