In this study, undoped and Ni-doped ZnS nanoparticles were fabricated using a hydrothermal method to explore their structural, optical, and surface properties. X-ray diffraction (XRD) analysis confirmed the cubic crystal structure of ZnS, with the successful incorporation of Ni ions at various doping levels (2%, 4%, 6%, and 8%) without disrupting the overall lattice configuration. The average particle size for undoped ZnS was found to be 5.27 nm, while the Ni-doped samples exhibited sizes ranging from 5.45 nm to 5.83 nm, with the largest size observed at 6% Ni doping before a reduction at higher concentrations. Fourier-transform infrared (FTIR) spectroscopy identified characteristic Zn-S vibrational bands, with shifts indicating successful Ni incorporation into the ZnS lattice. UV-visible spectroscopy revealed a decrease in the optical band gap from 3.72 eV for undoped ZnS to 3.54 eV for 6% Ni-doped ZnS, demonstrating tunable optical properties due to Ni doping, which could enhance photocatalytic performance under visible light. Scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) analyses confirmed the uniform distribution of Ni within the ZnS matrix, while X-ray photoelectron spectroscopy (XPS) provided further confirmation of the chemical states of the elements. Ni doping of ZnS nanoparticles alters the surface area and pore structure, optimizing the material's textural properties for enhanced performance. These findings suggest that Ni-doped ZnS nanoparticles offer promising potential for applications in photocatalysis, optoelectronics, and other fields requiring specific band gap tuning and particle size control.