The nickel@carbon dots hybrid material (Ni@C-dots) was prepared through a simple reduction route and characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and fluorescence spectroscopy. Additionally, the hybrid material was tested as a catalyst to reduce toxic Cr(VI) to nontoxic Cr(III), and UV-vis spectrophotometry was employed to monitor the reduction process. According to the results, the Ni@C-dots hybrid material showed excellent hydrophilicity, good stability, and highly catalytic activity at room temperature.