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In this study, Bi2Se3 thermoelectric materials with high density, low thermal conductivity, and excellent thermoelectric performance are prepared using a Se slow-release method. It was found that the number of Se defects in the material could be effectively reduced by changing the content of NaCl solvent, and a certain number of Na atoms are introduced into the Bi2Se3 matrix. The carrier concentration of Bi2Se3 is greatly optimized due to the synergistic effect of the two, leading to a gradual increase in the Seebeck coefficient from −94 to −122 μV K−1 at room temperature. Simultaneously, we conducted an in-depth investigation into the effects of Na doping and Se vacancies on the electronic structure of the materials. Our findings indicate that the presence of these two defects gives rise to resonance energy levels and sharpens the density of state peaks near the Fermi level. This discovery further underscores the potential for enhancing thermoelectric performance. Finally, the Bi2Se3(NaCl)10 sample achieved the maximum ZT value of 0.69 at 550 K, and the average ZT within the temperature detection range reached 0.36, increasing the thermoelectric performance of the material. [ABSTRACT FROM AUTHOR]