High-throughput phase elucidation using SerialRED: new opportunities for rapid materials development
Researchers at Stockholm University and Sinopec Shanghai Research Institute of Petrochemical Technology have demonstrated the high-throughput phase elucidation of highly complex polycrystalline zeolite materials using the automated serial rotation electron diffraction (SerialRED) method. Using SerialRED, five zeolite phases have been identified from a highly complex synthesized mixture.
This includes phases with ultra-low contents or similar unit cell parameters that are unable to be identified using the conventional X-ray diffraction (XRD) methods. SerialRED provides new opportunities for the exploration of complex materials synthesis systems and the rapid development of polycrystalline materials. The results are published in the scientific journal Nature Chemistry.
Rapid phase elucidation of polycrystalline materials is essential for developing new materials of chemical, pharmaceutical and industrial interest. XRD, since its first discovery over a century ago, has been well-established for phase analysis and structure determination. Yet, the size and quantity of many crystalline phases are too small for routine single-crystal/powder X-ray diffraction (SCXRD/PXRD) analysis. This has become a workflow bottleneck in modern materials development, especially in high-throughput synthesis screening. There is a great demand for new techniques that can unravel the phase compositions and atomic structures reliably at an early stage in the design of novel materials.
The automated SerialRED method, which can automatically screen crystals and collect 3D ED data from hundreds of nanometre- or submicrometre-sized crystals in a product, combines phase analysis and structure determination in a single method. Combined with hierarchical cluster analysis, SerialRED enables objective, high-throughput phase analysis and structure determination of complex polycrystalline products.
Using a real example in zeolite materials development, the benefit of SerialRED in characterizing and developing polycrystalline materials has been demonstrated. SerialRED is able to rapidly and reliably elucidate the phase and atomic structural information of highly complex polycrystalline materials, which contain multiple phases, phases with ultra-low contents (<1%), phases with similar unit cell parameters and/or phases with complex structures.
Being able to characterize complex polycrystalline materials in ways where the conventional XRD methods fall short, SerialRED can accelerate the design and development of novel materials by rapidly identifying interesting phases at an early stage of materials development. It also enables exploration of more complex materials synthesis systems, which expands the scope of synthetic chemistry in discovery of interesting polycrystalline materials. In addition, SerialRED experiments are performed on a trace amount of sample, which is desirable for nanomole-scale high-throughput synthesis screening. All these indicating SerialRED may greatly change our way in the innovation of a wide range of polycrystalline materials, from minerals, metal/metal oxides, ceramics, semiconductors to organic and pharmaceutical compounds.
Last updated: January 30, 2023
Source: MMK