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Abstract Bismuth telluride and its derivative selenide compounds are extremely interesting semiconductors due to their technological importance. The fabrication devices with alloys of these compounds, possessing thermoelectric generators have been an important and recent technological development. Therefore, thin films of new compounds Bi2(SexTe1-x)3 where 0 ≤ x ≤ 1, has been chosen as the subject of this work. Stoichiometric bulk ingot materials of Bi2(SexTe1-x)3 where 0 ≤ x ≤ 1 were prepared by Bridgman technique in vacuum-sealed silica tubes. X-ray diffractometry has revealed that the prepared ingot materials with indicated compositions are single –phase polycrystalline materials corresponding to the rhombohedral type structure. The elemental analysis (EDAX) of the ingot materials indicated that they are nearly stoichiometric. The lattice parameters were determined. Nearly stoichiometric thin films of Bi2(SexTe1-x)3 with different compositions were deposited on either glass or KBr discs as substrates by thermally evaporating method. The structural properties of the as-deposited and annealed films under vacuum at 373, 423, 473K for 2 hours were studied by X-ray diffractometry (XRD) and transmission and scanning electron microscopy. These studies confirmed that as-deposited and annealed films at 373K with different compositions were amorphous but for annealed films at 423, 473K were polycrystalline with rhombohedral structure as that of the bulk material with (015) predominant reflecting plane . Moreover, the grain size, microstrain, dislocation density and the number of crystallites were calculated. |