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Research on the development of high-end luminescent materials, especially nanostructured phosphors (thermoluminescent (TL) materials), is of interest for application in radiation dosimetry. This study hydrothermally synthesized CuO and subsequently annealed it at different temperatures to modify its structural and intrinsic defect properties. X-ray diffraction showed that CuO was a pure monoclinic phase and that its crystallinity improved with annealing temperature. The band gap ranged from 1.47 ± 0.01 to 1.51 ± 0.03 eV depending on the annealing temperature. Substantive measurements based on TL were made on a sample annealed at 700 °C, since it was the most sensitive of all annealed samples. A glow curve measured at a heating rate of 1 Research on the development of high-end luminescent materials, especially nanostructured phosphors (thermoluminescent (TL) materials), is of interest for application in radiation dosimetry. This study hydrothermally synthesized CuO and subsequently annealed it at different temperatures to modify its structural and intrinsic defect properties. X-ray diffraction showed that CuO was pure phase monoclinic and that its crystallinity improved with annealing temperature. The band gap ranged from 1.47 ± 0.01 to 1.51 ± 0.03 eV depending on the annealing temperature. Substantive measurements based on TL were made on a sample annealed at 700 °C, since it was the most sensitive of all annealed samples. A glow curve measured at a heating rate of 1 °C/s after a beta source of 50 Gy showed three distinct peaks. Finally, their corresponding trap depths were determined as 0.57 ± 0.11 and 1.28 ± 0.06 eV/s after a beta source of 50 Gy showed three distinct peaks. Finally, the corresponding trap depth was determined as 1.28 ± 0.06 eV.