SiO2 nanoparticles doped by 10 % mol Cu were prepared via a sol-gel method under process control. The effects of doping and calcination temperature on the structural and photo-catalytic properties of SiO2 nanopowders have been studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and UV-Vis absorption spectroscopy. Cristobalite and tridymite crystalline phases were found at a calcinations temperature range of 900∼1200 ◦C and amorphous phase was formed at a temperature of 800 ◦C for doped SiO2. The photocatalyst activity was evaluated by photocatalytic degradation kinetics of aqueous methyl orange (MO) under visible radiation. The results show that the photocatalytic activity of the 10 % mol Cu doped SiO2 nanopowders have a larger degradation efficiency than pure SiO2 under visible light at 900 ◦C temperature.