The structure of heat-treated sol-gel-made SiO 2 samples containing copper or iron in various amounts was studied using Raman spectroscopy and x-ray diffraction. The treatments were in air in the temperature range 200-800 • C. Copper and iron concentrations were in the range 7-55 wt%. It was found that in the samples containing copper, the metal is mainly dissolved in the SiO 2 network when the thermal treatment is at low temperatures. For higher annealing temperatures, first a copper silicate is formed and then most of the copper forms cupric oxide particles at temperatures of about 800 • C. In samples containing iron, the formation of particles with nanometric size of the g-Fe 2 O 3 (maghemite) phase is observed after annealing at 500 • C. At 800 • C the maghemite phase is transformed into the stable hematite (a-Fe 2 O 3 ) phase. Copyright