Rapid Identification of Synthetic Routes to Functional Metastable Phases Using X-Ray Probed Laser Anneal Mapping (XPLAM) Time-Temperature Quench Maps
Robert T. Bell, Peter A. Beaucage, Marc J. Murphy, Aine Connolly, David Ginley, Ulrich Wiesner, R. B. Van Dover, Michael O. Thompson
Most material systems have known or predicted functional phases that are metastable at standard temperature and pressure. While substantial advances have been made in the high-throughput and combinatorial synthesis of materials with a range of stoichiometries, investigation of thermal processing remains largely the domain of iterative uniform anneals. Here we develop X-ray probed laser anneal mapping (XPLAM), a high throughput technique coupling spatially resolved X-ray diffraction with microsecond to millisecond laser gradient anneals to produce temperature-dwell-transformation (TDT) diagrams of phase as a function of quench time and temperature. In addition to showing regimes where specific metastable phases nucleate preferentially, TDT diagrams provide insight into the sub- millisecond kinetics of solid-solid phase transitions. As a first demonstration of XPLAM, we study Bi2O3, which has a rich set of polytypes, including the δ-phase with the exceptionally high oxygen ion conductivity. We demonstrate the first annealing-driven synthesis of room temperature δ-Bi2O3. We expect XPLAM to prove a powerful technique for rapid identification of synthetic routes to metastable phases, and to generate the exhaustive datasets required for machine learning-guided exploration of materials processing.
, Beaucage, P.
, Murphy, M.
, Connolly, A.
, Ginley, D.
, Wiesner, U.
, Van, R.
and Thompson, M.
Rapid Identification of Synthetic Routes to Functional Metastable Phases Using X-Ray Probed Laser Anneal Mapping (XPLAM) Time-Temperature Quench Maps, Chemistry of Materials, [online], https://doi.org/10.1021/acs.chemmater.0c04926, https://tsapps.nist.gov/publication/get_pdf.cfm?pub_id=931076
(Accessed December 9, 2023)