Depending on the particle size of the zinc sulfide (ZnS), some optical properties may change. In particular, the inclusion of manganese (Mn2+) as an impurity shows interesting optical properties, which has become a topic of interest. Therefore, it is necessary to perform a complementary optical characterization of the ZnS: Mn nanocrystals. In this work was analyzed by different techniques of characterization the optical behavior of ZnS: Mn nanocrystals. We found that the sample doped with a concentration of 10% shows the highest luminescent response. It was also observed an atomic rearrangement using thermal treatments above 500 °C, resulting in a cubic-to-hexagonal (Wurtzite) phase transition. Finally, the shape and position of the experimental TL glow curves are analyzed using the glow curve deconvolution technique, in order to characterize the transfer of electrons observed in the nanocrystals.