High-throughput phase elucidation of polycrystalline materials using serial rotation electron diffraction

Rapid phase elucidation of polycrystalline materials is essential for developing new materials of chemical, pharmaceutical and industrial interest. Yet, the size and quantity of many crystalline phases are too small for routine X-ray diffraction analysis. This has become a workflow bottleneck in materials development, especially in high-throughput synthesis screening. Here we demonstrate the application of serial rotation electron diffraction (SerialRED) for high-throughput phase identification of complex polycrystalline zeolite products. The products were prepared from a combination of multiple framework T atoms ([Si,Ge,Al] or [Si,Ge,B]) and a simple organic structure-directing agent. We show that using SerialRED, five zeolite phases can be identified from a highly complex mixture. This includes phases with ultra-low contents undetectable using X-ray diffraction and phases with identical crystal morphology and similar unit cell parameters. By automatically and rapidly examining hundreds of crystals, SerialRED enables high-throughput phase analysis and allows the exploration of complex synthesis systems. It provides new opportunities for rapid development of polycrystalline materials.

Automated summary

Rapid phase elucidation is crucial in the development of new materials. However, routine X-ray diffraction analysis is often limited by the small size and quantity of crystalline phases. In this study, we demonstrate the use of SerialRED for high-throughput phase identification of complex polycrystalline zeolite products. By automating the analysis of hundreds of crystals, SerialRED enables the identification of zeolite phases that are undetectable using X-ray diffraction, providing new opportunities for rapid development of polycrystalline materials.