A high throughput synthetic workflow for solid state synthesis of oxides

• Published in: Chemical science (Cambridge) 2024-02, Vol.15 (7), p.264-2647
• Main Authors: Hampson, Christopher J, Smith, Moli P, Arciero, Luca L, Collins, Christopher M, Daniels, Luke M, Manning, Troy D, Gaultois, Michael W, Claridge, John B, Rosseinsky, Matthew J
• Format: Article
• Language: English
• Subjects: Chemistry; Composition; Inorganic materials; Polyelectrolytes; Reagents; Solid solutions; Solid state; Solidus; Synthesis; Workflow
• ISSN: 2041-6520; 2041-6539
• DOI: 10.1039/d3sc05688k

High-throughput synthetic methods are well-established for chemistries involving liquid- or vapour-phase reagents and have been harnessed to prepare arrays of inorganic materials. The versatile but labour-intensive sub-solidus reaction pathway that is the backbone of the functional and electroceramics materials industries has proved more challenging to automate because of the use of solid-state reagents. We present a high-throughput sub-solidus synthesis workflow that permits rapid screening of oxide chemical space that will accelerate materials discovery by enabling simultaneous expansion of explored compositions and synthetic conditions. This increases throughput by using manual steps where actions are undertaken on multiple, rather than individual, samples which are then further combined with researcher-hands-free automated processes. We exemplify this by extending the BaY x Sn 1− x O 3− x /2 solid solution beyond the reported limit to a previously unreported composition and by exploring the Nb-Al-P-O composition space showing the applicability of the workflow to polyanion-based compositions beyond oxides. A slurry based solid-state high-throughput workflow provides sample forms suitable for presenting to automated characterisation for the discovery of new oxide materials.