Abstract: A new silicon-based luminescence material—C(film)/Si(SiO2)(nanometer particles)/C(film) has been prepared by sputtering Si(SiO2) nano-particles on amorphous carbon film in Argas, then depositing amorphous carbon film on Si(SiO2) nano-particles in vacuum. The sample consists of 6 layers of carbon films and 5 layers of Si(SiO2) nano-particles. Finally, the sample is annealed at different temperatures(RT-750℃). Its configuration has been studied by means of TEM, SEM, XRD and XPS. TEM image shows that Si(SiO2) nano-particles almost be spherical, whose diameter is about 30nm. SEM images show that the thickness of the sample is about 50μm and the surface of the sample is relatively flat and compact. Hole structure is found on the surface of sample annealed at 400℃, the particles on the surface are well-distributed and compacted after annealed at 650℃, particle aggregations grow after annealed 750℃. XRD spectra shows that the sample is almost composed by SiO2and Si, and the ratio of SiO2/Si alternately changes with the increase of annealing temperature: SiO2are reduced to Si by C atoms at 400℃, so the content of Si is highest, on the contrary, the content of SiO2is lowest. Si nanometer particles are oxidized superiorly beyond 400℃, so the content of Si gradually decreases, the content of SiO2 gradually increases and becomes to highest at 650℃. XPS spectra shows that C atoms diffuse into Si (SiO2) nano-particles layer during annealing, and produce SiC by reacting with Si at 650℃.