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We offer a complete structural and optical study of samples containing silicon nanocrystals (Si-NCs) embedded in SiO2/SiON multilayers, varying the oxynitride layer thickness from 2.5 to 7nm. Using energy-filtered transmission electron microscopy we have determined the size distribution of the precipitated Si-nanoaggregates. Raman scattering measurements were used to investigate the Si-NC size and crystalline quality. By combining both techniques, the nanoaggregate crystalline degree has been evaluated, with values around 50% for all the samples. Photoluminescence spectroscopy has shown a blueshift of the emission at smaller NC sizes, presenting the sample with Si-NCs of 3.9nm the best emission properties.