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Operando methods: A new era of electrochemistry

CURRENT OPINION IN ELECTROCHEMISTRY (2023)

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Article Chemistry, Multidisciplinary

Anodic and Cathodic Platinum Dissolution Processes Involve Different Oxide Species

Timo Fuchs et al.

Summary: The degradation of Pt-containing oxygen reduction catalysts for fuel cell applications is studied using operando high-energy surface X-ray diffraction, online mass spectrometry, and density functional theory. It is found that anodic dissolution, detected during oxidation, and cathodic dissolution, observed during reduction, are linked to two different oxide phases. The amount of surface restructuring after an oxidation/reduction cycle is potential-independent after the saturation coverage of the first oxide phase.

ANGEWANDTE CHEMIE-INTERNATIONAL EDITION (2023)

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Review Chemistry, Multidisciplinary

Operando Scanning Electrochemical Probe Microscopy during Electrocatalysis

Carla Santana Santos et al.

Summary: Scanning electrochemical probe microscopy (SEPM) techniques are used to study the local electrochemical reactivity of interfaces. Operando SEPM measurements involve using a SEPM tip to investigate electrocatalysts' performance while modulating the interface reactivity. This combination allows the correlation of electrochemical activity with changes in surface properties and provides insights into reaction mechanisms.

CHEMICAL REVIEWS (2023)

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Article Multidisciplinary Sciences

Operando studies reveal active Cu nanograins for CO2 electroreduction

Yao Yang et al.

Summary: This study presents a comprehensive investigation of the structural dynamics of Cu nanocatalysts during the electrochemical synthesis of fuels and chemicals. The presence of active Cu nanograins under CO2 reduction conditions and their role in supporting C-C coupling reactions were observed. Quantitative structure-activity correlation revealed that a higher fraction of Cu nanograins leads to higher selectivity for C2+ products. This research provides a powerful platform for advancing our understanding of the complex structural evolution of nanocatalysts under electrochemical conditions.

NATURE (2023)

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Article Microscopy

Quantification of reagent mixing in liquid flow cells for Liquid Phase-TEM

Stefan Merkens et al.

Summary: Liquid-Phase Transmission Electron Microscopy (LP-TEM) allows the study of nanoscale dynamics in a native liquid environment. This manuscript introduces a method for characterizing the hydrodynamic properties of LP-TEM flow systems. Experimental measurements and a numerical model were used to understand the impact of flow channel geometry on solute transport.

ULTRAMICROSCOPY (2023)

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Article Chemistry, Multidisciplinary

Operando Electrochemical Liquid-Cell Scanning Transmission Electron Microscopy (EC-STEM) Studies of Evolving Cu Nanocatalysts for CO2 Electroreduction

Yao Yang et al.

Summary: The design and synthesis of nanocatalysts with well-defined sizes, compositions, and structures have greatly enhanced our ability to control catalyst activity and selectivity for energy-related electrochemical reactions. By using operando electrochemical liquid-cell scanning transmission electron microscopy (EC-STEM), the dynamic evolution of Cu nanocatalysts during CO2 electroreduction was observed, providing valuable insights into their active states. With further technical advancements, operando EC-STEM is expected to become a powerful electroanalytical method for studying nanoscale electrocatalysts at solid/liquid interfaces.

ACS SUSTAINABLE CHEMISTRY & ENGINEERING (2023)

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Article Chemistry, Physical

The Necessity for Multiscale In Situ Characterization of Tailored Electrocatalyst Nanoparticle Stability

Ward van der Stam

Summary: Tailored nanoparticles provide a perfect toolbox for synthesizing electrocatalyst nanoparticles with atomic precision to control and steer electrocatalytic reactions. However, due to the instability of electrocatalysts, in situ characterization techniques are necessary to probe the morphology and composition of nanoparticles and design stable electrocatalysts with superior activity and selectivity.

CHEMISTRY OF MATERIALS (2023)

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Review Chemistry, Multidisciplinary

Electrocatalysis in Alkaline Media and Alkaline Membrane-Based Energy Technologies

Yao Yang et al.

Summary: This article provides a comprehensive review of the fundamentals of electrocatalysis in alkaline media and its applications in alkaline-based energy technologies. Nonprecious anion exchange membrane fuel cells offer a promising alternative to proton exchange membrane fuel cells for sluggish oxygen reduction reaction. The understanding of proton-coupled electron transfer and active sites has contributed to the development of high-performance and durable alkaline fuel cells.

CHEMICAL REVIEWS (2022)

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Article Multidisciplinary Sciences

Nonprecious transition metal nitrides as efficient oxygen reduction electrocatalysts for alkaline fuel cells

Rui Zeng et al.

Summary: This study reports on a new type of nonprecious transition metal nitrides as ORR electrocatalysts in alkaline medium. The research found that the air-exposed nitrides spontaneously form a oxide shell, providing a highly active catalyst architecture. The carbon-supported cobalt nitride catalyst exhibited high half-wave potential and peak power density.

SCIENCE ADVANCES (2022)

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Article Chemistry, Physical

In Situ Liquid Electrochemical TEM Investigation of LiMn1.5Ni0.5O4 Thin Film Cathode for Micro-Battery Applications

Ankush Bhatia et al.

Summary: The study utilized an electrochemical transmission electron microscope (TEM) to demonstrate the structural and morphological changes of micro-batteries during cycling, shedding light on the capacity fade observed in the thin-film cathode.

SMALL METHODS (2022)

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Article Chemistry, Multidisciplinary

Operando Resonant Soft X-ray Scattering Studies of Chemical Environment and Interparticle Dynamics of Cu Nanocatalysts forCO2Electroreduction

Yao Yang et al.

Summary: Understanding the chemical environment and interparticle dynamics of nanoparticle electrocatalysts is crucial for controlling their activity and selectivity. In this study, the EC-RSoXS method was used to investigate the structural transformation and chemical identity of active sites in Cu nanoparticle ensembles. The results revealed different behaviors of nanoparticles of different sizes under X-ray exposure.

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY (2022)

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Article Materials Science, Multidisciplinary

Very-High Dynamic Range, 10,000 Frames/Second Pixel Array Detector for Electron Microscopy

Hugh T. Philipp et al.

Summary: This article introduces a new hybrid pixel array detector (EMPAD-G2) that improves the precision and accuracy of quantitative scanning transmission electron microscopy methods such as ptychography. It enables rapid collection of high-quality STEM data and has a wide dynamic range.

MICROSCOPY AND MICROANALYSIS (2022)

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Article Chemistry, Physical

Metal Monolayers on Command: Underpotential Deposition at Nanocrystal Surfaces: A Quantitative Operando Electrochemical Transmission Electron Microscopy Study

Yao Yang et al.

Summary: This study investigates the UPD of monolayer Cu at single-crystal Au nanocube surfaces. By correlating electrochemical results and high-resolution chemical mapping, it is revealed that Cu electrodeposition is guided by the crystallographic orientation of the Au substrate, providing a generalized platform for advancing the fundamental understanding of (electro)chemical reaction dynamics.

ACS ENERGY LETTERS (2022)

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Article Chemistry, Physical

Uncovering material deformations via machine learning combined with four-dimensional scanning transmission electron microscopy

Chuqiao Shi et al.

Summary: This study demonstrates a rapid and semi-automated unsupervised machine learning approach to uncover lattice deformations in materials. The method utilizes divisive hierarchical clustering to automatically reveal multi-scale deformations in the entire sample. This data-driven analysis provides insight into material structures and accelerates the discovery of new materials.

NPJ COMPUTATIONAL MATERIALS (2022)

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Article Chemistry, Multidisciplinary

Elucidating Cathodic Corrosion Mechanisms with Operando Electrochemical Transmission Electron Microscopy

Yao Yang et al.

Summary: Cathodic corrosion is a process where metallic electrodes corrode under reducing potentials. Recent studies using in situ electron microscopy have found that cathodic corrosion leads to higher levels of structural degradation in nanocrystals compared to bulk electrodes, and can unexpectedly result in the formation of Au-Pt alloy nanoparticles.

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY (2022)

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Article Nanoscience & Nanotechnology

The effect of flow on radiolysis in liquid phase-TEM flow cells

Stefan Merkens et al.

Summary: This study explores the peculiarities of beam-induced chemistry in the presence of a flowing liquid within a heterogeneously irradiated nanoconfined channel corresponding to a LP-TEM flow cell. It is found that under moderate flow conditions, the concentration of some principal chemical species increases significantly, which is counterintuitive.

NANO EXPRESS (2022)

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Article Chemistry, Multidisciplinary

Real-time Monitoring Reveals Dissolution/Redeposition Mechanism in Copper Nanocatalysts during the Initial Stages of the CO2 Reduction Reaction

Jan Vavra et al.

Summary: This study reveals the reconstruction mechanism of Cu-based nanocatalysts during the electrochemical CO2 reduction reaction, as well as the key role of copper oxides in this process, through a combination of electrochemical in situ transmission electron microscopy and operando X-ray absorption spectroscopy. Understanding these underlying processes provides a pathway to rational design of Cu electro(re)deposited catalysts and stability improvement for catalysts fabricated by other methods.

ANGEWANDTE CHEMIE-INTERNATIONAL EDITION (2021)

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Review Chemistry, Physical

Operando Methods in Electrocatalysis

Yao Yang et al.

Summary: Electrocatalysis is crucial for advancing renewable energy technologies, and understanding the structure and reaction mechanisms of electrocatalysts at electrode-electrolyte interfaces is fundamental. In situ and operando techniques, such as operando synchrotron-based X-ray techniques and in situ atomic-scale scanning transmission electron microscopy, provide valuable insights into the interfacial structural and compositional changes under reaction conditions, aiding in the study of charge transfer kinetics and reaction mechanisms. The continuous development of these techniques will contribute significantly to establishing structure/composition-reactivity correlations of electrocatalysts at unprecedented atomic-scale and molecular levels under realistic, real-time reaction conditions.

ACS CATALYSIS (2021)

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Article Chemistry, Multidisciplinary

Revealing the Dynamics and Roles of Iron Incorporation in Nickel Hydroxide Water Oxidation Catalysts

Chunguang Kuai et al.

Summary: The study shows a strong correlation between iron incorporation and oxygen evolution reaction (OER), with iron absorption rate being significantly higher at high working potentials and favoring electrochemically more reactive edge sites. Iron incorporation can suppress the oxidation of Ni and enhance the Ni reducibility, leading to improved OER catalytic activity. This provides a holistic approach to understanding and controlling catalytic processes by tailoring Fe incorporation dynamics across the electrocatalyst-electrolyte interface.

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY (2021)

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Article Multidisciplinary Sciences

Morphology and mechanism of highly selective Cu(II) oxide nanosheet catalysts for carbon dioxide electroreduction

Xingli Wang et al.

Summary: Copper oxides (CuO) selectively catalyze the electrochemical reduction of CO2 to hydrocarbons and oxygenates. Here, the authors study the activity and morphological evolution of 2D CuO nanosheets under applied electrode potentials to conclude the primacy of dendritic shapes and involvement of a new coupling pathway.

NATURE COMMUNICATIONS (2021)

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Article Multidisciplinary Sciences

Dynamic transformation of cubic copper catalysts during CO2 electroreduction and its impact on catalytic selectivity

Philipp Grosse et al.

Summary: To design effective and stable catalysts for energy conversion applications, it is essential to understand how they transform under reaction conditions and reveal the structure-property relationships, especially for catalysts used in the electroreduction of carbon dioxide. Real-time electrochemical studies show the restructuring of copper(I) oxide cubes during reaction and its impact on catalyst selectivity. Understanding the changes in catalysts during reaction is crucial for rational design, with studies linking structural transformations of cubic copper oxide catalysts with their selectivity.

NATURE COMMUNICATIONS (2021)

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Article Chemistry, Multidisciplinary

Nanoscale Chemical and Structural Analysis during In Situ Scanning/Transmission Electron Microscopy in Liquids

Rui Serra-Maia et al.

Summary: Liquid-cell scanning/transmission electron microscopy (S/TEM) has been used to study nanostructure nucleation and growth, electrochemistry, and corrosion. By generating a gas bubble during electrochemical water splitting, the thickness of the liquid can be reduced to allow for atomic-scale analysis. This method enables multi-modal, nanoscale understanding of solid-state samples in liquid media.

ACS NANO (2021)

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Article Multidisciplinary Sciences

Correlative operando microscopy of oxygen evolution electrocatalysts

J. Tyler Mefford et al.

Summary: Transition metal (oxy)hydroxides are promising electrocatalysts for the oxygen evolution reaction, with their properties evolving dynamically and heterogeneously with applied voltage. By studying single-crystalline beta-Co(OH)(2) platelet particles, researchers have found that the particles change structure and composition from inactive to active states as the voltage increases, ultimately linking bulk ion-insertion with surface catalytic activity. This study demonstrates the importance of understanding the nanoscale structure of electrocatalysts in predicting and optimizing their oxygen evolution activity.

NATURE (2021)

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Article Chemistry, Analytical

Leakless, Bipolar Reference Electrodes: Fabrication, Performance, and Miniaturization

Nicole L. Walker et al.

Summary: In this study, a new leakless, bipolar reference electrode was proposed, which replaces the traditional porous frit with a conductive wire to prevent ion leakage and enable miniaturization. The leakless BPRE demonstrated similar performance to commercial reference electrodes in potentiometric and voltammetric measurements. Promising results were obtained in nonaqueous solvents and with other conductive materials, showcasing the potential of leakless BPREs in various applications.

ANALYTICAL CHEMISTRY (2021)

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Article Multidisciplinary Sciences

Electron ptychography achieves atomic-resolution limits set by lattice vibrations

Zhen Chen et al.

Summary: Transmission electron microscopes use electrons with wavelengths of a few picometers to potentially image individual atoms in solids, but their image resolution is often reduced by lens aberrations and electron scattering. By using electron ptychography to solve these issues, researchers have achieved higher image resolution and precision in locating embedded atoms.

SCIENCE (2021)

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Article Chemistry, Multidisciplinary

Understanding the Dynamics of Molecular Water Oxidation Catalysts with Liquid-Phase Transmission Electron Microscopy: The Case of Vitamin B12

Zahra Abdi et al.

Summary: Cobalt compounds are efficient catalysts for the oxygen evolution reaction, and vitamin B-12, as a soluble cobalt compound with high enzymatic activity, is a relevant candidate for biomimetic catalyst research. By utilizing advanced techniques, this study provided direct evidence of diffuse layer dynamics on the working electrode interface and identified the formation of cobalt oxyphosphate nanoparticles as the initial stage of the catalytic pathway.

ACS SUSTAINABLE CHEMISTRY & ENGINEERING (2021)

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Article Multidisciplinary Sciences

Electrochemically scrambled nanocrystals are catalytically active for CO2-to-multicarbons

Yifan Li et al.

PROCEEDINGS OF THE NATIONAL ACADEMY OF SCIENCES OF THE UNITED STATES OF AMERICA (2020)

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Article Chemistry, Multidisciplinary

Dynamic Reoxidation/Reduction-Driven Atomic Interdiffusion for Highly Selective CO2 Reduction toward Methane

Chia-Jui Chang et al.

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY (2020)

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Article Microscopy

The exit -wave power-cepstrum transform for scanning nanobeam electron diffraction: robust strain mapping at subnanometer resolution and subpicometer precision

Elliot Padgett et al.

ULTRAMICROSCOPY (2020)

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Article Chemistry, Physical

Selective Electrochemical CO2 Reduction during Pulsed Potential Stems from Dynamic Interface

Kevin W. Kimura et al.

ACS CATALYSIS (2020)

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Article Chemistry, Multidisciplinary

In situ electrochemistry inside a TEM with controlled mass transport

Anne France Beker et al.

NANOSCALE (2020)

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Article Chemistry, Multidisciplinary

A Strategy for Increasing the Efficiency of the Oxygen Reduction Reaction in Mn-Doped Cobalt Ferrites

Yin Xiong et al.

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY (2019)

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Article Chemistry, Multidisciplinary

Regulating Key Variables and Visualizing Lithium Dendrite Growth: An Operando X-ray Study

Seung-Ho Yu et al.

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY (2019)

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Review Chemistry, Physical

Designing materials for electrochemical carbon dioxide recycling

Michael B. Ross et al.

NATURE CATALYSIS (2019)

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Article Chemistry, Multidisciplinary

Morphological and Structural Evolution of Co3O4 Nanoparticles Revealed by in Situ Electrochemical Transmission Electron Microscopy during Electrocatalytic Water Oxidation

Nathaly Ortiz Pena et al.

ACS NANO (2019)

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Review Chemistry, Multidisciplinary

Nanoscale Surface Structure-Activity in Electrochemistry and Electrocatalysis

Cameron L. Bentley et al.

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY (2019)

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Article Chemistry, Multidisciplinary

In Situ X-ray Absorption Spectroscopy of a Synergistic Co-Mn Oxide Catalyst for the Oxygen Reduction Reaction

Yao Yang et al.

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY (2019)

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Review Nanoscience & Nanotechnology

Resolution and aberration correction in liquid cell transmission electron microscopy

Niels de Jonge et al.

NATURE REVIEWS MATERIALS (2019)

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Article Chemistry, Multidisciplinary

Real-time imaging of activation and degradation of carbon supported octahedral Pt-Ni alloy fuel cell catalysts at the nanoscale using in situ electrochemical liquid cell STEM

Vera Beermann et al.

ENERGY & ENVIRONMENTAL SCIENCE (2019)

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Article Chemistry, Physical

Environment-Dependent Radiation Damage in Atmospheric Pressure X-ray Spectroscopy

Robert S. Weatherup et al.

JOURNAL OF PHYSICAL CHEMISTRY B (2018)

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Article Chemistry, Multidisciplinary

Direct visualization of sulfur cathodes: new insights into Li-S batteries via operando X-ray based methods

Seung-Ho Yu et al.

ENERGY & ENVIRONMENTAL SCIENCE (2018)

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Article Chemistry, Multidisciplinary

Identification of Stabilizing High-Valent Active Sites by Operando High-Energy Resolution Fluorescence-Detected X-ray Absorption Spectroscopy for High-Efficiency Water Oxidation

Sung-Fu Hung et al.

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY (2018)

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Article Multidisciplinary Sciences

Copper adparticle enabled selective electrosynthesis of n-propanol

Jun Li et al.

NATURE COMMUNICATIONS (2018)

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Article Multidisciplinary Sciences

Selective increase in CO2 electroreduction activity at grain-boundary surface terminations

Ruperto G. Mariano et al.

SCIENCE (2017)

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Review Chemistry, Physical

A materials driven approach for understanding single entity nano impact electrochemistry

Keith J. Stevenson et al.

CURRENT OPINION IN ELECTROCHEMISTRY (2017)

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Structure of the Photo-catalytically Active Surface of SrTiO3

Manuel Plaza et al.

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY (2016)

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Article Materials Science, Multidisciplinary

High Dynamic Range Pixel Array Detector for Scanning Transmission Electron Microscopy

Mark W. Tate et al.

MICROSCOPY AND MICROANALYSIS (2016)

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Unravelling the electrochemical double layer by direct probing of the solid/liquid interface

Marco Favaro et al.

NATURE COMMUNICATIONS (2016)

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Article Instruments & Instrumentation

A soft XAS transmission cell for operando studies

Christoph Schwanke et al.

JOURNAL OF SYNCHROTRON RADIATION (2016)

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Identification of Highly Active Fe Sites in (Ni,Fe)OOH for Electrocatalytic Water Splitting

Daniel Friebel et al.

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY (2015)

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In Situ Study of Lithiation and Delithiation of MoS2 Nanosheets Using Electrochemical Liquid Cell Transmission Electron Microscopy

Zhiyuan Zeng et al.

NANO LETTERS (2015)

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Nanoscale Imaging of Fundamental Li Battery Chemistry: Solid-Electrolyte Interphase Formation and Preferential Growth of Lithium Metal Nanoclusters

Robert L. Sacci et al.

NANO LETTERS (2015)

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Real-time imaging and local elemental analysis of nanostructures in liquids

Edward A. Lewis et al.

CHEMICAL COMMUNICATIONS (2014)

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Electron-Water Interactions and Implications for Liquid Cell Electron Microscopy

Nicholas M. Schneider et al.

JOURNAL OF PHYSICAL CHEMISTRY C (2014)

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Quantitative Electrochemical Measurements Using In Situ ec-S/TEM Devices

Raymond R. Unocic et al.

MICROSCOPY AND MICROANALYSIS (2014)

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Nanoscale Imaging of Lithium Ion Distribution During In Situ Operation of Battery Electrode and Electrolyte

Megan E. Holtz et al.

NANO LETTERS (2014)

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The structure of interfacial water on gold electrodes studied by x-ray absorption spectroscopy

Juan-Jesus Velasco-Velez et al.

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In Situ Electron Energy-Loss Spectroscopy in Liquids

Megan E. Holtz et al.

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Transmission electron microscopy with a liquid flow cell

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Aberration-corrected ADF-STEM depth sectioning and prospects for reliable 3D imaging in S/TEM

Huolin L. Xin et al.

JOURNAL OF ELECTRON MICROSCOPY (2009)

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Structure and bonding at the atomic scale by scanning transmission electron microscopy

David A. Muller

NATURE MATERIALS (2009)

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Operando methodology:: combination of in situ spectroscopy and simultaneous activity measurements under catalytic reaction conditions

MA Bañares

CATALYSIS TODAY (2005)

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An in situ cell for characterization of solids by soft x-ray absorption

IJ Drake et al.

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Differential electrochemical mass spectrometry

H Baltruschat

JOURNAL OF THE AMERICAN SOCIETY FOR MASS SPECTROMETRY (2004)

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Dynamic microscopy of nanoscale cluster growth at the solid-liquid interface

MJ Williamson et al.

NATURE MATERIALS (2003)

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Snapshots of a working catalyst: possibilities and limitations of in situ spectroscopy in the field of heterogeneous catalysis

BM Weckhuysen

CHEMICAL COMMUNICATIONS (2002)

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