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DOE OSTI2020

Evolution of Metastable Structures at Bimetallic Surfaces from Microscopy and Machine-Learning Molecular Dynamics

The restructuring of interfaces plays a crucial role in materials science and heterogeneous catalysis. Bimetallic systems, in particular, often adopt very different compositions and morphologies at surfaces compared to the bulk. For the first time, we reveal a detailed atomistic picture of long-time scale restructuring of Pd deposited on Ag using microscopy, spectroscopy, and novel simulation methods. By developing and performing accelerated machine-learning molecular dynamics followed by an automated analysis method, we discover and characterize previously unidentified surface restructuring mechanisms in an unbiased fashion, including Pd-Ag place exchange and Ag pop-out as well as step ascent and descent. Remarkably, layer-by-layer dissolution of Pd into Ag is always preceded by an encapsulation of Pd islands by Ag, resulting in a significant migration of Ag out of the surface and a formation of extensive vacancy pits within a period of microseconds. These metastable structures are of vital catalytic importance, as Ag-encapsulated Pd remains much more accessible to reactants than bulk-dissolved Pd. We report our approach is broadly applicable to complex multimetallic systems and enables the previously intractable mechanistic investigation of restructuring dynamics at atomic resolution.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

Fractal dimension of cohesive sediment flocs at steady state under seven shear flow conditions

The morphological properties of kaolin flocs were investigated in a Couette-flow experiment at the steady state under seven shear flow conditions (shear rates of 5.36, 9.17, 14, 24, 31, 41 and 53 s -1 ). These properties include a one-dimensional (1-D) fractal dimension (D 1 ), a two-dimensional (2-D) fractal dimension (D 2 ), a perimeter-based fractal dimension (D pf ) and an aspect ratio (AR). They were calculated based on the projected area (A), equivalent size, perimeter (P) and length (L) of the major axis of the floc determined through sample observation and an image analysis system. The parameter D 2 , which characterizes the relationship between the projected area and the length of the major axis using a power function, A ∝ L D 2 , increased from 1.73 ± 0.03, 1.72 ± 0.03, and 1.75 ± 0.04 in the low shear rate group (G = 5.36, 9.17, and 14 s -1 ) to 1.92 ± 0.03, 1.82 ± 0.02, 1.85 ± 0.02, and 1.81 ± 0.02 in the high shear rate group (24, 31, 41 and 53 s -1 ), respectively. The parameter D 1 characterizes the relationship between the perimeter and length of the major axis by the function P ∝ L D 1 and decreased from 1.52 ± 0.02, 1.48 ± 0.02, 1.55 ± 0.02, and 1.63 ± 0.02 in the low shear group (5.36, 9.17, 14 and 24 s -1 ) to 1.45 ± 0.02, 1.39 ± 0.02, and 1.39 ± 0.02 in the high shear group (31, 41 and 53 s -1 ), respectively. The results indicate that with increasing shear rates, the flocs become less elongated and that their boundary lines become tighter and more regular, caused by more breakages and possible restructurings of the flocs. The parameter D pf , which is related to the perimeter and the projected area through the function , decreased as the shear rate increased almost linearly. The parameter AR, which is the ratio of the length of the major axis and equivalent diameter, decreased from 1.56, 1.59, 1.53 and 1.51 in the low shear rate group to 1.43, 1.47 and 1.48 in the high shear rate group. These changes in D pf and AR show that the flocs become less convoluted and more symmetrical and that their boundaries become smoother and more regular in the high shear rate group than in the low shear rate group due to breakage and possible restructuring processes. To assess the effects of electrolyte and sediment concentration, 0.1 mol/L calcium chloride (CaCl 2 ) and initial sediment concentration from 7.87 × 10 -5 to 1.57 × 10 -5 were used in this preliminary study. The addition of electrolyte and increasing sediment concentration could produce more symmetrical flocs with less convoluted and simpler boundaries. In addition, some new information on the temporal variation of the median size of the flocs during the flocculation process is presented.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

CO–induced roughening of Cu(111): formation and detection of reactive nanoclusters on metal surfaces

The formation of nanoclusters on metal surfaces in the presence of reactive environments is a phenomenon with important implications for catalysis. These nanoclusters are composed of atoms ejected from undercoordinated sites such as step edges, and their presence alters the catalytic properties of solid materials. We perform density functional theory (DFT) and kinetic Monte Carlo (KMC) simulations to investigate the formation and reactivity of copper clusters on Cu(111). Our results indicate a considerably higher reactivity of small copper nanoclusters, with up to seven atoms in size on roughened copper surfaces than on pristine Cu(111) and Cu(211). Regarding the restructuring events that give rise to nanoclusters under CO atmospheres, we determine that the ejection of Cu atoms from step edges and their migration therefrom to adjacent Cu(111) terraces are, by and large, driven by CO coverage effects. By means of KMC simulations, which account for CO–CO lateral interactions and CO–induced surface restructuring, we show that temperature programmed desorption (TPD) holds promise for the detection of highly reactive nanoclusters. Furthermore, our approach showcases how surface restructuring and surface–adsorbate bond breaking can be combined when modeling surface reactions and contributes to the development of an advanced understanding of the nature of active site under reaction conditions.

catalyst dynamic restructuring↗

DOE OSTI2024

Intermittent oxidation kinetics and metal/oxide interfacial undulation

The phenomenon of oxygen-adsorption-induced surface restructuring is widespread across various metal-oxygen systems, yet its impact on initiating bulk oxide formation remains largely unexplored. In this study, through in-situ atomic-resolution electron microscopy observations of surface oxidation of Cu(110) and Cu 85 Au 15 (110), we unveil intermittent oxide-film growth modulated by oxygen-induced surface restructuring. This modulation is evidenced by repeated pinning of Cu 2 O growth front at isolated Cu columns of the c(6×2)-O reconstruction, owing to required long-range diffusion of Cu and O atoms to the Cu 2 O growth front. We reveal that Cu vacancies, generated at the Cu 2 O growth front, are injected into the Cu 2 O/Cu interface, inducing hill-and-valley undulation of the Cu 2 O film. In contrast, atomic vacancies produced during the Cu 85 Au 15 (110) oxidation preferentially migrate into interfaces between Au-rich and Au-poor regions in the bulk, resulting in a flat and adherent Cu 2 O film. These findings demonstrate the critical role of oxygen-induced surface restructuring in modulating oxide-film-growth kinetics and manipulability of the fate of injected vacancies by alloying, thereby offering insights applicable to a broader range of metal-oxygen systems for fine-tuning oxidation kinetics and enhancing oxide/metal interfacial adhesion.

25 ENERGY STORAGE↗

DOE OSTI2022

The complex structural and chemical nature of monolithic U-10Mo fuel and Zr barrier layer

Nanoscale microstructural characterization by advanced transmission electron microscopy techniques on a U-10Mo/Zr barrier layer monolithic fuel plate was performed to evaluate the microstructural evaluation after high burn-up. Gas bubble superlattice evolution, grain restructuring, and evolution of the Zr interaction layer is investigated through detailed electron microscopy characterization. The use of automated crystallographic orientation mapping to irradiated U-10Mo fuel highlights that the restructured ultra-fine grains are separated by high angle grain boundaries at a burn up of 4.42 × 10 21 fissions/cm 3 . Additionally, advanced chemical analysis and multi-variable statistical analysis shows spatial clustering of solid fission product precipitates. Finally, characterization of a newly observed porous nanocrystalline Zr region in the barrier layer is studied. Finally, this work provides insights into the grain subdivision and restructuring process while using advanced microscopy techniques to analyze fission products in neutron-irradiated U-10Mo fuel.

36 MATERIALS SCIENCE↗

DOE OSTI2025

In-situ ion irradiation induced nanograin growth in a spent UO 2 fuel

This study investigates the irradiation-driven evolution of nanograins in the early-stage restructured rim region of medium burnup spent uranium dioxide (UO 2 ) fuel. Transmission electron microscopy (TEM) lamellas prepared from Belgium Reactor 3 (BR-3) fuel were subjected to in-situ 300 keV Xe ion irradiations under varying doses, fluxes, and temperatures to evaluate their effect on the evolution of the nanograins. Our results reveal that the nanograins grow during ion irradiation. Additionally, the growth is most pronounced at elevated temperatures (300 °C), moderate at room temperature, and negligible at cryogenic temperature (−223 °C). This behavior indicates that thermal activation, alongside irradiation effects, is essential to overcome grain boundary pinning by fission gas bubbles, metallic precipitates, and porosity. Furthermore, while nanograins (<200 nm) consistently coarsened under irradiation, larger grains did not undergo further restructuring, which can be attributed to the strong defect annihilation at TEM lamella surfaces combined with the limited electronic stopping power of low energy Xe ions used in this work. These findings highlight the roles of thermal spike effects, defect mobility, and impurity pinning in governing grain evolution in the rim region of spent UO 2 fuel during ion irradiation, providing key insights for predictive models of restructuring and performance of the high burnup nuclear fuel.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2012

Synthesis and characterization of a PbO{sub 2}-clay nanocomposite: Removal of lead from water using montmorillonite

Graphical abstract: The replacement of Na by Pb in the interlayer space of the smectite leads to a decrease in the intensity of the the (0 0 1) reflection as the concentration of lead nitrate increases. A significant restructuring at the particle scale is observed leading probably to the exfoliation of the caly. In addition, the thermal behaviour of the montmorillonite samples with regard to their dehydration and dehydroxilation capacities is significantly influenced. This leads to a lowering of the water content and a decrease in the ionic conductivity of the clay. Highlights: Black-Right-Pointing-Pointer In the clay, Pb replaces Na ions and a significant restructuring at the particle scale is observed. Black-Right-Pointing-Pointer Pb influenced significantly the thermal behaviour of the clay with regard to its dehydration. Black-Right-Pointing-Pointer In the interlayer space, the exchange of Na by Pb leads to a decrease in the protonic conductivity. Black-Right-Pointing-Pointer A PbO{sub 2}-clay nanocomposite material with good conductivity is synthesized. -- Abstract: The aim of this paper is to present the results obtained with Pb(II) sorption on an Algerian Clay. The experiments were carried out using a batch process. Powder X-rays diffraction patterns (PXRD) prove that in the montmorillonite Pb replaces Na ions. A significant restructuring at the particle scale is observed leading to the disappearance of the d{sub 001} reflection of the clay at high concentrations of lead. The replacement of hydrated Na with Pb ions influenced significantly the thermal behaviour of the montmorillonite samples with regard to their dehydration and dehydroxilation capacities with a lowering of the water content. A PbO{sub 2}-clay composite material with good electrical conductivity is synthesized.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Mending cracks atom-by-atom in rutile TiO2 with electron beam radiolysis

Abstract Rich electron-matter interactions fundamentally enable electron probe studies of materials such as scanning transmission electron microscopy (STEM). Inelastic interactions often result in structural modifications of the material, ultimately limiting the quality of electron probe measurements. However, atomistic mechanisms of inelastic-scattering-driven transformations are difficult to characterize. Here, we report direct visualization of radiolysis-driven restructuring of rutile TiO 2 under electron beam irradiation. Using annular dark field imaging and electron energy-loss spectroscopy signals, STEM probes revealed the progressive filling of atomically sharp nanometer-wide cracks with striking atomic resolution detail. STEM probes of varying beam energy and precisely controlled electron dose were found to constructively restructure rutile TiO 2 according to a quantified radiolytic mechanism. Based on direct experimental observation, a “two-step rolling” model of mobile octahedral building blocks enabling radiolysis-driven atomic migration is introduced. Such controlled electron beam-induced radiolytic restructuring can be used to engineer novel nanostructures atom-by-atom.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Atomic dynamics of electrified solid–liquid interfaces in liquid-cell TEM

Electrified solid–liquid interfaces (ESLIs) play a key role in various electrochemical processes relevant to energy, biology and geochemistry. The electron and mass transport at the electrified interfaces may result in structural modifications that markedly influence the reaction pathways. For example, electrocatalyst surface restructuring during reactions can substantially affect the catalysis mechanisms and reaction products. Despite its importance, direct probing the atomic dynamics of solid–liquid interfaces under electric biasing is challenging owing to the nature of being buried in liquid electrolytes and the limited spatial resolution of current techniques for in situ imaging through liquids. Here, with our development of advanced polymer electrochemical liquid cells for transmission electron microscopy (TEM), we are able to directly monitor the atomic dynamics of ESLIs during copper (Cu)-catalysed CO 2 electroreduction reactions (CO 2 ERs). Our observation reveals a fluctuating liquid-like amorphous interphase. It undergoes reversible crystalline–amorphous structural transformations and flows along the electrified Cu surface, thus mediating the crystalline Cu surface restructuring and mass loss through the interphase layer. Furthermore, the combination of real-time observation and theoretical calculations unveils an amorphization-mediated restructuring mechanism resulting from charge-activated surface reactions with the electrolyte. Our results open many opportunities to explore the atomic dynamics and its impact in broad systems involving ESLIs by taking advantage of the in situ imaging capability.

36 MATERIALS SCIENCE↗

DOE OSTI2011

Genome-Scale Analysis of Programmed DNA Elimination Sites in Tetrahymena thermophila

Genetically programmed DNA rearrangements can regulate mRNA expression at an individual locus or, for some organisms, on a genome-wide scale. Ciliates rely on a remarkable process of whole-genome remodeling by DNA elimination to differentiate an expressed macronucleus (MAC) from a copy of the germline micronucleus (MIC) in each cycle of sexual reproduction. Here we describe results from the first highthroughput sequencing effort to investigate ciliate genome restructuring, comparing Sanger long-read sequences from a Tetrahymena thermophila MIC genome library to the MAC genome assembly. With almost 25% coverage of the unique-sequence MAC genome by MIC genome sequence reads, we created a resource for positional analysis of MIC-specific DNA removal that pinpoints MAC genome sites of DNA elimination at nucleotide resolution. The widespread distribution of internal eliminated sequences (IES) in promoter regions and introns suggests that MAC genome restructuring is essential not only for what it removes (for example, active transposons) but also for what it creates (for example, splicing-competent introns). Consistent with the heterogeneous boundaries and epigenetically modulated efficiency of individual IES deletions studied to date, we find that IES sites are dramatically under-represented in the 25% of the MAC genome encoding exons. As an exception to this general rule, we discovered a previously unknown class of small (,500 bp) IES with precise elimination boundaries that can contribute the 39 exon of an mRNA expressed during genome restructuring, providing a new mechanism for expanding mRNA complexity in a developmentally regulated manner.

DNA breakage and joining↗

NASA NTRS1985

Techniques for accommodating control effector failures on a mildly statically unstable airplane

Commercial airplanes are becoming increasingly more sophisticated, placing an increasing burden on pilots to detect and resolve the exhaustive set of possible control effector failures. Automatic techniques are needed to either reconfigure an existing control law or restructure a new control law after failure. A discrete control law has been designed for the longitudinal channel of a mildly statically unstable commercial airplane, to track the glideslope during the approach to landing phase of flight. Single effector failures with time delays for failure detection and identification are analyzed for both the reconfigured and restructured control laws, and results are compared with those from previous research using a statically stable airplane. Strategies considered include reconfiguration and restructuring with new flight conditions. Validation of all cases is made using a 6 DOF nonlinear airplane simulation.

Ostroff, A. J.↗

DOE OSTI2012

IAEA reorganizes nuclear information services

As part of an overall restructuring of the International Atomic Energy Agency's Department of Nuclear Energy, the agency has established the Nuclear Information Section (NIS). The restructuring, recently announced by IAEA Director General Yukiya Amano, also includes the creation of a separate Nuclear Knowledge Management (NKM) Section, as demand for assistance in this area is growing among member countries. According to the NIS Web site, 'This restructuring and the creation of the NIS provides an opportunity for further enhancing existing information products and services and introducing new ones-all with an eye towards advancing higher organizational efficiency and effectiveness.'

99 GENERAL AND MISCELLANEOUS↗

DOE OSTI2018

Retooling a Trade Association in a Challenged Industry: The Nuclear Energy Institute Story - 18503

The U.S. Nuclear industry is facing significant challenges to maintain economic competitiveness in an electricity supply sector where advances in natural gas, wind, and solar technologies are reshaping the marketplace. As clean and reliable baseload generation, nuclear still has a valuable role to play. But in order for the power of the atom to remain available for meeting the nation's energy, environmental, and national security needs, it will be imperative that industry leadership innovate and become more efficient at a pace that matches the competition. Industry leaders rely, to a large extent, on their trade association - the Nuclear Energy Institute (NEI) - to be the prime mover in championing initiatives that will enable a successful future. NEI realized that, in the face of an increasingly difficult economic situation, it must become both leaner and more forward looking - it would have to extend its reach and influence while at the same time reigning in costs to its membership. Therefore, on January 17, 2017 NEI completed a restructuring to improve member value and organizational effectiveness. This restructuring was designed in recognition that the nuclear industry is at a pivotal time, and NEI had a unique opportunity to change its trajectory and underline the importance of nuclear energy's role in the nation's critical infrastructure. NEI is now better positioned to support the existing reactor fleet, promote commercialization of advanced reactors, and drive American leadership in commercial nuclear exports and technology around the world. NEI began this restructuring in the fall of 2016 when it consolidated Government Affairs, Communications, Policy and Public Affairs under a new External Affairs function. The January 2017 action extended that effort across the remainder of the organization, ensuring that the organization is highly aligned, member-focused and results driven. The new NEI takes pride in the fact that it is comprised of talented employees who are passionate about nuclear energy and can make a difference for our membership. With this team in place, NEI looks forward to advancing the interests of the nuclear industry while contributing to a safer, cleaner and more productive world. This paper will examine the details of how this new organization was constructed, provide an overview of the National Nuclear Energy Strategy it developed to guide its efforts, examine the trials and tribulations that come along with disruptive change, and reflect on what has been accomplished in the retooled organizations first year. (authors)

99 GENERAL AND MISCELLANEOUS↗

DOE OSTI2017

Structural Dynamics and Evolution of Bismuth Electrodes during Electrochemical Reduction of CO 2 in Imidazolium-Based Ionic Liquid Solutions

Real-time changes in the composition and structure of bismuth electrodes used for catalytic conversion of CO2 into CO were examined via X-ray absorption spectroscopy (including XANES and EXAFS), electrochemical quartz crystal microbalance (EQCM), and in situ X-ray reflectivity (XR). Measurements were performed with bismuth electrodes immersed in acetonitrile (MeCN) solutions containing a 1-butyl-3-methylimidazolium ([BMIM]+) ionic liquid promoter or electrochemically inactive tetrabutylammonium supporting electrolytes (TBAPF6 and TBAOTf). Altogether, these measurements show that bismuth electrodes are originally a mixture of bismuth oxides (including Bi2O3) and metallic bismuth (Bi0) and that the reduction of oxidized bismuth species to Bi0 is fully achieved under potentials at which CO2 activation takes place. Furthermore, EQCM measurements conducted during cyclic voltammetry revealed that a bismuth-coated quartz crystal exhibits significant shifts in resistance (ΔR) prior to the onset of CO2 reduction near -1.75 V vs Ag/AgCl and pronounced hysteresis in frequency (Δf) and ΔR, which suggests significant changes in roughness or viscosity at the Bi/[BMIM]+ solution interface. In situ XR performed on rhombohedral Bi (001) oriented films indicates that extensive restructuring of the bismuth film cathodes takes place upon polarization to potentials more negative than -1.6 V vs Ag/AgCl, which is characterized by a decrease of the Bi (001) Bragg peak intensity of ≥50% in [BMIM]OTf solutions in the presence and absence of CO2. Over 90% of the reflectivity is recovered during the anodic half-scan, suggesting that the structural changes are mostly reversible. In contrast, such a phenomenon is not observed for thin Bi (001) oriented films in solutions of tetrabutylammonium salts that do not promote CO2 reduction. Overall, these results highlight that Bi electrodes undergo significant potential-dependent chemical and structural transformations in the presence of [BMIM]+-based electrolytes, including the reduction of bismuth oxide to bismuth metal and changes in roughness and near-surface viscosity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Structural and Valence State Modification of Cobalt in CoPt Nanocatalysts in Redox Conditions

Platinum is the primary catalyst for many chemical reactions in the field of heterogeneous catalysis. However, platinum is both expensive and rare. Therefore, it is advantageous to combine Pt with another metal to reduce cost while also enhancing stability. To that end, Pt is often combined with Co to form Co-Pt nanocrystals. However, dynamical restructuring effects that occur during reaction in Co-Pt ensembles can impact catalytic properties. In this study, model Co 2 Pt 3 nanoparticles supported on carbon were characterized during a redox cycle with two in situ approaches, namely X-ray absorption spectroscopy (XAS) and scanning transmission electron microscopy (STEM) using a multimodal microreactor. The sample was exposed to temperatures up to 500 °C under H 2 , and then to O 2 at 300 °C. Irreversible segregation of Co in the Co-Pt particles was seen during redox cycling and substantial changes of the oxidation state of Co were observed. After the H 2 treatment, a fraction of Co could not be fully reduced and incorporated into a mixed Co-Pt phase. Re-oxidation of the sample increased Co segregation, and the segregated material had a different valence state than in the fresh, oxidized sample. Furthermore, this in situ study describes dynamical restructuring effects in CoPt nano-catalysts at the atomic scale that are crucial to understand to improve the design of catalysts used in major chemical processes.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Observing structural reorientations at solvent–nanoparticle interfaces by X-ray diffraction – putting water in the spotlight

Nanoparticles are attractive in a wide range of research genres due to their size-dependent properties, which can be in contrast to those of micrometre-sized colloids or bulk materials. This may be attributed, in part, to their large surface-to-volume ratio and quantum confinement effects. There is a growing awareness that stress and strain at the particle surface contribute to their behaviour and this has been included in the structural models of nanoparticles for some time. One significant oversight in this field, however, has been the fact that the particle surface affects its surroundings in an equally important manner. It should be emphasized here that the surface areas involved are huge and, therefore, a significant proportion of solvent molecules are affected. Experimental evidence of this is emerging, where suitable techniques to probe the structural correlations of liquids at nanoparticle surfaces have only recently been developed. The recent validation of solvation shells around nanoparticles has been a significant milestone in advancing this concept. Restructured ordering of solvent molecules at the surfaces of nanoparticles has an influence on the entire panoply of solvent–particle interactions during, for example, particle formation and growth, adhesion forces in industrial filtration, and activities of nanoparticle–enzyme complexes. This article gives an overview of the advances made in solvent–nanoparticle interface research in recent years: from description of the structure of bulk solids and liquids via macroscopic planar surfaces, to the detection of nanoscopic restructuring effects. Water–nanoparticle interfaces are given specific attention to illustrate and highlight their similarity to biological systems.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Integrating Renewable Generation into Grid Operations: Four International Experiences

International experiences with power sector restructuring and the resultant impacts on bulk power grid operations and planning may provide insight into policy questions for the evolving United States power grid as resource mixes are changing in response to fuel prices, an aging generation fleet and to meet climate goals. Australia, Germany, Japan and the UK were selected to represent a range in the level and attributes of electricity industry liberalization in order to draw comparisons across a variety of regions in the United States such as California, ERCOT, the Southwest Power Pool and the Southeast Reliability Region. The study draws conclusions through a literature review of the four case study countries with regards to the changing resource mix and the electricity industry sector structure and their impact on grid operations and planning. This paper derives lessons learned and synthesizes implications for the United States based on answers to the above questions and the challenges faced by the four selected countries. Each country was examined to determine the challenges to their bulk power sector based on their changing resource mix, market structure, policies driving the changing resource mix, and policies driving restructuring. Each countries’ approach to solving those changes was examined, as well as how each country’s market structure either exacerbated or mitigated the approaches to solving the challenges to their bulk power grid operations and planning. All countries’ policies encourage renewable energy generation. One significant finding included the low- to zero-marginal cost of intermittent renewables and its potential negative impact on long-term resource adequacy. No dominant solution has emerged although a capacity market was introduced in the UK and is being contemplated in Japan. Germany has proposed the Energy Market 2.0 to encourage flexible generation investment. The grid operator in Australia proposed several approaches to maintaining synchronous generation. Interconnections to other regions provides added opportunities for balancing that would not be available otherwise, and at this point, has allowed for integration of renewables.

24 POWER TRANSMISSION AND DISTRIBUTION↗

DOE OSTI2025

In-situ/operando study of Cu-based nanocatalysts for CO 2 electroreduction using electrochemical liquid cell TEM

The structure of a nanocatalyst during electrocatalytic reactions often deviates from its pristine structure due to intrinsic properties, or physical and chemical adsorption at the catalytic surfaces. Taking Cu-based catalysts for CO 2 electroreduction reactions (CO 2 RR) as an example, they often experience segregation, leaching, and alloying during reactions. With the recent breakthrough development of high-resolution polymer electrochemical liquid cells, in-situ electrochemical liquid cell transmission electron microscopy (EC-TEM) alongside other advanced microscopy techniques, has become a powerful platform for revealing electrocatalysts restructuring at the atomic level. Considering the complex reactions involving electrified solid-liquid interfaces and catalyst structural evolution with intermediates, systematic studies with multimodal approaches are crucial. In this article, we demonstrate a research protocol for the study of electrocatalysts structural evolution during reactions using the in-situ EC-TEM platform. Using Cu and CuAg nanowire catalysts for CO 2 RR as model systems, we describe the experimental procedures and findings. We highlight the platform’s crucial role in elucidating atomic-scale pathways of nanocatalyst restructuring and identifying catalytic active sites, as well as avoiding potential artifacts to ensure unbiased conclusions. Using the multimodal characterization toolbox, we provide the opportunity to correlate the structure of a working catalyst with its performance. Finally, we discuss advancements as well as the remaining gap in elucidating the structural-performance relationship of working catalysts. We expect this article will assist in establishing guidelines for future investigations of complex electrochemical reactions, such as CO 2 RR and other catalytic processes, using the in-situ EC-TEM platform.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗