Nanoparticles of NaMgF3:Ce3+, BaLiF3:Ce3+, BaYF5:Ce3+ and BaF2:Ce3+ were prepared from the quaternary microemulsions of CTAB, n-butanol, n-octane and water or brine solution. The X-ray diffraction (XRD) patterns were indexed to pure BaF2, BaLiF3, BaYF5 and NaMgF3 phases. The diameter of the particales, calculated with the help of Debye-Scherrer equation, revealed that these particales were nanoparticals. ESEM images showed the shape and diameter of BaF2:Ce3+ nanoparticles. The spectrum of prepared nanoparticles was observed and discussed. Compared with their powder crystal prepared by high temperature solid reaction, the peaks of the fluorescent spectra changed.Nanoparticles of BaLiF3:Er3+ were prepared from the quaternary microemulsions of CTAB, n-butanol, n-octane and water by hydrothermal method. The X-ray diffraction (XRD) patterns were indexed to a pure BaLiF3 phase. The diameter of the particales was calculated by Debye-Scherrer equation, which was within the range of nanometer. Transmisson electron microscopy (TEM) images proved BaLiF3:Er3+ (hydrothermally treating for 65 h) nanoparticles spherical. The fluorescence emission band of BaLiF3:Er3+ nanoparticles peaked at 1540 nm (4I13/2 →4I15/2). The research showed that hydrothermal method was important in suppressing the appearance of BaF2 impurity.
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