4.0 Article

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

Journal

ACS COMBINATORIAL SCIENCE
Volume 15, Issue 9, Pages 458-463

Publisher

AMER CHEMICAL SOC
DOI: 10.1021/co3001346

Keywords

high-throughput; hydrothermal synthesis; phase diagram; Raman spectroscopy; X-ray diffraction

Funding

  1. EPSRC [EP/E040551/1]
  2. Zhejiang Provincial Natural Science Foundation of China [LQ12E08011]
  3. National Natural Science Fundation of China [51208458]
  4. EPSRC [EP/D038499/2, EP/E040551/1] Funding Source: UKRI
  5. Engineering and Physical Sciences Research Council [EP/D038499/2, EP/E040551/1] Funding Source: researchfish

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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).

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