, Phone: þ380 312 643822, Fax: þ380 312 643650As follows from Raman studies, the formation of cadmium chalcogenide nanocrystals in borosilicate glass under thermal treatment at 625-700 8C can be accompanied by precipitation of elemental Se or Te in the form of molecular Se 2 or Te 2 clusters or larger aggregations. The clusters are in most cases formed when the thermal treatment temperature and/or duration values are beyond the range most suitable for the formation of the II-VI nanocrystals. Larger aggregations are formed at intense thermal treatment, precipitation of tellurium being achieved much easier than that of selenium.1 Introduction II-VI (mostly CdSe 1Àx S x ) semiconductor nanocrystal-doped glasses were extensively studied by Raman spectroscopy and the excellent applicability of this technique to determine the nanocrystal parameters was demonstrated. Low-wavenumber Raman scattering by acoustic phonons due to the confinement-related selection rules relaxation in CdSe 1Àx S x nanocrystals was used to estimate the average nanocrystal size [1][2][3][4][5]. Raman spectroscopy was also proven to be a very efficient tool to examine the chemical composition of ternary II-VI nanocrystals diluted in the glass matrix, based on the LO phonon frequencies taking into account the specific effects related to glass matrix pressure, phonon confinement, surface phonon scattering and compositional and size dispersion of nanocrystals within the ensemble [6][7][8][9][10][11][12][13][14][15][16][17][18].Fabrication of II-VI semiconductor nanocrystals in glass matrices is performed by a well-elaborated diffusion-limited growth technique [19][20][21]. Recently Raman scattering studies revealed that not only the nanocrystal size, but also their composition is affected by the growth conditions (thermal treatment temperature and duration) [16,18]. Moreover, it was reported that at certain thermal treatment conditions molecular clusters of selenium can be formed in CdSe and CdSe 1Àx S x nanocrystal-doped glasses [22].