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Development of serial crystallography methods for structure solution of polycrystalline materials using electron diffraction

Applicant Smeets Stef
Number 165282
Funding scheme Early Postdoc.Mobility
Research institution Department of Materials and Environmental Chemistry Stockholm University
Institution of higher education Institution abroad - IACH
Main discipline Material Sciences
Start/End 01.01.2016 - 30.06.2017
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Keywords (6)

Structure determination; Serial crystallography; Electron diffraction; Microporous materials; Zeolites; Polycrystalline materials

Lay Summary (German)

Lead
Viele industriell und kommerziell wichtige Materialien, wie Katalysatoren, Pharmazeutika, Mineralien oder Halbleiter werden in polykristalliner Form synthetisiert und eingesetzt. Die Kenntnis der Anordnung der Atome in einem Material (die sogenannte Kristallstruktur) ist der Schlüssel für das Verständnis der chemischen und vor allem auch der physikalischen Eigenschaften dieser Materialien. Dies ermöglicht es dann auch, diese Eigenschaften durch gezielte Änderungen der Kristallstruktur zu verbessern. Es ist daher wichtig, Methoden zu entwickeln um solche Strukturen zu bestimmen. Die Kristallstrukturbestimmung von einem polykristallinen Material ist indes keine triviale Aufgabe und das Interesse an Methoden, mit denen die immer komplizierteren Materialien und deren Strukturen untersucht werden können, ist dementsprechend hoch.
Lay summary

Das Ziel dieses Projektes ist es, einen neuen Ansatz zu entwickeln, der es möglich macht, die Kristallstrukturen von komplexen polykristallinen Materialien zu bestimmen, insbesondere von solchen, die nur wenige Nanometer grosse Kristallen aufweisen. Alle Untersuchungsmethoden basieren auf Experimenten mit Röntgen- oder Elektronenstrahlen und die Strahlungsempfindlichkeit der Proben stellt bei den bestehenden Methoden ein grosses Problem dar. Die "Serial Snapshot Crystallography" wurde entwickelt um die Strukturen von komplizierten Proteinen mit den modernen Röntgenlaser zu lösen. Mit dieser Technik werden Beugungsbilder aus einer Vielzahl Kristallen zu einem einzigen Datensatz kombiniert. Diese Idee soll nun übertragen werden auf das Sammeln von dreidimensionalen Elektronenbeugungsdaten mit einem Elektronenmikroskop. Dies wird es möglich machen, nützliche Daten von Kristallen zu sammeln, die normalweise empfindlich gegenüber den Elektronenstrahlen sind. In diesen Fällen ist es sehr schwierig diese Materialien mit konventionellen Methoden, die auf langen Belichtungszeiten beruhen, zu studieren. Bei der neuen Methode werden viele Kristalle nur einmal kurz dem Strahl ausgesetzt und die Messung ist abgeschlossen, bevor der einzelne Kristall beschädigt oder zerstört ist.

Direct link to Lay Summary Last update: 14.12.2015

Responsible applicant and co-applicants

Publications

Publication
High-throughput continuous rotation electron diffraction data acquisition via software automation
Cichocka Magdalena Ola, Ångström Jonas, Wang Bin, Zou Xiaodong, Smeets Stef (2018), High-throughput continuous rotation electron diffraction data acquisition via software automation, in Journal of Applied Crystallography, 51(6), 1652-1661.
Insights into the Chemistry of Organic Structure-Directing Agents in the Synthesis of Zeolitic Materials
Smeets Stef, McCusker Lynne B. (2018), Insights into the Chemistry of Organic Structure-Directing Agents in the Synthesis of Zeolitic Materials, Springer International Publishing, Cham.
Insights into the Chemistry of Organic Structure-Directing Agents in the Synthesis of Zeolitic Materials
Smeets Stef, McCusker Lynne B. (2018), Insights into the Chemistry of Organic Structure-Directing Agents in the Synthesis of Zeolitic Materials, Springer International Publishing, Cham.
Multidimensional Disorder in Zeolite IM-18 Revealed by Combining Transmission Electron Microscopy and X-ray Powder Diffraction Analyses
Cichocka Magdalena O., Lorgouilloux Yannick, Smeets Stef, Su Jie, Wan Wei, Caullet Philippe, Bats Nicolas, McCusker Lynne B., Paillaud Jean-Louis, Zou Xiaodong (2018), Multidimensional Disorder in Zeolite IM-18 Revealed by Combining Transmission Electron Microscopy and X-ray Powder Diffraction Analyses, in Crystal Growth & Design, 18(4), 2441-2451.
Synthesis and Structure Determination of Large-Pore Zeolite SCM-14
Luo Yi, Smeets Stef, Peng Fei, Etman Ahmed S., Wang Zhendong, Sun Junliang, Yang Weimin (2017), Synthesis and Structure Determination of Large-Pore Zeolite SCM-14, in Chemistry - A European Journal, 23(66), 16829-16834.
Well-Defined Silanols in the Structure of the Calcined High-Silica Zeolite SSZ-70: New Understanding of a Successful Catalytic Material
Smeets Stef, Berkson Zachariah J., Xie Dan, Zones Stacey I., Wan Wei, Zou Xiaodong, Hsieh Ming-Feng, Chmelka Bradley F., McCusker Lynne B., Baerlocher Christian (2017), Well-Defined Silanols in the Structure of the Calcined High-Silica Zeolite SSZ-70: New Understanding of a Successful Catalytic Material, in Journal of the American Chemical Society, 139(46), 16803-16812.
Serial electron crystallography: merging diffraction data through rank aggregation
Smeets Stef, Wan Wei (2017), Serial electron crystallography: merging diffraction data through rank aggregation, in Journal of Applied Crystallography, 50(3), 885-892.
Zeolite Structures
Smeets Stef, Zou Xiaodong (2017), Zeolite Structures, in Nachtigall Petr, Morris Russel, Čejka Jiří (ed.), Royal Society of Chemistry, London (UK), 37-72.
Locating Organic Guests in Inorganic Host Materials from X-ray Powder Diffraction Data
Smeets Stef, McCusker Lynne B., Baerlocher Christian, Elomari Saleh, Xie Dan, Zones Stacey I. (2016), Locating Organic Guests in Inorganic Host Materials from X-ray Powder Diffraction Data, in J. Am. Chem. Soc., 138(22), 7099-7106.
Synthesis and Characterization of CIT-13, a Germanosilicate Molecular Sieve with Extra-Large Pore Openings
Kang J.H., Xie D., Zones S.I., Smeets S., McCusker L.B., Davis M.E. (2016), Synthesis and Characterization of CIT-13, a Germanosilicate Molecular Sieve with Extra-Large Pore Openings, in Chemistry of Materials, 28(17), 6250-6259.

Scientific events

Active participation

Title Type of contribution Title of article or contribution Date Place Persons involved
Meeting of the Dutch Crystallographic Society (NVK-2017) Talk given at a conference Serial electron diffraction for phase analysis and structure deter- mination of polycrystalline materials 03.11.2017 Oss, Netherlands Smeets Stef;
Meeting of the Swiss Crystallographic Society (SGK-2017) Talk given at a conference Structure analysis of polycrystalline materials using X-rays and electrons 21.09.2017 Geneva, Switzerland Smeets Stef;
Meeting of the International Union for Crystallography (IUCr2017) Talk given at a conference Serial electron diffraction for phase analysis and structure determination 21.08.2017 Hyderabad, India Smeets Stef;
7th International FEZA conference (FEZA2017) Talk given at a conference Characterization of zeolite structures using X-ray powder diffraction: framework structures, heteroatoms, and structure-directing agents 03.07.2017 Sofia, Bulgaria Smeets Stef;
Inorganic days Talk given at a conference The structure of zeolite SSZ-70 through combined HRTEM, XRPD, and DNP-enhanced 2D NMR 12.06.2017 Nynashamn, Sweden Smeets Stef;
Debye-Rietveld Symposium Poster Locating organic guests in inorganic host materials from X-ray powder diffraction data 22.09.2016 Amsterdam, Netherlands Smeets Stef;
European Crystallographic Meeting (ECM-30) Talk given at a conference Serial snapshot crystallography using electron diffraction 28.08.2016 Basel, Switzerland Smeets Stef;
European Powder Diffraction Conference (EPDIC-15) Poster Locating organic guests in inorganic host materials from X-ray powder diffraction data 12.06.2016 Bari, Italy Smeets Stef;


Awards

Title Year
EPDIC Award for Young Scientists for outstanding scientific achievement in the field of powder diffraction (http://epdic.ing.unitn.it/html/epdic_awards) 2018
7th FEZA PhD prize for the highest quality zeolite-related publications 2017
Swiss Society for Crystallography PhD prize for the best thesis in crystallography 2017
ETH medal for outstanding thesis (top 8%) 2016

Use-inspired outputs

Software

Name Year
Instamatic 2017


Associated projects

Number Title Start Funding scheme
177761 Development of serial electron crystallography methodology for quantitative phase analysis 01.01.2018 Advanced Postdoc.Mobility

Abstract

Many industrially and commercially important materials, such as catalysts, pharmaceuticals, minerals, and semiconductors, are synthesized and used in polycrystalline form. Understanding the regular arrangement of atoms within the crystal structure is key to understanding why and how these materials function, and to improve on the structural characteristics that make them useful. It is therefore essential to develop methods that allow their structures to be unraveled and studied. Structure determination of a polycrystalline material is not a trivial task, so interest in methods that can handle increasingly complicated materials and structures is high. The purpose of this project is to develop a new approach to determine the crystal structures of complex polycrystalline materials, particularly those that only form nano-sized crystals and are sensitive to radiation damage. This will be done by taking the idea of serial snapshot crystallography, an approach that is being developed for data collection on micro-crystals of materials and macromolecules with X-ray free electron lasers, and bringing it to the electron microscope as an alternative strategy for the collection of 3-dimensional electron diffraction data. With this technique, diffraction patterns from a large number of individual crystals are combined into a single data set. This will enable useful data to be collected on materials that are sensitive to the electron beam, and thus difficult to measure using the conventional methods that require long exposure of the same crystal. Crystals are exposed to the beam only once, and therefore the problem of beam damage is avoided.Therefore, the question that is central to this project is: Can the serial crystallography method be applied to collect a useful data set using electron diffraction techniques? This involves the development of a strategy to collect data from a large number of randomly oriented nano- or micro-crystals, algorithms to combine these data into a single 3-dimensional ED data set, and testing whether the resulting data set can be used for structure determination of materials that are sensitive to radiation damage. The new method will be applied for studying zeolites and metal-organic frameworks with unknown structures.
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