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In this work, the physical characterization of LiGdxY1−xF4 (x = 0.05, 0.3, 0.7, and 1.0) and LiGdF4:Eu3+ microparticles was performed. The distribution coefficient of LiGdxY1−xF4 (x = 0.05) was determined for the first time (0.84). Based on kinetic characterization data, the LiGdF4 sample was chosen for further Eu3+ doping (0.1 and 1.0 at.%). For the LiGdF4:Eu3+ sample, Eu3+ emission was clearly observed under the excitation of Gd3+. This fact indicates an effective energy transfer from Gd3+ to Eu3+. The temperature-dependent spectral characterization of the LiGdF4:Eu3+ (1.0%) sample revealed that in the 30–250 K temperature range, a broad emission peak is evidenced. Its intensity sharply increases with the temperature decrease. We made a suggestion that this phenomenon is related to the irradiation-induced defects. The integrated luminescence intensity ratio of this broad peak and the Eu3+ emission were taken as temperature-dependent parameters. The sensitivity values are very competitive, and the first maximum occurs at 174 K (3.18%/K). The kinetic characteristics of both Gd3+ and Eu3+ did not demonstrate a notable temperature dependence. The LiGdF4:Eu3+ sample showed the possibility of being used as an optical temperature sensor, operating in the cryogenic temperature range.