Nickel sulfide nanoparticles were successfully synthesized through a meticulous process involving a well-mixed powder of Ni(CH3COO)2∙2H2O and Thiourea. The X-ray diffraction analysis provided insights into the structural nature of NiS, revealing its polycrystalline characteristics with a hexagonal system. This information is fundamental, as it forms the basis for understanding the material’s behavior and functionality in various applications. Determining the average values of mean crystallite size, microstrain, and dislocation Nickel sulfide nanoparticles were successfully synthesized through a careful process involving a well-mixed powder of Ni(II)2∙2H2O and Thiourea. The X-ray diffraction analysis provided insights into the structural nature of NiS, revealing its polycrystalline characteristics with a hexagonal system. This information is crucial as it forms the basis for understanding the material’s behavior and functionality in various applications. Determining the average values of mean crystallite size, microstrain, and dislocation density for the (100) plane (32.62 nm, 0.000296, and 0.000939 nm-2, respectively) contributes to a comprehensive understanding of the material’s structural features. The photoluminescence spectrum of NiS in the visible region revealed split peaks at 405.8 and 428.25 nm, shedding light on the radiative recombination process between electrons and holes. The confirmation of thermal stability through a thermogravimetry diagram is essential for applications in elevated temperature environments, ensuring the material’s reliability under varying conditions. Analyzing the stoichiometry of NiS using energy dispersive spectroscopy attached to transmission electron microscopy provides insights into the material’s composition. Cyclic voltammetry results indicating a diffusion coefficient greater than that of NiS added to carbon hold significance for electrochemical applications. The unique characteristic peaks observed in cyclic voltammetry for fuel cell applications suggest the potential use of NiS in energy conversion technologies, broadening its scope of application. The confirmation of NiS’s ability to elucidate the physical and electronic properties of electrochemical systems through electrochemical impedance spectroscopy underlines its importance as a versatile material in various research and practical domains.