Abstract: nanocomposites Ag₂Se/Se/SiO₂ were successfully synthesized by two steps. Firstly, nano Se/SiO₂ precursors were prepared by acidifying the mixture of sodium metasilicate(Na₂SiO₃) and sodium selenosulphate(Na₂SeSO₃). Secondly, the precursors were transformed into nanocomposites Ag₂Se/Se/SiO₂ by reacting with aqueous AgNO3 solutions. Then the samples were characterized by Transmission electron microscopy(TEM), X-ray diffraction(XRD), Ultraviolet-visible Spectrophotometer(UV-vis), Fourier Transform Infrared(FT-IR), Laser Raman(LRS) and Photoluminescence(PL). Finally, the electrochemical properties and electrochemiluminescence(ECL) of as-obtained products were studied. Resultsshow that the compound has certain electrochemical activity, and electroluminescent has good performance.