Ptychographic measurements of varying size and shape along zeolite channels

Sha, Haozhi; Cui, Jizhe; Li, Jialu; Zhang, Yuxuan; Yang, Wenyuan; Li, Yadong; Yu, Rong

doi:10.1126/sciadv.adf1151

Cited by 15 publications

(13 citation statements)

References 80 publications

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“…The advantages of 4D-STEM ptychography were clearly demonstrated in recent studies on zeolite and MOF structures. ,− For example, Zhang et al acquired 4D-STEM data for zeolites using relatively low electron doses (3000–4000 e – /Å 2 ) and performed ptychography reconstruction using an iterative algorithm that incorporated the multislice method . The reconstructed ptychographic image displays subangstrom resolution (∼0.85 Å), surpassing that of the iDPC-STEM image (Figure a,b), and it exhibits a perfect match with the projected structural model (Figure c).…”

Section: Discussionmentioning

confidence: 92%

Applications of Transmission Electron Microscopy in Phase Engineering of Nanomaterials

Li,

Zhang,

Han

2023

Chem. Rev.

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Section: Discussionmentioning

confidence: 92%

Applications of Transmission Electron Microscopy in Phase Engineering of Nanomaterials

Li,

Zhang,

Han

2023

Chem. Rev.

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“…Among the latter, multislice electron ptychography is promising for MOFs. This technique combines STEM and 2D coherent ED patterns and has been successfully used for the measurement of zeolite atomic structures, a type of material that is also sensitive to the electron beam [111]. An incorporated adaptive propagator helps to address the impact of specimen misorientations on the accuracy and reliability of the image [89].…”

Section: Discussionmentioning

confidence: 99%

“…HRTEM characterization under cryogenic conditions of CO2@ZIF-8(Zn)[47] and protein-ZIF-8(Zn) composites[49]. (a-d) Host-Guest Structures within ZIF-8(Zn) viewed along[111] (a, b) and [001] (c, d) projection. (a, c) Left: CTF-corrected Cryo-TEM images of CO2-filled ZIF-8 particle taken with electron dose rate of ∼4.5 e -Å -2 s -1 for 1.5 s. Bright regions correspond to mass density, and contrast in the center of the 6-ring window (a) and 4-ring window (c) is observed respectively for multiple unit cells.…”

mentioning

confidence: 99%

“…(b, d) Simulated structure of ZIF-8 with DFTpredicted binding site of CO2 indicated with red spheres in (a, c), respectively[47]. (e-g) iDPC-STEM images, corresponding FFT, and the structural analysis of the selected area (indicated with the same color) of BZIF-8-S from the[111] (e) and[100] (f), and BZIF-8-B from the[111] (g) zone axis. (e, f) show high-crystallinity with ~3.4 Å 6-ring window and ~2.8 Å 4-ring window, respectively.…”

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confidence: 99%

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Research Progress on Metal-Organic Frameworks by Advanced Transmission Electron Microscopy

Zheng¹,

Yin²,

Pan³

et al. 2023

Preprint

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Metal-organic frameworks (MOFs), composed of metal nodes and inorganic linkers are promising for a wide range of applications due to their unique periodic frameworks that can be flexibly tuned. Understanding of the structure-activity relationships can facilitate the development and application of MOFs nanomaterials. Transmission electron microscopy (TEM) is a one-of-a-kind technique capable of characterizing MOFs microstructures at the atomic scale. Besides, in-situ TEM set-ups make it possible to direct visualize the microstructural evolution of MOFs in real time, which enables monitoring transitions of MOFs during growth as well as under working conditions. However, MOFs are so sensitive to the high-energy electron beam which makes TEM-based characterizing methods challenging. In this review, we first introduce the main damage mechanisms for MOFs under electron beam irradiation and two strategies to minimize the damages: low-dose TEM and cryo-TEM. Then, we discuss the techniques combined with the two strategies to analyze the MOFs’ microstructure, including three-dimensional electron diffraction, direct detection electron counting camera, and iDPC-STEM. Groundbreaking milestones and research advances with respect to static characterization of MOFs structures are highlighted. In-situ TEM studies are exemplary reviewed to provide insights into MOFs dynamics induced by various stimuli. Additionally, perspectives on promising techniques that may further facilitate the MOFs study using TEM are analyzed.

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“…In terms of imaging thick specimens, electron ptychography has recently made exciting and significant progress in the field of zeolites. It uses a pixelated array detector to record the information on the transmitted beam and obtains the three-dimensional atomic structure through repeated multislice iterative methods. ,, It has achieved the atomic imaging of thick samples (>40 nm) and at the same time has higher spatial resolution (∼0.85 Å) and possible Z -direction resolution (∼6.6 nm) at a dose of around 3500 e – /Å 2 . It offers an efficient low-dose 3D imaging technique that enables an investigation of the structural inhomogeneity in zeolites.…”

Section: Atomic Imaging To Reveal Comprehensive Structural Informationmentioning

confidence: 99%

Atomic Imaging of Zeolites and Confined Single Molecules by iDPC-STEM

Xiong,

Wang,

Chen

et al. 2023

ACS Catal.

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Zeolites are a family of nanoporous crystalline materials with ordered channel systems, flexibly adjustable activity, and high hydrothermal stability and have been widely used as adsorbents and catalysts. The micropores of zeolites are comparable to the size of single molecules, which can function as "molecular sieves" by selectively adsorbing or transforming targeted guest molecules. Therefore, a slight mismatch in the dimensions of the pore architecture and guest molecules sometimes will cause thousands of times of changes in the physicochemical processes inside zeolite channels. Adjusting the pore structures to match targeted molecules to precisely regulate the host−guest interactions between them and thereby control the diffusion or reaction pathways has always been one of the most essential principles for designing novel zeolite materials and applications. Thus, it is highly desirable to understand the moving and transforming behaviors of different small molecules in zeolitic nanopores and probe the intricate interactions between them in such delicate situations. The recently emerged integrated differential phase contrast scanning transmission electron microscopy (iDPC-STEM) holds great potential for imaging zeolite materials at an atomic resolution, since it can greatly improve electron utilization efficiency to reduce the required electron dose and is conducive to light element imaging. This Perspective focuses on the in situ observation of single-molecule adsorption−desorption behaviors in zeolites using the in situ iDPC-STEM imaging technique. We demonstrated that iDPC-STEM is an effective method for probing atomic structures of beam-sensitive zeolite materials and exhibits a remarkable ability in imaging light elements under low-dose conditions. Subsequently, we introduce a general "confined freezing" strategy to immobilize small molecules in size-matchable nanopores, which are stable enough for atomically resolved single-molecule imaging. Finally, three industrially important aromatic molecules with slight differences, including benzene, p-xylene, and pyridine, were selected to demonstrate the different adsorption/desorption behaviors and corresponding host−guest interactions at the subnanometer scale. In this way, we provide a real-space methodology to actually "see" the movement and transformation of individual molecules at the atomic scale and pave the way for clarifying the key role of host−guest interactions in molecular adsorption, diffusion, and reaction processes.

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Ptychographic measurements of varying size and shape along zeolite channels

Cited by 15 publications

References 80 publications

Applications of Transmission Electron Microscopy in Phase Engineering of Nanomaterials

Applications of Transmission Electron Microscopy in Phase Engineering of Nanomaterials

Research Progress on Metal-Organic Frameworks by Advanced Transmission Electron Microscopy

Atomic Imaging of Zeolites and Confined Single Molecules by iDPC-STEM

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