Lithium triborate (LiB 3 O 5 ) was produced by different synthesis methods, which included hightemperature solid-state reaction, microwave-assisted high-temperature solid-state reaction, and precipitation-assisted high-temperature solid-state reaction. After the synthesis, metal oxides (CuO and Al 2 O 3 ) were doped into LiB 3 O 5 to enhance its thermoluminescent (TL) properties, and the TL intensities were compared with each other. The identification and characteristics of undoped and doped LiB 3 O 5 were determined by X-ray diffraction (XRD), Fourier transform infrared (FTIR) analyses, differential thermal analyses (DTA), scanning electron microscopy (SEM), and particle size analyzer. The glow curves were obtained by using a TL reader. The results showed that synthesis routes affected the physical and structural properties of lithium triborate, which have an important effect on its TL intensity.