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In this research work, pure and doped hydroxyapatite samples were synthesized using hydrolysis and hydrothermal methods to produce powder material. The crystal structure was carried out by producing data using the X-ray diffraction system and the Rietveld method using material analysis using diffraction software. Then the sample was irradiated with different radiation absorbed doses, and their thermoluminescence response was investigated from the dosimetry point of view. The results showed that the synthesis method, doping, and annealing temperature could significantly affect the crystal structure and thermoluminescence dosimetry response of hydroxyapatite samples, consequently. The results showed that the high-temperature annealing process and dopant could lead to the formation of the β-TCP crystal phase during or after the synthesis of hydroxyapatite, and the percentage of this formed phase increased when raising the temperature, and finally led to increase in the thermoluminescence response.