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A series of solid solutions in the system (GaxIn1−x)2(SexTe1−x)3, 1 ≥ x ≥ 0, were prepared by direct synthesis from α-Ga2Se3 and α-In2Te3. The samples (powders and single crystals) were examined at room temperature by X-ray diffraction. In the whole range of concentrations cubic phases of defect zinc-blende types (ZB) are present. The unit-cell parameter, aZB, continuously increases with the In2Te3 content, undergoing an abrupt change at x ≃0.5. In the Ga2Se3-rich region the diffraction lines show complex profiles, similar to the ones of α-Ga2Se3 and of (GaxIn1−x)2Se3 in the Ga-rich region. In the In2Te3-rich region the diffraction pattern is similar to that of the disordered, β, phase of In2Te3. In a narrow range from x≃0.6 to x≃0.5 a two-phase region of these phases exists. For small values of x a superstructure appears, with the unit-cell parameter 3aZB, isostructural with the ordered, α, phase of In2Te3(F{\bar 4}3m). The JCPDS Diffraction File No. for α-In2Te3 is 33-1488.
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