In the present study, a solvent-thermal method was used to successfully synthesise hydroxylated nickel chloride with a fullerene-like structure. This synthesized material was implemented as a substrate for surface-enhanced Raman scattering (SERS), and crystal violet (CV) served as a probe molecule to evaluate the SERS performance under an excitation wavelength of 532 nm. The results obtained demonstrate the remarkable sensitivity of the substrate in detecting crystal violet, even at the significantly low concentration of 10-8 mol/L.Furthermore, by introducing sulphur and carefully adjusting the concentration ratios of the reactants, a sulphur-hydroxylated nickel chloride compound was synthesised while retaining its characteristic fullerene-like structure. This incorporation of sulfur into the substrate effectively enhanced the Raman scattering effect, thereby significantly improving its sensitivity for the detection of trace amounts of crystal violet (CV) at an unprecedented concentration as low as 10-11 mol/L, resulting in an improvement of three orders of magnitude. In addition, an examination of the SERS signal from 5000 data points revealed a standard deviation (RSD) of 4.4% for the sulphur-hydroxylated nickel chloride substrate, indicating exceptional reproducibility and uniformity.The morphological and structural characterisation of both hydroxylated and sulphur-hydroxylated nickel chloride was carried out using various analytical techniques such as scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD).