The compounds of the type A2 B6 (CdS , ZnS , CdxZn1-xS ) are widely applied in photoreceptors and solar cell manufacturing. Development of technologies for obtaining inexpensive thin layer of semiconductor on large surfaces remains a major current scientific issue . A new original method for obtaining thin layers of CdS and CdxZn1-xS has been developed [1]. The thin films were obtained using the method of pulverization of solutions containing cadmium or zinc ions and sulfur containing organic reagent – thiosemicarbazide. It is known that the cadmium forms with thiosemicarbazide coordination compounds with variable composition. The molar ratio cadmium: thiosemicarbazide can vary from 1:1 up to 1:3. To establish the optimal conditions for preparation of the thin layers, we have studied the influence on the quality of the nature of the anions from the initial cadmium or zinc salts (chlorides, nitrates, sulfates and etc.), the solvent, total concentration and the molar ratio of the reagents, heat treatment regime (duration and rate of heating of the surface during the process of deposition). A highest quality was achieved when a solution of cadmium nitrate and tiosemicarbazide taken in molar ratio 1:1 has been used in dimethylformamide as solvent. The optimal thermal conditions for deposition of the best layers were found in the temperature range 300-350 °C when was observed an increase of the polycrystalline forms. The technological parameters have a sufficient reproducibility and ensure the property of the prepared films. The layer thickness was varied changing the volume of pulverized solutions, keeping permanent concentration. As a substrate for thin film deposition were used glass, mica and monocrystaline substrates of Si. Technology of deposition of layers allows to range the thickness within (2-20 ) nm. All the layers obtained had resistivity from 1011 – 1012 Ω•cm and were not photosensitive. Heat treatment of short duration in open volume at 350 °C leads to the decrease of the resistivity by 1-2 orders and the layers becoming photosensitive, combined σl / σd , which reached 102 at illumination of 100 Lx. The obtained layers had a high transparency up to 86 % in the wavelength range (0.42 - 0.9) μm. The width of the band gap was calculated from the spectra of transparency and was found approximately 2.45 - 2.49 eV, which corresponds to the width of the band gap of CdS at room temperature. Crystal lattice parameters, determined from diffractgrams show, that the films obtained by spray method have a cubic crystal lattice in the direction (200). It was established that the variation of "x" from 1 to 0.5 in the heterometallic CdxZn1-xS films is accompanied by a shift of the absorption zone to the region of the short wave lengths. Band gap width calculated from the spectra of transparency is in the range (2.45 - 2.96 ) eV and varies when the concentrations of metal ions Zn and Cd in solution ( 1 ≥ x ≥ 0.5 ) varies respectively. The technological parameters are sufficiently reproducible and provide constant properties of the prepared layers.