Nanomaterials presented with a lot of attention in this generation. It is one of the most advancing technology in recent date. It involves many benefits in semiconductors, solar cells medicine, agriculture, photovoltaic cell, electrooptic modulator sensors, electroluminescent and doped phosphor materials. Owning to its various methods have been employed to synthesis metal sulphide nanoparticles and many others. However, many conventional synthesis method use toxic, expensive substances which can increase production cost and pose significant environmental and health problems to the society. Recently, nanoparticles are play an important role in environment and economy. All the prepared complexes were used to synthesize metal sulfide nanoparticles. The metal sulfide nanoparticles were successful prepared by thermal decomposition of the single-source precursor in HDA solution at different synthesizing temperature 140 ℃, 180 ℃ and 220 ℃. Hence, in the present study, metal sulphide Hexa Decyl Amine capped copper sulphide nanoparticles prepared from Thiourea substituted pyrrolidone copper (II) complex. copper complexes were characterized by Thermo-gravimetric analyser (TGA), Fourier-transform infrared spectroscopy (FTIR) and elemental analysis (EA). HDA Capped CuS nanoparticles was characterized via Ultra- violet visible spectroscopy (UV/Vis), Photoluminescence spectroscopy (PL) X – Ray diffraction (XRD) and transmission electron microscopy (TEM). The maximum peak observed at 298nm for all different temperature and the effect of temperature was significant factor in the synthesis of HDA-Capped Copper sulfide nanoparticles, which the particles size decreasing with increasing synthesizing temperature 220 ℃ with blue shifted also X- Ray diffraction at 45º (112).