Exploring Polycrystalline Materials: High-throughput Phase Elucidation Using Serial Rotation Electron Diffraction

Abstract Rapidly and reliably elucidating the phases in polycrystalline materials is essential for developing new materials. Yet, crystals of many materials of chemical, pharmaceutical, or industrial interest are too small for routine X-ray diffraction analysis. This can be workflow bottlenecks in material development, especially in high-throughput synthesis screenings. With the increased prevalence of electron diffraction, we explore a series of zeolite syntheses, resulting in polycrystalline products, via high-throughput phase identification using serial rotation electron diffraction (SerialRED). Five zeolite phases were identified in one product, the most complex mixture ever discovered in zeolite chemistry. Some of the phases are of ultra-low contents, similar unit cells, and/or identical morphologies. Via automatically examining hundreds of crystals, SerialRED enables the reliable and high-throughput phase analysis of products that X-ray diffraction cannot handle. It allows the exploration of more complex synthesis systems and provides new opportunities for rapidly developing novel materials, greatly benefiting synthesis chemistry and material science.