Alkaline earth (AE) metals are irreplaceable ingredients in the synthesis of AE metal-based antiperovskite oxides, and it can be achieved by a chemical reduction of a stable AE metal compound. In this study, hydrogen and carbothermal reduction of BaO and BaCO3 were attempted, and we here report an undesirable side reaction creating barium hydroxide (Ba(OH)2) as the product of the reaction with the small amount of water in ultra-high purity inert gas used in the reduction processes. Such side reaction pathways and products are hardly identifiable in a high-temperature reaction; yet, systematic investigations on phase evolutions using X-ray diffraction, IR spectroscopy, and thermogravimetric analysis enabled the detection of Ba(OH)2·xH2O. Unintentional creation of alkaline earth metal oxides in intermediate and subsequent hydration even under a negligible amount of H2O may lead to an unexpected loss of alkaline earth metal element and, consequently, its deficiency in a desired final product.
Read full abstract