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At least 163 records · Page 9

Exploring dynamic surface processes during silicate mineral (wollastonite) dissolution with liquid cell

Most liquid cell transmission electron microscopy (LC TEM) studies focus on nanoparticles or nanowires, in large part because the preparation and study of materials in this size range is straightforward. By contrast, this is not true for samples in the micrometre size range, in large part because of the difficulties associated with sample preparation starting from a ‘bulk’ material. There are also many advantages inherent to the study of micrometre-sized samples compared to their nanometre-sized counterparts. Here, we present a liquid cell transmission electron study that employed an innovative sample preparation technique using focused ion beam (FIB) milling to fabricate micrometre-sized electron transparent lamellae that were then welded to the liquid cell substrate. This technique, for which we have described in detail all of the fabrication steps, allows for samples having dimensions of several square micrometres to be observed by TEM in situ in a liquid. We applied this technique to test whether we could observe and measure in situ dissolution of a crystalline material called wollastonite, a calcium silicate mineral. More specifically, this study was used to observe and record surface dynamics associated with step and terrace edge movement, which are ultimately linked to the overall rate of dissolution. The wollastonite lamella underwent chemical reactions in pure deionized water at ambient temperature in a liquid cell with a 5-math formulam-spacer thickness. The movement of surface steps and terraces was measured periodically over a period of almost 5 h. Quite unexpectedly, the one-dimensional rates of retreat of these surface features were not constant, but changed over time. In addition, there were noticeable quantitative differences in retreat rates as a function crystallographic orientation, indicating that surface retreat is anisotropic. Several bulk rates of dissolution were also determined (1.6–4.2 • 10 -7 mol m -2 s -1 ) using the rates of retreat of representative terraces and steps, and were found to be within one order of magnitude of dissolution rates in the literature based on aqueous chemistry data.

36 MATERIALS SCIENCE↗

Multiphasic size-dependent growth dynamics of nanoparticle ensembles

Colloidal nanoparticles are of great interest in modern science and industry. However, the thermodynamic mechanism and dynamics of nanoparticle growth have yet to be understood. Addressing these issues, we tracked hundreds of in-situ growth trajectories of a nanoparticle ensemble using liquid-phase TEM and found that the nanoparticle growth, including coalescence, exhibits nanoparticle size-dependent multiphasic dynamics, unexplainable by current theories. Motivated by this finding, we developed a model and theory for an ensemble of growing nanoparticles, providing a unified, quantitative understanding of the time-dependent mean and fluctuation of nanoparticle size and size-dependent growth rate profiles across various nanoparticle systems and experimental conditions. Our work reveals that the chemical potential in a small nanoparticle strongly deviates from the Gibbs-Thomson equation, shedding light on how it governs the size-dependent growth dynamics of nanoparticles.

Kim, Ji-Hyun↗

A comparative analysis of YOLOv8 and U-Net image segmentation approaches for transmission electron micrographs of polycrystalline thin films

Metallic thin films offer a platform to experimentally study the dynamics of microstructural evolution, but the required transmission electron microscopy (TEM)-based imaging generates complex images that are challenging to segment and quantify. This work provides a comparative analysis of a new YOLOv8 model and an established U-Net model for bright-field TEM images of polycrystals, employing a framework leveraging physical observables to evaluate performance against two hand-traced benchmark datasets. This methodology obviates the comparison of large, diversely structured, and manually labeled datasets that are required to assess performance on a per-image/per-pixel basis. It is found that the YOLOv8 model, adapted for real-time instance segmentation, has up to 43× faster inferencing (NVIDIA GeForce RTX 4090) compared to U-Net and reconstructs hand-traced grain size distributions (GSDs) with excellent fidelity, finding mean diameter within 3% for grains near an optimal magnification; for grains that deviate from the optimal pixel-diameter, the size of small- (large)-diameter grains is systematically over- (under)-estimated. This is partially mitigated by including scale-aware augmentations during training. Moreover, when the bias is corrected post-inference by a rigid shift in distribution, the YOLOv8 model reproduces ground truth GSDs with exceptional fidelity, with statistical tests indicating <5% probability that the distributions are distinct. Based on ground truth data, calibration curves pertaining to this shift can be constructed for a given model. This issue is not present in the U-Net model’s results, indicating that for quantitative measurements where the true size of objects is of interest, special procedures must be implemented for YOLO-based models.

36 MATERIALS SCIENCE↗

2D-EFICACY: Control of Metastable 2D Carbide[1]Chalcogenide Heterolayers: Strain and Moire Engineering

The experimental isolation of graphene led to the discovery of an entirely new world of two-dimensional (2D) materials in which the 2D nature often leads to emergent behaviors not seen in bulk systems. 2D transition metal dichalcogenides (TMDs) exhibit physico-chemical properties that depend on the transition metal, polymorph, thickness, and presence and type of defects. Recently, a group of thin (10-100nm) transition metal carbides (TMCs), such as Mo2C, has been synthesized that exhibit a thickness-dependent superconducting critical temperature (Tc). These thin TMCs are different from MXenes, another class of 2D materials consisting of few layers of nitrides or carbides (<5nm) produced by chemical etching and delamination. The goal of this renewal proposal is to combine experiment and computation to synthesize and elucidate the guiding principles that control the growth, orientation and strain of heterostacks of thin TMCs and TMDs composed with Nb, Ti and W. We expect to stabilize metastable hybrid phases of TMCs sandwiched between TMDs (H-TMD/Cs) with unprecedented physico-chemical properties. As part of previous DOE-funded work by the Terrones/Sinnott groups, thin (10-100 nm thick) Mo2C flakes were successfully synthesized by chemical vapor deposition (CVD). By subsequently exposing Mo2C to H2S, partial chalcogenization was achieved, resulting in heterostacks of MoCx phases and MoS2. The formation of MoS2 led to a deficiency of Mo atoms in the underlying Mo2C, resulting in an inhomogeneous phase change from α-Mo2C to γ’-MoCx and then to γ-MoC. The γ’-MoCx is a strained metastable phase and the heterostack of all three phases demonstrated an increased Tc relative to that of α-Mo2C, from 4 to 6K; its interleaved layered structure consisting of superconducting and semiconducting phases is ideal for future studies of Josephson junction series arrays. Moiré patterns in these heterostacked systems could result in new phenomena, as moiré patterns in bilayer graphene showed unconventional superconductivity and moiré excitons have been observed in twisted TMD heterobilayers. The scientific hypothesis of the proposed synergistic computational and experimental research is that orientation and strain control within confined thin metastable TMCs, sandwiched by stable phases of TMCs and layered TMDs, will depend on kinetic and thermodynamic “knobs” that include fast temperature changes, chalcogen diffusion through preferred crystallographic planes, reaction times, pressure, reactive atmosphere, precursors, and surfactants, which will also tailor properties such as superconductivity, magnetism, ferroelectricity, piezoelectricity, and catalytic performance. We will develop the guiding principles for the synthesis and stabilization of metastable H-TMD/Cs based on Nb, Ti and W. In order to validate the hypothesis, four tasks are proposed: The first task will synthesize ultra-thin TMCs based on Nb, W and Ti, by: 1) adapting the CVD method used for Mo2C, 2) plasma assisted CVD, 3) defect-mediated CVD processes, and 4) cryo-milling of carbide powders. The second task will accomplish the synthesis and basic physico-chemical characterizations of H-TMD/Cs by chalcogenization of the materials synthesized in task one, and by carbonization of TMDs. H-TMD/Cs will also be investigated for their suitability in energy conversion applications such as supercapacitors, Li and multivalent ion batteries, and electrocatalysts, topics of interest to DoE. These tasks will be carried out in close conjunction with density functional theory (DFT) calculations with insights into energetics, lattice parameters, stability, phase diagrams, band structures, and density of states of H-TMD/Cs. The third task will characterize and evaluate strain and moiré patterns at the interfaces of different H-TMD/Cs by high-resolution scanning transmission electron microscopy (HR-STEM), scanning tunneling microscopy (STM), and conductive tip atomic force microscopy. Nudged elastic band calculations with DFT will be performed to understand the chalcogen diffusion process, which will provide insights into the interfaces between different phases of TMCs and TMDs. The fourth task aims at quantifying the stability and dynamics of H-TMD/Cs by in-situ TEM and Raman studies under heating, strain, and electrical biasing. Phonon calculations using DFT will provide a basis for interpreting Raman spectra. This coherent framework involving synthesis, characterization, and computation will result in a broad scientific impact for energy related applications. The ability to develop new H-TMD/Cs will enhance a range of applications that include batteries, catalysts, switches, sensors, quantum computing components and smart coatings.

2-Dimensional materials↗

2D-EFICACY: Control of Metastable 2D Carbide Chalcogenide Heterolayers: Strain and Moire Engineering

The experimental isolation of graphene led to the discovery of an entirely new world of two-dimensional (2D) materials in which the 2D nature often leads to emergent behaviors not seen in bulk systems. 2D transition metal dichalcogenides (TMDs) exhibit physico-chemical properties that depend on the transition metal, polymorph, thickness, and presence and type of defects. Recently, a group of thin (10-100nm) transition metal carbides (TMCs), such as Mo 2 C, has been synthesized that exhibit a thickness-dependent superconducting critical temperature (Tc). These thin TMCs are different from MXenes, another class of 2D materials consisting of few layers of nitrides or carbides (<5nm) produced by chemical etching and delamination. The goal of this renewal proposal is to combine experiment and computation to synthesize and elucidate the guiding principles that control the growth, orientation and strain of heterostacks of thin TMCs and TMDs composed with Nb, Ti and W. We expect to stabilize metastable hybrid phases of TMCs sandwiched between TMDs (H-TMD/Cs) with unprecedented physico-chemical properties. As part of previous DOE-funded work by the Terrones/Sinnott groups, thin (10-100 nm thick) Mo 2 C flakes were successfully synthesized by chemical vapor deposition (CVD). By subsequently exposing Mo 2 C to H 2 S, partial chalcogenization was achieved, resulting in heterostacks of MoCx phases and MoS 2 . The formation of MoS 2 led to a deficiency of Mo atoms in the underlying Mo 2 C, resulting in an inhomogeneous phase change from α-Mo 2 C to γ’-MoCx and then to γ-MoC. The γ’-MoCx is a strained metastable phase and the heterostack of all three phases demonstrated an increased Tc relative to that of α-Mo 2 C, from 4 to 6K; its interleaved layered structure consisting of superconducting and semiconducting phases is ideal for future studies of Josephson junction series arrays. Moiré patterns in these heterostacked systems could result in new phenomena, as moiré patterns in bilayer graphene showed unconventional superconductivity and moiré excitons have been observed in twisted TMD heterobilayers. The scientific hypothesis of the proposed synergistic computational and experimental research is that orientation and strain control within confined thin metastable TMCs, sandwiched by stable phases of TMCs and layered TMDs, will depend on kinetic and thermodynamic “knobs” that include fast temperature changes, chalcogen diffusion through preferred crystallographic planes, reaction times, pressure, reactive atmosphere, precursors, and surfactants, which will also tailor properties such as superconductivity, magnetism, ferroelectricity, piezoelectricity, and catalytic performance. We will develop the guiding principles for the synthesis and stabilization of metastable H-TMD/Cs based on Nb, Ti and W. In order to validate the hypothesis, four tasks are proposed: The first task will synthesize ultra-thin TMCs based on Nb, W and Ti, by: 1) adapting the CVD method used for Mo 2 C, 2) plasma assisted CVD, 3) defect-mediated CVD processes, and 4) cryo-milling of carbide powders. The second task will accomplish the synthesis and basic physico-chemical characterizations of H-TMD/Cs by chalcogenization of the materials synthesized in task one, and by carbonization of TMDs. H-TMD/Cs will also be investigated for their suitability in energy conversion applications such as supercapacitors, Li and multivalent ion batteries, and electrocatalysts, topics of interest to DoE. These tasks will be carried out in close conjunction with density functional theory (DFT) calculations with insights into energetics, lattice parameters, stability, phase diagrams, band structures, and density of states of H-TMD/Cs. The third task will characterize and evaluate strain and moiré patterns at the interfaces of different H-TMD/Cs by high-resolution scanning transmission electron microscopy (HR-STEM), scanning tunneling microscopy (STM), and conductive tip atomic force microscopy. Nudged elastic band calculations with DFT will be performed to understand the chalcogen diffusion process, which will provide insights into the interfaces between different phases of TMCs and TMDs. The fourth task aims at quantifying the stability and dynamics of H-TMD/Cs by in-situ TEM and Raman studies under heating, strain, and electrical biasing. Phonon calculations using DFT will provide a basis for interpreting Raman spectra. This coherent framework involving synthesis, characterization, and computation will result in a broad scientific impact for energy related applications. The ability to develop new H-TMD/Cs will enhance a range of applications that include batteries, catalysts, switches, sensors, quantum computing components and smart coatings.

2-Dimensional Materials↗

Sample Preparation and Experimental Design for In Situ Multi-Beam Transmission Electron Microscopy Irradiation Experiments

We discuss the need to understand materials exposed to overlapping extreme environments such as high temperature, radiation, or mechanical stress. When these stressors are combined there may be synergistic effects that enable unique microstructural evolution mechanisms to activate. Understanding of these mechanisms is necessary for the input and refinement of predictive models and critical for engineering of next generation materials. The basic physics and underlying mechanisms require advanced tools to be investigated. The in situ ion irradiation transmission electron microscope (I 3 TEM) is designed to explore these principles. To quantitatively probe the complex dynamic interactions in materials, careful preparation of samples and consideration of experimental design is required. Particular handling or preparation of samples can easily introduce damage or features that obfuscate the measurements. There is no one correct way to prepare a sample; however, many mistakes can be made. The most common errors and things to consider are highlighted within. The I 3 TEM has many adjustable variables and a large potential experimental space, therefore it is best to design experiments with a specific scientific question or questions in mind. Experiments have been performed on large number of sample geometries, material classes, and with many irradiation conditions. The following are a subset of examples that demonstrate unique in situ capabilities utilizing the I 3 TEM. Au nanoparticles prepared by drop casting have been used to investigate the effects of single ion strikes. Au thin films have been used in studies on the effects of multibeam irradiation on microstructure evolution. Zr films have been exposed to irradiation and mechanical tension to examine creep. Ag nanopillars were subjected to simultaneous high temperature, mechanical compression, and ion irradiation to study irradiation induced creep as well. These results impact fields including: structural materials, nuclear energy, energy storage, catalysis, and microelectronics in space environments.

47 OTHER INSTRUMENTATION↗

Direct Observation of Defect Range and Evolution in Ion-Irradiated Single Crystalline Ni and Ni Binary Alloys

We report that energetic ions have been widely used to evaluate the irradiation tolerance of structural materials for nuclear power applications and to modify material properties. It is important to understand the defect production, annihilation and migration mechanisms during and after collision cascades. In this study, single crystalline pure nickel metal and single-phase concentrated solid solution alloys of 50%Ni50%Co (NiCo) and 50%Ni50%Fe (NiFe) without apparent preexisting defect sinks were employed to study defect dynamics under ion irradiation. Both cross-sectional transmission electron microscopy characterization (TEM) and Rutherford backscattering spectrometry channeling (RBS-C) spectra show that the range of radiation-induced defect clusters far exceed the theoretically predicted depth in all materials after high-dose irradiation. Defects in nickel migrate faster than in NiCo and NiFe. Both vacancy-type stacking fault tetrahedra (SFT) and interstitial loops coexist in the same region, which is consistent with molecular dynamics simulations. Kinetic activation relaxation technique (k-ART) simulations for nickel showed that small vacancy clusters, such as di-vacancies and tri-vacancies, created by collision cascades are highly mobile, even at room temperature. The slower migration of defects in the alloy along with more localized energy dissipation of the displacement cascade may lead to enhanced radiation tolerance.

36 MATERIALS SCIENCE↗

Impacts of Climate Change on Biofuels Production

The overall goal of this research project was to improve and use our biogeochemistry model, TEM, to simulate the effects of climate change and other environmental changes on the production of biofuel feedstocks. We used the improved version of TEM that is coupled with the economic model, EPPA, a part of MIT’s Earth System Model, to explore how alternative uses of land, including land for biofuels production, can help society meet proposed climate targets. During the course of this project, we have made refinements to TEM that include development of a more mechanistic plant module, with improved ecohydrology and consideration of plant-water relations, and a more detailed treatment of soil nitrogen dynamics, especially processes that add or remove nitrogen from ecosystems. We have documented our changes to TEM and used the model to explore the effects on production in land ecosystems, including changes in biofuels production.

09 BIOMASS FUELS↗

Interfacial Microstructural Evolution and Metallurgical Bonding Mechanisms for IN718 Superalloy Joint Produced by Hot Compressive Bonding

The novel metallurgical joining process for bonding IN718 superalloy was investigated by hot compressive bonding (HCB) process under the deformation temperature range of 1000 °C to 1150 °C and true strains ranging from 0 to 0.5 at a strain rate of 0.001 s{sup −1}. The effect of HCB process parameters on the tensile strength was analyzed. Both the as-deformed and the interfacial microstructures were characterized using the optical microscope, electron backscattered diffraction and transmission electron microscope (TEM) analysis. The results of tensile property revealed that the degree of metallurgical bonding is promoted by increasing deformation temperature and strain. The evolution of the interfacial microstructure showed that the migration of interfacial grain boundary (IGB), which is characterized by discontinuous dynamic recrystallization, is the dominant metallurgical bonding mechanism in the early stages of bonding. TEM analysis indicated that the dislocation density is distributed heterogeneously over both sides of IGB, which is the significant reason for the migration of IGB, during the initial stage of HCB process.

36 MATERIALS SCIENCE↗

Evaluating Cryo–TEM Reconstruction Accuracy of Self–Assembled Polymer Nanostructures

Cryogenic transmission electron microscopy (cryo–TEM) combined with single particle analysis (SPA) is an emerging imaging approach for soft materials. However, the accuracy of SPA–reconstructed nanostructures, particularly those formed by synthetic polymers, remains uncertain due to potential packing heterogeneity of the nanostructures. In this study, the combination of molecular dynamics (MD) simulations and image simulations is utilized to validate the accuracy of cryo–TEM 3D reconstructions of self–assembled polypeptoid fibril nanostructures. Using CryoSPARC software, image simulations, 2D classifications, ab initio reconstructions, and homogenous refinements are performed. By comparing the results with atomic models, the recovery of molecular details is assessed, heterogeneous structures are identified, and the influence of extraction location on the reconstructions is evaluated. In conclusion, these findings confirm the fidelity of single particle analysis in accurately resolving complex structural characteristics and heterogeneous structures, exhibiting its potential as a valuable tool for detailed structural analysis of synthetic polymers and soft materials.

36 MATERIALS SCIENCE↗

Modeling of dislocation channel width evolution in irradiated metals

Defect-free dislocation channel formation has been reported to promote plastic instability during tensile testing via localized plastic flow, leading to a distinct loss of ductility and strain hardening in many low-temperature irradiated materials. In order to study the underlying mechanisms governing dislocation channel width and formation, the channel formation process is modeled via a simple stochastic dislocation-jog process dependent upon grain size, defect cluster density, and defect size. Dislocations traverse a field of defect clusters and jog stochastically upon defect interaction, forming channels of low defect-density. And based upon prior molecular dynamics (MD) simulations and in-situ experimental transmission electron microscopy (TEM) observations, each dislocation encounter with a dislocation loop or stacking fault tetrahedron (SFT) is assumed to cause complete absorption of the defect cluster, prompting the dislocation to jog up or down by a distance equal to half the defect cluster diameter. Channels are predicted to form rapidly and are comparable to reported TEM measurements for many materials. Predicted channel widths are found to be most strongly dependent on mean defect size and correlated well with a power law dependence on defect diameter and density, and distance from the dislocation source. Due to the dependence of modeled channel width on defect diameter and density, maximum channel width is predicted to slowly increase as accumulated dose increases. The relatively weak predicted dependence of channel formation width with distance, in accordance with a diffusion analogy, implies that after only a few microns from the source, most channels observed via TEM analyses may not appear to vary with distance because of limitations in the field-of-view to a few microns. Furthermore, examinations of the effect of the so-called “source-broadening” mechanism of channel formation showed that its effect is simply to add a minimum thickness to the channel without affecting channel dependence on the given parameters.

36 MATERIALS SCIENCE↗

In-situ irradiation of uranium carbide

Uranium carbide (UC) is a leading candidate fuel for Generation IV reactors due to its high uranium density and thermal conductivity. However, its irradiation performance—particularly gas bubble swelling and defect dynamics—remains poorly characterized. Using in-situ transmission electron microscopy (TEM), we irradiated UC with 300 keV Xe + and 1 MeV Kr 2+ ions at temperatures up to 900 °C to quantify swelling behavior and dislocation loop evolution. The swelling remained below 0.6 % across all temperatures, suggesting the dimensional stability of UC under irradiation at these temperatures. Dislocation loops grew faster in UC than in UO 2 or UN, correlating with its lower homologous temperature. Notably, nanograin structures emerged in thin regions of the lamellar, mirroring phenomena previously observed in UO 2 and ZrC. These results address critical knowledge gaps in the radiation tolerance of UC and provide insight into its suitability for advanced reactor systems.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Deterministic Ferroelastic Domain Switching Using Ferroelectric Bilayers

Composition gradients, or dissimilar ferroelectric bilayers, demonstrate colossal electromechanical figures of merit attributed to the motion of ferroelastic domain walls. Yet, mechanistic understanding of polarization switching pathways that drive ferroelastic switching in these systems remains elusive. Here, the crucial roles of strain and electrostatic boundary conditions in ferroelectric bilayer systems are revealed, which underpin their ferroelastic switching dynamics. Using in situ electrical biasing in the transmission electron microscope (TEM), the motion of ferroelastic domain walls is investigated in a tetragonal (T) Pb(Zr,Ti)O 3 (PZT)/rhombohedral (R) PZT epitaxial bilayer system. Atomic resolution electron microscopy, in tandem with phase field simulations, indicates that ferroelastic switching is triggered by predominant nucleation at the triple domain junctions located at the interface between the T/R layers. Furthermore, this interfacial nucleation leads to systematic reversable reorientation of ferroelastic domain walls. Finally, deterministic ferroelastic domain switching, driven by the interfacial strain and electrostatic boundary conditions in the ferroelectric bilayer, provides a viable pathway toward novel design of miniaturized energy-efficient electromechanical devices.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Thermoelectric magnetic flows in melt during directional solidification

Thermoelectric magnetic (TEM) flows in melts, which are generated by TEM forces in liquids, were uncovered by the shape evolution of the planar solid/liquid interface during directional solidification. The solid/liquid interface developing from an initially tilted shape to a nearly flat one has been in situ and real-time observed by means of synchrotron X-ray radiography. The corresponding numerical 3D simulations and velocity measurements of flows in the melt confirm that TEM flows exist and respond to this interface shape change. This observation provides visible evidence for TEM flows in melt and their influence on the solid/liquid interface dynamics when directional solidification is conducted in a magnetic field.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Simulating Space Weathering in the Transmission Electron Microscope via Dynamic in Situ Heating and Helium Irradiation of Olivine

The chemical composition, microstructure, and optical properties of grains on the surfaces of airless bodies are predominantly altered by micrometeorite impacts and solar wind irradiation. These processes drive space weathering and result in the formation of features including chemically-altered, amorphous grain rims, Fe nanoparticles (npFe), and vesiculated grain textures. These characteristics have been identified in returned samples from the surfaces of the Moon and asteroid Itokawa. In order to advance our understanding of the formation of these microstructural and chemical features in returned samples, we have simulated space weathering processes for a variety of materials via laboratory experiments. These experiments include ion irradiation to simulate solar wind exposure and laser irradiation and in situ heating to simulate micrometeorite impacts. While these experiments have provided considerable insight into the formation mechanisms of many space weathering features, they are predominantly static and typically performed separately. Here we present results from the simulated space weathering of olivine grains via He irradiation and dynamic heating, both performed in situ inside the transmission electron microscope (TEM). These experiments allow for the real-time observation of chemical and microstructural changes resulting from the superposed effects of ion irradiation and pulsed heating.

Thompson, M. S.↗

Tutorial on In Situ and Operando (Scanning) Transmission Electron Microscopy for Analysis of Nanoscale Structure–Property Relationships

In situ and operando (scanning) transmission electron microscopy [(S)TEM] is a powerful characterization technique that uses imaging, diffraction, and spectroscopy to gain nano-to-atomic scale insights into the structure–property relationships in materials. This technique is both customizable and complex because many factors impact the ability to collect structural, compositional, and bonding information from a sample during environmental exposure or under application of an external stimulus. In the past two decades, in situ and operando (S)TEM methods have diversified and grown to encompass additional capabilities, higher degrees of precision, dynamic tracking abilities, enhanced reproducibility, and improved analytical tools. Much of this growth has been shared through the community and within commercialized products that enable rapid adoption and training in this approach. This tutorial aims to serve as a guide for students, collaborators, and nonspecialists to learn the important factors that impact the success of in situ and operando (S)TEM experiments and assess the value of the results obtained. As this is not a step-by-step guide, readers are encouraged to seek out the many comprehensive resources available for gaining a deeper understanding of in situ and operando (S)TEM methods, property measurements, data acquisition, reproducibility, and data analytics.

(S)TEM↗

Aggregation of cyclic polypeptoids bearing zwitterionic end-groups with attractive dipole–dipole and solvophobic interactions: a study by small-angle neutron scattering and molecular dynamics simulation

Aggregation behavior of cyclic polypeptoids bearing zwitterionic end-groups in methanol has been studied using a combination of experimental and simulation techniques. Here, the data from SANS and cryo-TEM indicate that the solution contains small clusters of these cyclic polypeptoids, ranging from a single polypeptoid chain to small oligomers, while the linear counterpart shows no cluster formation. Atomistic molecular dynamics simulations reveal that the driving force for this clustering behavior is due to the interplay between the effective repulsion due to the solvation of the dipoles formed by the charged end-groups in each polypeptoid chain and the attractive forces due to dipole–dipole interactions and the solvophobic effect.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗