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Multilayer structures with five periods of amorphous SiGe nanoparticles/SiO2 layers with different thickness were deposited by Low Pressure Chemical Vapor Deposition and annealed to crystallize the SiGe nanoparticles. The use of grazing incidence RBS was necessary to obtain sufficient depth resolution to separate the signals arising from the individual layers only a few nm thick. The average size and areal density of the embedded SiGe nanoparticles as well as the oxide interlayer thickness were determined from the RBS spectra. Details of eventual composition changes and diffusion processes caused by the annealing processes were also studied. Transmission Electron Microscopy was used to obtain complementary information on the structural parameters of the samples in order to check the information yielded by RBS. The study revealed that annealing at 900 °C for 60 s, enough to crystallize the SiGe nanoparticles, leaves the structure unaltered if the interlayer thickness is around 15 nm or higher.