Zinc sulphide was obtained through hydrothermal decomposition of [Zn(S2CNEt2)] under different experimental conditions such as temperatures and reaction times. Hydrothermal reactions were carried out in a stainless steel autoclave at 160, 180 and 200 °C for 3, 6 and 24 hours. The obtained products were characterized using X-ray diffraction, scanning and high resolution transmission electron microscopies. Particle size and microstrain were determined by Rietveld refinement of experimental X-ray diffraction patterns. The obtained crystal size values were in the range of 6.1 to 30 nm and as the temperature and reaction times increase the particle size also increases. Band gap values are in the range of 3.34 to 3.60 eV and are highly dependent on the crystal microstrain. The catalyst activities were studied through the degradation of methylene blue dye solutions under ultraviolet radiation.