SerialRED’s new method enables rapid, high-throughput phase analysis of polycrystalline materials

On January 31, 2023, Beijing time, Academician Zou Xiaodong of Stockholm University in Sweden (academician of the Royal Swedish Academy of Sciences and the Academy of Engineering) and the team of Academician Yang Weimin of Sinopec Shanghai Petrochemical Research Institute published an article entitled “High-throughput phase elucidation of polycrystalline materials using serial” in the journal Nature Chemistry Rotation electron diffraction”.

This achievement reports the great advantages of the new automated, high-throughput SerialRED method for rapid, high-throughput phase analysis and structural elucidation of complex microcrystalline/nanocrystalline materials. The use of SerialRED will have the potential to change the way important polycrystalline materials such as minerals, metals/metal oxides, ceramics, semiconductors, backbone type materials, small organic molecules, and pharmaceuticals are researched and developed.

The corresponding authors of the paper are Zou Xiaodong and Yang Weimin; The first authors are Luo Yi and Wang Bin.

The application of X-ray diffraction (XRD) technology in phase analysis and structure elucidation of crystalline materials has greatly promoted the development of chemistry, material science, biomedicine and other fields. However, many important crystalline materials are currently at the submicron or nanometer scale, which poses challenges to characterize their phase composition and structure using single crystal/powder XRD technology. The challenge is further increased when the material contains multiphase, trace phase (<1%), similar unit-cell phase, large unit-cell phase, or low-symmetry structural phase. This has become a bottleneck in the development of many polycrystalline materials, especially in high-throughput material synthesis screening. In addition, the difficulty of phase and structure analysis also limits the use of more complex systems to explore the synthesis of new materials. Therefore, there is an urgent need for new technologies that can quickly and reliably analyze the phase composition and structure of complex polycrystalline products.

The new SerialRED method developed based on transmission electron microscopy can automatically and quickly identify hundreds or thousands of submicron or nanocrystals in polycrystalline samples and acquire three-dimensional electron diffraction (3D ED) data for each crystal. This enables SerialRED to enable rapid, high-throughput phase analysis and structural elucidation of complex multiphase nano/submicron crystal samples. In this work, the collaborative team of Academician Zou Xiaodong/Academician Yang Weimin took the synthesis of typical polycrystalline material zeolite as an example to demonstrate the advantages of SerialRED method in assisting the exploration of complex systems to synthesize new materials, quickly obtaining phase composition and structural information, and accelerating material development.

They used multivariate skeleton T atoms ([Si、Ge、Al]or[Si、Ge、B]Combined with simple OSDA to explore synthetic zeolite sieves. A series of highly complex polycrystalline zeolite samples that are difficult to analyze using XRD analyte phases were synthesized by modulating the dosage of multivariate framework T atoms. By using SerialRED, it was successfully identified in a highly complex synthetic mixtureRTH(small holes),*UOE(mesohole),POS(large hole),IWV(large hole) and*CTH(super large pores) five molecular sieve phases. Some of these phases are ultra-low and have similar morphology or unit cell parameters that cannot be detected/determined by XRD or even traditional 3D ED techniques. According to the obtained reliable phase and structure information, the role of different skeleton T atoms in inducing the formation of different zeolite structures in the constructed synthetic system is revealed, which provides opportunities for the design, synthesis and rapid development of zeolite materials. Through the construction of complex synthesis system, simple and inexpensive OSDA can replace complex and expensive OSDA synthesisSFEIWVand*CTHMacroporous/extra-porous molecular sieve.

Because highly complex polycrystalline hybrid samples can be analyzed, SerialRED provides new opportunities to expand the scope of synthetic chemistry and explore more complex systems to synthesize new polycrystalline materials. Because no pure phase samples are required for phase analysis and structure elucidation, SerialRED is able to detect valuable crystal phases and determine their structure at an early stage of synthesis development, which provides new opportunities for the design, synthesis and rapid development of new polycrystalline materials. At the same time, when the number of detected crystals is sufficient, SerialRED can quantify the phase composition. In addition, SerialRED experiments require only a small amount of sample, which can be combined with nanomolar high-throughput synthetic screening techniques to accelerate material development. These unique capabilities of SerialRED will have the potential to change the way important materials such as minerals, metals/metal oxides, ceramics, semiconductors, organic small molecules, and pharmaceuticals are researched and developed. (Source: Science Network)

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