Abstract. We have reported the influence of annealing temperature and heating rate on thermoluminescence (TL) properties of nanocrystalline calcium borate, CaB2O4, powder synthesized by solution combustion method. Powder X-ray diffraction experiments were carried out on CaB2O4 to get the crystal phase and size. The samples were annealed using the TLD oven and exposed to cobalt-60 source. TL glow curves were measured and recorded using a Harshaw model 3500 TLD reader. The crystal phase confirmed one major phase of CaB2O4 with 27 nm in size. CaB2O4 has a simple glow curve with only one and a well defined peak at around 150 °C. TL intensity was higher after annealing the material before irradiation which indicated the importance of annealing. It was found that an annealing temperature at 300 °C for one hour and the heating rate of 10 °C s -¹ was the best procedure to produce high TL intensity.