Automated & high-throughput electron diffraction techniques for dev. of novel nanoporous materials

Описание: Automated and high-throughput electron diffraction techniques for the development of novel nanoporous materials

Nanoporous materials such as zeolites, metal-organic frameworks (MOFs) and covalent organic frameworks (COFs) have a wide range of applications in catalysis, storage and separation. This is because these materials have uniform pore sizes, large surface areas, and adjustable chemical functionality. In order to understand the functions of these materials and develop new porous materials, it is essential to know their 3D atomic structures. However, many zeolites, MOFs and COFs are synthesized as polycrystalline materials and multiphasic mixtures, which are too difficult to be studied by conventional single crystal and powder X-ray diffraction. During the past decade, various new electron crystallographic techniques, i.e. three-dimensional electron diffraction (3D ED) and serial electron diffraction (SerialED) have bene developed for studying such materials, which have made important breakthroughs in the development of nanoporous materials [1-2].

In this talk, I will present the 3D ED and SerialED techniques developed in my group and demonstrate their applications for structure characterization of novel nanoporous materials [3-5]. Today, the structure determination of zeolites, MOFs and COFs by 3D ED is as feasible and accurate as that by single crystal X-ray diffraction. A complete 3D ED dataset can be obtained in less than a minute on a standard TEM [6]. The refined structural models can reach better than 0.05 Å in accuracy for all non-H atoms and in many cases H-atoms could also be located. Detailed structural features such as disorders and linker motions in MOFs could by identified [7]. To further speed up and automate data collection, we have developed high-throughput automated data collection and data analysis for 3D electron diffraction [5]. SerialED makes it possible not only for studying extremely beam-sensitive crystals, but also for phase analysis and for detection of minor phases invisible by X-ray diffraction [8]. The developments of new 3D ED and SerialED techniques have revolutionized crystallography, and provided new opportunities for discovering novel structures and new materials, and exploring their properties and applications.

References:
[1] Z. Huang, T. Willhammar, X. Zou, Chem. Sci. 2021, 12, 1206.
[2] Z. Huang, E. S. Grape, J. Li, A. K. Inge, X. Zou, Coord. Chem. Rev. 2021, 427, 213583.
[3] W. Wan, J.L. Sun, J. Su, S. Hovmoller, X Zou, J. Appl. Cryst. 2013, 46, 1863.
[4] S. Smeets, X. Zou, W. Wan, J. Appl. Cryst. 2018, 51, 1262.
[5] B. Wang, X, Zou, and S. Smeets, IUCrJ, 2019, 6, 854.
[6] T. Yang, T. Willhammar, H. Xu, X. Zou, Z. Huang, Nat. Protocol. 2022, 17, 2389-2413.
[7] L. Samperisi, A. Jaworski, G. Kaur, K.P. Lillerud, X. Zou, Z. Huang, J. Am. Chem. Soc. 2021, 143, 17947.
[8] Y. Luo, B. Wang, S. Smeets, J. Sun, W. Yang, X. Zou, ChemRxiv, 2021, doi: 10.33774/chemrxiv-2021-34v44.