High gamma dose-resistant undoped ZnO and Tb-doped ZnO thermoluminescent (TL) micro-phosphors were prepared by the spray pyrolysis method. Scanning electron microscopy shows crystalline rods with hexagonal morphology, (0.1-0.4 µm diameter, and about 1 µm length). Raman spectra dispersion reveals a würtzite form. Photoluminescence (PL) study of irradiated zinc oxide films indicates the generation of defects produced by gamma irradiation resulting in an increased probability of electron-hole exciton recombination. PL spectrum shows emission bands from 5D4-7Fj=6,5,4,3 transitions ascribed to Tb3+ dopant in zinc oxide phosphor. X-ray diffraction patterns for both types of films growth (undoped ZnO and Tb-doped ZnO) are typical of zinc oxide crystalline structure, with no noticeable effect of Tb ions. Dosimetric properties, for both samples, show a low TL fading signal and TL reproducibility signal for undoped ZnO and Tb-doped ZnO samples was 29 and 57 %, respectively. The kinetic parameters such as activation energy E, frequency factor s, and Rm values, were obtained by Computerized Glow Curve Deconvolution (CGCD) assuming Mixed Order Kinetic model (MOK). The results show that the MOK well described the glow curves of zinc oxide films. The heating rate effects produced a broadening of glow peak located at 420 K. For purposes like radiation detector, atomic effective number (Zeff) was obtained: 27.74 and 56.47 for undoped ZnO and Tb-doped ZnO samples, respectively. The samples were exposed to gamma radiation in a wide range of 0.25–20 kGy dose. TL properties of undoped ZnO and Tb-doped ZnO samples show that these materials could be used to detect high doses in a gamma radiation field.