The relationship between the factors (i.e. the concentrations of Yb3+ and Er3+ and heating temperature in air) and the properties of photoluminescence (PL) and up-conversion luminescence of YTiTaO6:Er3+/Yb3+ whose crystalline phase depended on heating temperature in air was examined using samples synthesized hydrothermally. The intense green emission (: 2H11/2,4S3/2→4I15/2 transitions of Er3+) was obtained by the excitation at 288 nm using the indirect energy transfer from the YTiTaO6 host crystal, which was about 1.8 times stronger than that obtained by the direct excitation at 380 nm via the f-f transition (: 4I15/2→4G11/2) of Er3+. Aeschynite phase exhibited intermediate luminescence property. The up-conversion emission intensity increased with increasing heating temperature and became the maximum at x = 0.10 and y = 0.20 with euxenite phase, although the co-presence of Yb3+ gave negative effect on the PL intensity of ErxYbyY1-x-yTiTaO6. As heating temperature rose to 1300–1400 °C the intensity of the red up-conversion emission (: 4F9/2→4I15/2 transition) became greater than that of the green emission (: 4S3/2→4I15/2 transition), accordingly the position of the color chromaticity coordinates shifted slightly from green to yellow.
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