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This work deals with the spectroscopic properties of single crystalline samples of KTb3F10. Green luminescing KTb3F10 is an efficient UV radiation converter with a quantum yield of about 40% upon UV-A excitation, while it is also an efficient scintillator upon excitation by 20–50 kV X-ray photons. The temperature dependence of the integral photoluminescence as well as the decay time of KTb3F10 monitored for the Tb3+ emission show that the internal quantum yield between 100 and 800 K is almost constant, while the external quantum yield is modulated, likely due to a change in reabsorption at elevated temperatures. In contrast, the low temperature range between 3 and 63 K reveals a change of the local Tb3+ environment in KTb3F10, which is indicated by an anomaly in the heat capacity and by a strong change of the decay time as well as by a distinct shift of the photoluminescence spectra at low temperatures. In addition, temperature dependent magnetic susceptibility measurements and a structure refinement based on single crystal X-ray diffraction data were performed.