Synthesis and crystal structures are described for the Bi 1−x Sb 1−x Te 2x O 4 solid solution with 0 ≤ x ≤ 0.1. It crystallizes in the monoclinic system, space group I2/c. Rietveld refinements of X-ray powder diffraction data indicate that the atomic positions are: Bi/Te (2) (4c), Sb/Te (1) (4d). The oxygen occupied two sites, 8f and 8b, respectively. The reliability factors are: R p = 7.45%, R wp = 10.6% and R b = 3.88% for x = 0.1. The structure contains [(Sb/Te (1))O 4 ] n layers formed by (Sb/Te (1))O 6 octahedra sharing corners, which are parallel to (001) plan and held together by bismuth and tellurium atoms. The Raman study of this solid solution shows the bands which are assigned to O-Bi 3+-O, O-Sb 5+-O and connects (Bi/Te (2))O 8-(Sb/Te (1))O 6 vibration in the crystal.
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