A high throughput synthetic workflow for solid state synthesis of oxides.

Area of Science:

• Materials Science
• Inorganic Chemistry
• Chemical Engineering

Background:

• High-throughput synthesis is established for liquid/vapor reagents but challenging for solid-state reactions in functional and electroceramics industries.
• Automating sub-solidus reaction pathways, crucial for materials industries, is difficult due to solid-state reagent use.

Purpose of the Study:

• To develop a high-throughput sub-solidus synthesis workflow for rapid screening of oxide chemical space.
• To accelerate materials discovery by expanding explored compositions and synthetic conditions simultaneously.
• To demonstrate the workflow's applicability to polyanion-based compositions beyond simple oxides.

Main Methods:

• A hybrid approach combining manual, multi-sample actions with researcher-hands-free automated processes.
• Implementation of a sub-solidus reaction pathway for solid-state reagent synthesis.
• Application to extend known solid solutions and explore new composition spaces.

Main Results:

• Successfully extended the BaYSnO solid solution beyond its reported limit to a new composition.
• Explored the Nb-Al-P-O composition space, demonstrating applicability to polyanion systems.
• Achieved increased throughput by processing multiple samples concurrently.

Conclusions:

• The developed workflow significantly accelerates materials discovery in oxide and polyanion systems.
• The hybrid manual-automated approach overcomes automation challenges in solid-state synthesis.
• This method enables rapid screening of vast chemical spaces for novel functional materials.