Abstract: Cr(VI) is highly soluble in water, and more than 0.1 mg/L of Cr(VI) can be toxic to the environment and life and health.Therefore, the exploitation of a sensitive method for the determination of hexavalent chromium ions is particularly important. Herein, N-3-(trimethoxysilyl) propylethylenediamine (DAMO) and trimethylsiliconazole (TSIM) were used as the double silicon source precursors, and sodium citrate was used as the reductive agent, and the spherical double silicon source silicon quantum dots (D-SiQDs) were prepared by hydrothermal method. Results showed that D-SiQDs had a spherical structure and a large number of amino and imidazole groups on the surface. Under the optimal conditions, the optimal excitation wavelength of D-SiQDs was 359 nm, and the maximum emission wavelength was 451 nm, and D-SiQDs had good light stability. The fluorescence of D-SiQDs could be selectively quenched by Cr(VI) and the fluorescence quenching degree as a good linear relationship with the concentration of Cr(VI) in the range of 0.5-100 μmol/L. The detection limit was 0.056 μmol/L. The recoveries of detecting Cr(VI) in tap water samples were in the range of 100.37%-105.83%, and the relative standard deviations were all less than 2.36%. Therefore, this paper provides an idea for developing D-SiQDs fluorescent probes for the high-sensitivity detection of Cr(VI).