Synthesis and structure determination<i>via</i>ultra-fast electron diffraction of the new microporous zeolitic germanosilicate ITQ-62

Bieseki, Lindiane; Simancas, Raquel; Jordá, José L.; Bereciartua, Pablo J.; Cantı́n, Ángel; Simancas, Jorge; Pergher, Sibele B. C.; Valencia, Susana; Rey, Fernando; Corma, Avelino

doi:10.1039/c7cc09240g

Cited by 24 publications

(14 citation statements)

References 47 publications

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“…For example, Bieseki et al. have used ultra‐fast 3D electron diffraction tomography to solve the newly synthesized zeolite structure, ITQ‐62 . After refinement using pXRD to analyze the calcined zeolite, the authors confirm the presence of highly distorted 8‐member (tri‐directional channel) and 12‐member (mono‐directional) rings in ITQ‐62.…”

Section: Characterization Of Metal‐zeolite Composite Catalystsmentioning

confidence: 83%

Characterization of Metal‐zeolite Composite Catalysts: Determining the Environment of the Active Phase

et al. 2020

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Metal‐zeolite composite catalysts are attracting increased attention due to their unique multifunctional properties. However, it is challenging to identify the physicochemical environment of the active phase, which is essential to improve our understanding of the structure‐performance relationships of such complex catalysts. In this work, commonly available analytical techniques (FTIR, TEM, XRD, etc.) and state‐of‐the‐art user instrumentation (XAS, SANS, e‐TEM, etc.) are reviewed with respect to their applications at different stages of the catalyst lifetime, from early nucleation, to the reaction mechanism and deactivation. Each technique is discussed in detail with examples to provide suggestions and guidelines for choosing the characterization technique(s) that are most appropriate for determining the desired structure‐property relationships of metal‐zeolite composite catalysts. Understanding the most appropriate applications of characterization techniques promotes development of novel synthesis methodologies, and in turn, applications for designing active, selective and stable multifunctional metal‐zeolite composite catalysts.

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Section: Characterization Of Metal‐zeolite Composite Catalystsmentioning

confidence: 83%

Characterization of Metal‐zeolite Composite Catalysts: Determining the Environment of the Active Phase

et al. 2020

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“…This method of data collection was first proposed in 2013 for studying protein crystals (Nederlof et al, 2013) and it is now known with several acronyms as MicroED (Nannenga et al, 2014), IEDT (Gemmi et al, 2015), cRED (Wang et al, 2017). Continuous rotation data collection has been a second revolution for 3D ED making it possible to perform single-crystal studies on very beam-sensitive compounds that could only be synthesized in nanocrystalline form such as zeolites (Simancas et al, 2016;Bieseki et al, 2018), pharmaceuticals (van Genderen et al, 2016;Jones et al, 2018), organics (Sawaya et al, 2016) and proteins (Nannenga et al, 2014;Yonekura et al, 2015).…”

Section: Continuous Rotation Methods (Cred Microed Iedt)mentioning

confidence: 99%

3D electron diffraction techniques

Gemmi

Lanza

2019

Acta Crystallogr B Struct Sci Cryst Eng Mater

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3D electron diffraction is an emerging technique for the structural analysis of nanocrystals. The challenges that 3D electron diffraction has to face for providing reliable data for structure solution and the different ways of overcoming these challenges are described. The route from zone axis patterns towards 3D electron diffraction techniques such as precession-assisted electron diffraction tomography, rotation electron diffraction and continuous rotation is also discussed. Finally, the advantages of the new hybrid detectors with high sensitivity and fast readout are demonstrated with a proof of concept experiment of continuous rotation electron diffraction on a natrolite nanocrystal.

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“…3D electron diffraction (3DED) and microcrystal electron diffraction (MicroED) have been shown to be powerful techniques for the structure determination of solids, and are especially advantageous for studies of micro-and nanocrystals. So far, hundreds of structures have been determined by 3DED (Gemmi et al, 2019), including zeolites (Jiang et al, 2011;Martínez-Franco et al, 2013;Guo et al, 2015;Simancas et al, 2016;Lee et al, 2018;Bieseki et al, 2018;Zhang et al, 2018;Smeets et al, 2019), metal-organic frameworks (Denysenko et al, 2011;Feyand et al, 2012;Wang, Rhauderwiek et al, 2018;Lenzen et al, 2019), pharmaceuticals Gruene et al, 2018;Jones et al, 2018;Brá zda et al, 2019), proteins (Nannenga et al, 2014;de la Cruz et al, 2017;Xu et al, 2019;Lanza et al, 2019) and many others.…”

Section: Introductionmentioning

confidence: 99%

InsteaDMatic: towards cross-platform automated continuous rotation electron diffraction

Roslova¹,

Smeets²,

Wang³

et al. 2020

J Appl Cryst

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A DigitalMicrograph script, InsteaDMatic, has been developed to facilitate rapid automated 3D electron diffraction/microcrystal electron diffraction data acquisition by continuous rotation of a crystal with a constant speed, denoted as continuous rotation electron diffraction. The script coordinates microscope functions, such as stage rotation, and camera functions relevant for data collection, and stores the experiment metadata. The script is compatible with any microscope that can be controlled by DigitalMicrograph and has been tested on both JEOL and Thermo Fisher Scientific microscopes. A proof of concept has been performed through employing InsteaDMatic for data collection and structure determination of a ZSM-5 zeolite. The influence of illumination settings and electron dose rate on the quality of diffraction data, unit-cell determination and structure solution has been investigated in order to optimize the data acquisition procedure.

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Synthesis and structure determinationviaultra-fast electron diffraction of the new microporous zeolitic germanosilicate ITQ-62

Cited by 24 publications

References 47 publications

Characterization of Metal‐zeolite Composite Catalysts: Determining the Environment of the Active Phase

Characterization of Metal‐zeolite Composite Catalysts: Determining the Environment of the Active Phase

3D electron diffraction techniques

InsteaDMatic: towards cross-platform automated continuous rotation electron diffraction

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