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Micro‐Raman spectra of amorphous As–Se–S:Cd films prepared by thermal evaporation on silicon and silicate glass substrates measured at different laser power densities show the formation of CdS1–xSex nanocrystals in the As–Se–S:Cd film under laser beam illumination due to a photoinduced material transfer and photoenhanced diffusion in the laser spot area. The material transfer and the photoenhanced diffusion are caused by a non‐thermal interaction of light with the amorphous As–Se–S:Cd films. The chemical composition of the CdS1–xSex nanocrystals can be determined from the difference of the CdSe‐like and CdS‐like LO phonon wavenumbers in the Raman spectra. The photoluminescence peak energies are in agreement with the CdS1–xSex composition, with the average nanocrystal size being somewhat above the exciton Bohr radius.

Nanometric Sn2P2S6 crystalline powders and ceramics are studied by x-ray diffraction and Raman spectroscopy. The average crystallite size is estimated from TEM and x-ray data. The observed features in the Raman spectra are discussed in view of confinement-related selection rules relaxation, surface phonon modes and possible partial substitution of sulfur by oxygen at the nanometric powder surface.

Spectral dependence of photoinduced structural transformation and related changes of E g opt , α and n of thermally evaporated ternary As 40 S 60-x Se x thin films have been studied under the exposure to bandgap and super-/sub-bandgap light of LED. The irradiation by bandgap and super-bandgap light with intensity 0.1 W/cm 2 leads to partial photoinduced polymerization of molecular structural units into continuous network that is characteristic for the bulk glasses with appropriate stoichiometric composition. The efficiency of structural transformation depends on penetration depth of excitation beam. The maximum photosensitivity (i.e. changes of E g opt , α and n) were achieved at the wavelengths ~ 100 nm above the bandgap wavelength for each appropriate composition. Beyond the region of maximal photosensitivity the values of optical parameters and kinetics of photoinduced changes depend on relation between exposed and unexposed sublayer for super-bandgap beams or on absorption coefficient for sub-bandgap light.

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