The vacuum ultraviolet (VUV) spectroscopic properties of praseodymium (Pr3+, 1at%) doped LaF3 nanocrystals/glass at room temperature and 20 K are reported. Two types of Pr3+ ions, those in LaF3 nanocrystals and those in the glass host, were excited to 4f 5d band by VUV using synchrotron radiation as an excitation source, and emissions of 1S0 → 1D2 (336 nm), 1S0 → 1I6 (397 nm ) of Pr3+ in the nanocrystals and emissions of 4f 5d → 3HJ, 3FJ of Pr3+ in the glass appeared at the same time. But unlike in the bulk sample crystals, emission of 3P0 → 3HJ, 3FJ as the second step of the quantum splitting (QS) of Pr3+ in the LaF3 nanocrystals was not observed at room temperature, which could be explained that Pr3+ ions in the glass absorbed the energy of 3P0 → 3H4 of Pr3+ in the nanocrystals. Two types of excitation spectra monitoring different emissions were also measured, so it could be observed that the lowest energy of 4f 5d band of Pr3+ in the nanocrystals was about 53 500 cm-1 (186 nm) and in the glass about 33 800 cm-1(295 nm), respectively. These emission and excitation spectra were contrasted to those of bulk sample crystals LaF3∶Pr3+.
