β-NaYF4 microcrystals co-doped with Yb3++, Er3++/Tm3++, and Gd3++ ions were synthesized via a hydrothermal method using rare-earth chlorides as the precursors. The SEM and XRD data show that the doped β-NaYF4 form uniform hexagonal prisms with an approximate size of 600-800 nm. The partial substitution of Y by Gd results in size reduction of microcrystals. Upconversion luminescence spectra of microcrystals upon 980 nm excitation contain characteristic intra-configurational ff bands of Er3++/Tm3++ ions. An addition of Gd3++ ions leads to a significant enhancement of upconversion luminescence intensity with maxima at 5 mol % of dopant.
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