![]() Three scenarios, based on Rietveld refinement analysis, were considered for the description of the crystal structure evolution from β- to α-modification, including the (3+3)D-modulated cubic structure at 693 K as an intermediate state during the β–α transformation. These observations, together with a clear endothermic peak in the heat capacity, the magnitude of enthalpy/entropy change and the temperature dependence of electrical resistivity (associated with hysteresis), hinted towards the 1st order type of transition. A high temperature PXRD study revealed both abrupt (in full widths at half maxima of main reflections and in unit-cell volume) and gradual (in intensity of satellites and c/ a ratio) changes in the vicinity of the α–β phase transition. Combining single-crystal XRD, transmission electron microscopy and selected-area electron diffraction studies, the presence of three twin domains in the as-grown crystals was confirmed. High-resolution powder X-ray diffraction (PXRD) experiments at 80 K enabled the observation of split tetragonal reflections (completely overlapped at room temperature), which prove the correctness of the crystal structure model accepted for the β-polymorph. All synthesized samples contained β-In 0.67□ 0.33In 2S 4 modification only, independent of the synthesis procedure. Poly- and single-crystalline samples of In 0.67□ 0.33In 2S 4 thiospinel were obtained by various powder metallurgical and chemical vapor transport methods, respectively. The Rossendorf Beamline BM20, European Synchrotron Radiation Facility, 71, avenue des Martyrs, 38043 Grenoble, FranceĮxperimental Physics VI, Center for Electronic Correlations and Magnetism, Institute of Physics, University of Augsburg, 86135 Augsburg, Germany Institute of Resource Ecology, Helmholtz-Zentrum Dresden-Rossendorf, Bautzner Landstraße 400, 01328 Dresden, Germany Institut für Anorganische Chemie, TU Bergakademie Freiberg, Leipziger Straße 29, 09599 Freiberg, Germany Institute for Ion Beam Physics and Materials Research, Helmholtz-Zentrum Dresden-Rossendorf, Bautzner Landstraße 400, 01328 Dresden, Germany Ivan Franko National University of Lviv, Kyryla and Mefodiya Str. ![]() Institut für Experimentelle Physik, TU Bergakademie Freiberg, Leipziger Straße 23, 09599 Freiberg, GermanyĮ-mail: für Chemische Physik fester Stoffe, Nöthnitzer Straße 40, 01187 Dresden, Germany ![]()
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