ZnS nanocrystals (NCs) capped with tetramethylammonium (TMAH) were synthesized from ZnCl₂ · 2H₂O and thiourea using a wet chemical process. Further treatments of the nanocrystals such as aging, and annealing have been conducted to examine the stability of the grown samples. The X-ray diffraction spectra show that the crystal has a zinc blende structure with particle size of about 2 nm. The evidence of nanocrystalline character is also clear in the UV–Vis absorption that shows an excitonic peak at about 236 nm (5.2 eV) arising from band edge transitions. A photoluminescence emission peak centered at about 450 nm (2.7 eV) is attributed to transitions between shallow donors and Zn⁺ vacancies. Both absorption and photoluminescence spectra show that sample aging does not affect the characteristics of the sample, possibly due to protection by TMAH capping. Annealing at 700 °C and 900 °C results in the red shift of the photoluminescence.