In this work, the synthesis and thermoluminescence properties of new ZnO phosphors obtained by a chemical method are reported. Some samples were exposed to beta particle irradiation for doses ranging from 10.0 up to 6,400 Gy, and it was found that the thermoluminescence response as a function of dose is linear for doses below 200 Gy, and sublinear with no saturation clouds for greater doses. A broad shape glow curve with maximum located above 230 °C, that shifts to lower temperatures as dose increases, indicating that second order kinetics thermoluminescence processes are involved. The lower detection limit was estimated to be 13 Gy. We conclude that the phosphors under study are promising to develop dosimeters for high dose radiation dosimetry.