Barium zirconium trisulfide (BZS) is a three-dimensional (3D) perovskite with optoelectronic properties suitable for photovoltaic (PV) and light-emitting diode (LED) applications that is conventionally reported in the orthorhombic (62) symmetry. Synchrotron X-ray diffraction, thermal analysis, and Raman and absorption spectroscopy revealed three high-temperature polymorphs that appear when BZS is heated in air prior to complete oxidation (BaZrS + 5O → BaSO + ZrO + 2SO↑) at 700 °C with the approximate stability ranges: BaZrS IV (62)T < 400 °CBaZrS III (63)400 °C ≤ T ≤ 500 °CBaZrS II14/ (140)500 °C ≤ T ≤ 700 °CDifferential scanning calorimetry (DSC) revealed exothermic features accompanying the IV → III and III → II phase changes. Furthermore, the direct band gap varied inversely with temperature with distinct energies for each polymorph (1.84 eV ≤ IV ≤ 1.65 eV; 1.65 eV ≤ III ≤ 1.54 eV; 1.54 eV ≤ II ≤ 1.52 eV). Raman spectroscopy found that polymorphic changes up to 600 °C were reversible with bands characteristic of BaZrS IV entirely restored upon cooling to room temperature (RT). This more complete understanding of BSZ polymorphism provides a basis for producing crystallochemical variants with enhanced optoelectronic properties under ambient conditions.
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