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β-NaYF 4 microcrystals co-doped with Yb 3+ , Er 3+ /Tm 3+ , and Gd  3+  ions were synthesized via a hydrothermal method using rare-earth chlorides as the precursors. The SEM and XRD data show that the doped β-NaYF 4 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 Er 3+ /Tm 3+ ions. An addition of Gd 3+ ions leads to a significant enhancement of upconversion luminescence intensity with maxima at 5 mol % of dopant.

Gd3+-Doping Effect on Upconversion Emission of NaYF4: Yb3+, Er3+/Tm3+ Microparticles