Application of advanced (S)TEM methods for the study of nanostructured porous functional surfaces: A few working examples

Santos, Antonio J.; Lacroix, Bertrand; Maudet, Florian; Paumier, F.; Hurand, S.; Dupeyrat, Cyril; Gómez, Valentín Bote; Huffaker, Diana L.; Girardeau, T.; Garcı́a, R.; Morales, F. M.

doi:10.1016/j.matchar.2022.111741

Cited by 6 publications

(5 citation statements)

References 99 publications

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“…As HAADF‐STEM takes images on the basis of electron‐beam diffraction, the bright‐dark contrast in an image reflects the atom numbers of elements (called z‐contrast). [ 13,26 ] The bright/dark area in Figure 6g corresponds to the dark/bright area in Figure 6e, respectively, indicating the thick/thin region of the sample. The fairly uniform contrast for most parts of the particular area in Figure 6g implies the even distribution of all elements.…”

Section: Resultsmentioning

confidence: 99%

Toward High‐Quality Sulfide Solid Electrolytes: A Liquid‐Phase Approach Featured with an Interparticle Coupled Unification Effect

Han,

Xu,

Wang

et al. 2023

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Sulfide solid electrolytes (SSEs) are highly wanted for solid‐state batteries (SSBs). While their liquid‐phase synthesis is advantageous over their solid‐phase strategy in scalable production, it confronts other challenges, such as low‐purity products, user‐unfriendly solvents, energy‐inefficient solvent removal, and unsatisfactory performance. This article demonstrates that a suspension‐based solvothermal method using single oxygen‐free solvents can solve those problems. Experimental observations and theoretical calculations together show that the basic function of suspension‐treatment is “interparticle‐coupled unification”, that is, even individually insoluble solid precursors can mutually adsorb and amalgamate to generate uniform composites in nonpolar solvents. This anti‐intuitive concept is established when investigating the origins of impurities in SSEs electrolytes made by the conventional tetrahydrofuran‐ethanol method and then searching for new solvents. Its generality is supported by four eligible alkane solvents and four types of SSEs. The electrochemical assessments on the former three SSEs show that they are competitive with their counterparts in the literature. Moreover, the synthesized SSEs presents excellent battery performance, showing great potential for practical applications.

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Section: Resultsmentioning

confidence: 99%

Toward High‐Quality Sulfide Solid Electrolytes: A Liquid‐Phase Approach Featured with an Interparticle Coupled Unification Effect

Han,

Xu,

Wang

et al. 2023

Small

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“…The transmitted electrons can be analyzed by various detectors to provide accurate information about atomic arrangement, crystalline phases and defects, allowing for the achievement of structural, chemical and electronic characterization across length scales ranging from the atomic scale crystallography to the microstructure. Advanced TEMs are capable of an atomic-scale resolution below 0.5 Å, which is especially suited to probe thin film interfaces, defects, grain structure, orientations, dislocations, and more [59,60]. However, due to the relatively short mean free path of electrons in matter, samples must be suitably prepared as thin slices, so to study thin films, it is necessary to cut thin cross-sections of the samples (cross-sectional TEM (XTEM)) using, for example, a focused ion beam (FIB) facility.…”

Section: Scanning Transmission Electron Microscopy (Tem)mentioning

confidence: 99%

Advances in Structural and Morphological Characterization of Thin Magnetic Films: A Review

Aich,

Meneghini,

Tortora

2023

Materials

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The present review places emphasis on a comprehensive survey of experimental techniques to probe the structural and morphological features at the nanoscale range in thin magnetic films, incorporating those available at in-house laboratories as well as those at state-of-the-art synchrotron radiation facilities. This elucidating the range of available techniques, and the information they can yield represents a step for advancing the understanding of and for unlocking new possibilities in the design and optimization of thin magnetic films across a wide range of applications.

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“…An alternative to assessing tortuosities of porous materials by PFG NMR diffusion measurements are microscopy-based methods. A technique which, in this respect, underwent a steep development in the recent years and proved its capability to provide such information and to furthermore give detailed insight into the mesoscopic structure of porous materials is STEM tomography [14][15][16]. To this end, thin electron transparent specimen in the range of a few 10 nm need to be prepared.…”

Section: Determination Of Tortuosities By Stem Tomographymentioning

confidence: 99%

“…(For more details, the interested reader is referred to Refs. [14][15][16]). By applying a further numerical analysis, also tortuosity factors characterizing the pore system can be determined [64,65].…”

Section: Determination Of Tortuosities By Stem Tomographymentioning

confidence: 99%

“…A problem, however, often existing in this context relates to missing knowledge about those porosity-related features of a material, which determine gas diffusivities within its pore system. Basically, two experimental options are available to get such information: (i) STEM (scanning transmission electron microscopy) tomography [14][15][16][17] as well as related techniques and, (ii) techniques capable of microscopic diffusion measurements, such as pulsed field gradient nuclear magnetic resonance (PFG-NMR [2,18]). While (i) is based on 3D reconstructions of the mesoscopic pore structure, from which these quantities can be numerically derived or estimated, (ii) allows to measure the diffusion of gas molecules within the pores directly.…”

Section: Introductionmentioning

confidence: 99%

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New Perspectives for Evaluating the Mass Transport in Porous Catalysts and Unfolding Macro- and Microkinetics

et al. 2022

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In this article we shed light on newly emerging perspectives to characterize and understand the interplay of diffusive mass transport and surface catalytic processes in pores of gas phase metal catalysts. As a case study, nanoporous gold, as an interesting example exhibiting a well-defined pore structure and a high activity for total and partial oxidation reactions is considered. PFG NMR (pulsed field gradient nuclear magnetic resonance) measurements allowed here for a quantitative evaluation of gas diffusivities within the material. STEM (scanning transmission electron microscopy) tomography furthermore provided additional insight into the structural details of the pore system, helping to judge which of its features are most decisive for slowing down mass transport. Based on the quantitative knowledge about the diffusion coefficients inside a porous catalyst, it becomes possible to disentangle mass transport contributions form the measured reaction kinetics and to determine the kinetic rate constant of the underlying catalytic surface reaction. In addition, predictions can be made for an improved effectiveness of the catalyst, i.e., optimized conversion rates. This approach will be discussed at the example of low-temperature CO oxidation, efficiently catalysed by npAu at 30 °C. The case study shall reveal that novel porous materials exhibiting well-defined micro- and mesoscopic features and sufficient catalytic activity, in combination with modern techniques to evaluate diffusive transport, offer interesting new opportunities for an integral understanding of catalytic processes. Graphical Abstract

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Application of advanced (S)TEM methods for the study of nanostructured porous functional surfaces: A few working examples

Cited by 6 publications

References 99 publications

Toward High‐Quality Sulfide Solid Electrolytes: A Liquid‐Phase Approach Featured with an Interparticle Coupled Unification Effect

Toward High‐Quality Sulfide Solid Electrolytes: A Liquid‐Phase Approach Featured with an Interparticle Coupled Unification Effect

Advances in Structural and Morphological Characterization of Thin Magnetic Films: A Review

New Perspectives for Evaluating the Mass Transport in Porous Catalysts and Unfolding Macro- and Microkinetics

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