Cu-SiO2 nanocomposites have been studied to achieve hybrid structures at room temperature without an inert atmosphere. First, SiO2 nanoparticles were synthesized by the sol-gel method. Second, SiO2 nanoparticles deposited with copper (Cu-SiO2) were prepared by the reaction of the SiO2 nanoparticles and copper chloride at room temperature for 6 hrs with catalyst and without catalyst, respectively. Results showed that the SiO2 nanoparticles with about 90 nm diameters were covered with Cu nanoparticles. The Cu-SiO2 nanocomposites were investigated with TEM, energy dispersive X-ray spectroscopy analysis (EDS), and X-ray photoelectron spectroscopy (XPS).