Cadmium sulfide nanoparticles have been synthesized by hydrothermal method using cadmium acetate, thiosemicarbazide, and sodium hydroxide as precursors with hexamethylene tetramine as the surfactant. From the X-ray diffraction analysis, it is observed that synthesized CdS nanoparticles show cubic phase. The presence of HMTA in CdS was confirmed by FT-IR analysis. The bandgap value of CdS nanostructure has been estimated by DRS–UV-Visible spectral analysis. The formation of flower-like nanoclusters was observed using scanning electron microscopy (SEM). The application of CdS nanoparticles in photocatalytic degradation was also studied.