The NaYF4:Yb3+,Tb3+(xYb:0.20, xTb:0.04) materials were prepared using the co-precipitation method. The as-prepared material was washed either with or without water in addition to ethanol and thereafter annealed for 5 hat 500 °C. This resulted in materials with moderate or very high up-convers?on luminescence intensity, respectively. The structural study carried out with X-ray powder diffraction revealed microstrains in the rare earth (R) sublattice that were relaxed for the material with very high up-conversion intensity thus decreasing energy losses. The local structural details were investigated with R LII and YK edge ex-tended X-ray absorption fine structure (EXAFS) using synchrotron radiation. Around 10 mol.% of the Yb3+ions were found to occupy the Na site in the material with very high up-conversion intensity. These Yb species formed clusters with the Tb3+ions occupying the regular Na/R sites. Such clustering enhanced the energy transfer between Yb3+ and Tb3+ thus intensifying the up-conversion emission.
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