Abstract Studies of Raman scattering spectra and scanning electron microscopy imaging combined with energy-dispersive X-ray spectroscopy data of II-VI semiconductor nanocrystals formed in zinc-containing borosilicate glass matrix are carried out. It is shown that diffusion of zinc from the matrix at 625 to 700 ?C results in the formation of mixed Cd1yZnyS1xSex nanocrystals with Zn content up to 30 %, as determined from the LO phonon frequencies. An increase of the Zn content in the nanocrystals with the thermal treatment temperature and duration is observed. A uniform distribution of zinc over the nanocrystal volume is assumed based on the diffusion coefficient data.