Upconversion luminescence materials have been proved to have a good efficiency on converting low energy light to high energy light. These materials have received considerable attentions for many applications such as bio-labels, sensors, using for developing solar cells and photocatalytic applications under sunlight. Among many inorganic host materials, NaYF4 has been proved to be the best for doping lanthanide ions and have a good upconversion emission due to its low phonon energy, chemical stability, and transparency in the near infrared to ultraviolet range. In this study, NaYF4:Yb3+,Tm3+ upconversion luminescence materials were synthesized by hydrothermal method at temperature of 90 to 200 °C for period between 1 to 24 hours. The synthesized NaYF4:Yb3+,Tm3+ were characterized by X-ray diffraction, scanning electron microscopy, and fluorescence spectroscopy. The hydrothermal temperature and reaction time have
strongly influence on phases and upconversion emission of the synthesized NaYF4:Yb3+,Tm3+. At
90 °C for 1 hour of reaction time, the pure cubic phase of NaYF4:Yb3+,Tm3+ was found. After increasing temperature and reaction time, the NaYF4:Yb3+,Tm3+ converted from cubic phase to hexagonal phase. Under excitation of 980 nm diode laser, the hexagonal NaYF4:Yb3+,Tm3+ exhibited the emission wavelength at about 656 nm (3F2 → 3H6), 469, 492, 552 nm (1G4 → 3H6), 537 nm (1D2 → 3H5), 450, 461 nm (1D2 → 3F4), 362 nm (1D2 → 3H6) and 345 nm (1I6 → 3F4). The upconversion emission intensity of the hexagonal NaYF4:Yb3+,Tm3+ was much stronger, compared with that of the cubic NaYF4:Yb3+,Tm3+.