High-Throughput Continuous Hydrothermal Synthesis of Nanomaterials (Part II): Unveiling the As-Prepared CexZryYzO2−δ Phase Diagram

High-throughput continuous hydrothermal flow synthesis was used to manufacture 66 unique nanostructured oxide samples in the Ce–Zr–Y–O system. This synthesis approach resulted in a significant increase in throughput compared to that of conventional batch or continuous hydrothermal synthesis methods. The as-prepared library samples were placed into a wellplate for both automated high-throughput powder X-ray diffraction and Raman spectroscopy data collection, which allowed comprehensive structural characterization and phase mapping. The data suggested that a continuous cubic-like phase field connects all three Ce–Zr–O, Ce–Y–O, and Y–Zr–O binary systems together with a smooth and steady transition between the structures of neighboring compositions. The continuous hydrothermal process led to as-prepared crystallite sizes in the range of 2–7 nm (as determined by using the Scherrer equation).