Materials Chemistry

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

Authors

  • Yi Luo Department of Materials and Environmental Chemistry, Stockholm University, SE-106 91 Stockholm, Sweden. ,
  • Bin Wang Department of Materials and Environmental Chemistry, Stockholm University, SE-106 91 Stockholm, Sweden. ,
  • Stef Smeets Netherlands eScience Center, Science Park 140, 1098 XG Amsterdam, The Netherlands ,
  • Junliang Sun College of Chemistry and Molecular Engineering, Beijing National Laboratory for Molecular Sciences, Peking University, Beijing 100871, China. ,
  • Weimin Yang State Key Laboratory of Green Chemical Engineering and Industrial Catalysis, Sinopec Shanghai Research Institute of Petrochemical Technology, 1658 Pudong Beilu, Shanghai 201208, China. ,
  • Xiaodong Zou Department of Materials and Environmental Chemistry, Stockholm University, SE-106 91 Stockholm, Sweden.

Abstract

Rapidly and reliably elucidating the phases in polycrystalline materials is essential for developing new materials. Yet, crystals of many materials of biological, pharmaceutical, chemical, or industrial interest are too small (<1 μm) for routine X-ray diffraction (XRD) analysis. For complex materials, this can result in workflow bottlenecks in high-throughput synthesis screenings favoured by industrial laboratories. With the increased prevalence of electron diffraction as an alternative technique for materials characterization, we explore a series of zeolite syntheses, resulting in typical 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 XRD could not handle. It allows the exploration of more complex synthesis systems and provides new opportunities for rapidly developing novel polycrystalline materials, greatly benefiting synthesis chemistry and material science.

Content

Thumbnail image of manuscript.pdf

Supplementary material

Thumbnail image of Supporting_information.pdf
Supporting_information.pdf
The supporting information includes the methods of synthesis, characterization, and catalytic reaction. The supplementary figures and tables are also presented.
Thumbnail image of CTH_Product_A_SerialRED.cif
CTH_Product_A_SerialRED.cif
The SerialRED structure of CTH phase in Product A.
Thumbnail image of IWV_Product_A_SerialRED.cif
IWV_Product_A_SerialRED.cif
The SerialRED structure of IWV phase in Product A.
Thumbnail image of RTH_Product_A_SerialRED.cif
RTH_Product_A_SerialRED.cif
The SerialRED structure of RTH phase in Product A.
Thumbnail image of CTH_Product_B_SPXRD.cif
CTH_Product_B_SPXRD.cif
The synchrotron powder X-ray diffraction (SPXRD) structure of CTH phase in Product B.
Thumbnail image of IWV_Product_B_SPXRD.cif
IWV_Product_B_SPXRD.cif
The synchrotron powder X-ray diffraction (SPXRD) structure of IWV phase in Product B.