This paper presented the photoluminescence of Tb-doped Mg-Al layered double hydroxides (Tb-doped MgAl-LDHs) de-pending on phase transition caused by annealing. Tb-doped MgAl-LDHs structure transformed from hexagonal LDHs, cubic MgO to spinel MgAl2O4 phase as temperature varied from 200 to 1000 °C. Emission and excitation spectra of Tb-doped MgAl-LDHs obvi-ously changed with phase transformation. The emissions of Tb3+ ions attributed to5D4→7FJ transitions (J=3, 4, 5, 6) were observed in the emission spectra of all the Tb-doped samples. The ratio of (5D4→7F5)/(5D4→7F6) emission intensity, which was sensitive to sur-roundings of Tb3+ ion, markedly enhanced with temperature rising to 600 from 400 °C. Over 600 °C, the ratio of (5D4→7F5)/ (5D4→7F6) intensity tended to decreasing up to 1000 °C. The change concerning the ratio of the (5D4→7F5)/(5D4→7F6) emission in-tensity might be due to various surroundings of Tb3+ induced by phase transformation.
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