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At least 343 records · Page 19

Understanding Interfacial Electrochemical Reactions through in situ ec-STEM and IL-Cryo-STEM

A major criterion in the design of next generation materials for electrical energy storage applications is a comprehensive understanding of interfacial electrochemical reactions as well as correlating the structure and chemistry across site-specific electrode/electrolyte interfaces with electron, charge, and mass transport processes as they govern performance characteristics. Scanning transmission electron microscopy (STEM) based techniques have emerged as an indispensable materials characterization tool that provides high spatial resolution imaging and chemical analysis and has been effectively utilized to obtain an atomic to nanoscale view of the interfacial structure before and after electrochemical cycling. More recently, there have been several advances that now allows us to obtain more detailed mechanistic insight into evolving reactions through in situ ec-STEM and electrical biasing platforms such as in the understanding of the mechanisms of solid electrolyte interphase formation, lithium dendrite nucleation and growth mechanisms and ionic transport mechanisms within intercalation, conversion, and alloying electrode materials. Several major advantages of the in situ ec-STEM approach is the quantitative electrochemical measurement of charge passed during cycling with simultaneous analysis of the electrochemical processes with STEM imaging and diffraction. Here, while spectroscopic analysis of the electrochemical reactions products has been performed, there is the issue of beam sensitivity and therefore, Cryo-STEM imaging combined with electron energy loss spectroscopy (EELS) techniques have been employed to analyze the chemistry of the SEI and Li dendrites. In this talk, we discuss the potential for combining identical location (IL) STEM techniques with Cryo-EM. The advantage of using this approach is that the sample is placed on a conventional TEM grid and the exact same location of the specimen can be analyzed before and after quantitative electrochemical measurements. Moreover, since the sample is on the TEM grid, the grid itself can be prepared for further Cryo-TEM experiments by plunge freezing in liquid nitrogen then transferred to the Cryo-TEM under liquid nitrogen. Results obtain from these experiments can be used to enhance our scientific understanding of interfacial chemistry at electrode/electrolyte interfaces and may be useful in the design of new materials.

36 MATERIALS SCIENCE↗

In Situ Transmission Electron Microscopy: Signal processing challenges and examples

Transmission electron microscopy (TEM) is a powerful tool for imaging material structure and characterizing material chemistry. Recent advances in data collection technology for TEM have enabled high-volume and high-resolution data collection at a microsecond frame rate. Here, taking advantage of these advances in data collection rates requires the development and application of data processing tools, including image analysis, feature extraction, and streaming data processing techniques. In this article, we highlight a few areas in materials science that have benefited from combining signal processing and statistical analysis with data collection capabilities in TEM and present a future outlook on opportunities of integrating signal processing with automated TEM data analysis.

36 MATERIALS SCIENCE↗

Temperature-induced degradation of GaN HEMT: An in situ heating study

High-power electronics, such as GaN high electron mobility transistors (HEMTs), are expected to perform reliably in high-temperature conditions. This study aims to gain an understanding of the microscopic origin of both material and device vulnerabilities to high temperatures by real-time monitoring of the onset of structural degradation under varying temperature conditions. This is achieved by operating GaN HEMT devices in situ inside a transmission electron microscope (TEM). Electron-transparent specimens are prepared from a bulk device and heated up to 800 °C. High-resolution TEM (HRTEM), scanning TEM (STEM), energy-dispersive x-ray spectroscopy (EDS), and geometric phase analysis (GPA) are performed to evaluate crystal quality, material diffusion, and strain propagation in the sample before and after heating. Gate contact area reduction is visible from 470 °C accompanied by Ni/Au intermixing near the gate/AlGaN interface. Elevated temperatures induce significant out-of-plane lattice expansion at the SiNx/GaN/AlGaN interface, as revealed by geometry-phase GPA strain maps, while in-plane strains remain relatively consistent. Exposure to temperatures exceeding 500 °C leads to almost two orders of magnitude increase in leakage current in bulk devices in this study, which complements the results from our TEM experiment. The findings of this study offer real-time visual insights into identifying the initial location of degradation and highlight the impact of temperature on the bulk device’s structure, electrical properties, and material degradation.

36 MATERIALS SCIENCE↗

Investigation of the thermal decomposition of Pu(IV) oxalate: a transmission electron microscopy study

The degradation of the internal structure of plutonium (IV) oxalate during calcination was investigated with Transmission Electron Microscopy (TEM), electron diffraction, Electron Energy-Loss Spectroscopy (EELS), and 4D Scanning TEM (STEM). TEM lift-outs were prepared from samples that had been calcined at 300°C, 450°C, 650°C and 950°C. The resulting phase at all calcination temperatures was identified as PuO 2 with electron diffraction. The grain size range was obtained with high-resolution TEM. In addition, 4D STEM images were analyzed to provide grain size distributions. In the 300°C calcined sample, the grains were <10 nm in diameter, at 650°C, the grains ranged from 10 to 20 nm, and by 950°C, the grains were 95–175 nm across. Using the Kolmogorov-Smirnov (K-S) two sample test, it was shown that morphological measurements obtained from 4D-STEM provided statistically significant distributions to distinguish samples at the different calcination conditions. Using STEM-EELS, carbon was shown to be present in the low temperature calcined samples associated with oxalate but had formed carbon (possibly graphite) deposits in the 950°C calcined sample. This work highlights the new methods of STEM-EELS and 4D-STEM for studying the internal structure of special nuclear materials (SNM).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Mixing states of Amazon basin aerosol particles transported over long distances using transmission electron microscopy

The Amazon basin is important for understanding the global climate because of its carbon cycle and as a laboratory for obtaining basic knowledge of the continental background atmosphere. Aerosol particles play an important role in the climate and weather, and knowledge of their compositions and mixing states is necessary to understand their influence on the climate. For this study, we collected aerosol particles from the Amazon basin during the Green Ocean Amazon (GoAmazon2014/5) campaign (February to March 2014) at the T3 site, which is located about 70 km from Manaus, and analyzed them using transmission electron microscopy (TEM). TEM has better spatial resolution than other instruments, which enables us to analyze the occurrences of components that attach to or are embedded within other particles. Based on the TEM results of more than 10 000 particles from several transport events, this study shows the occurrences of individual particles including compositions, size distributions, number fractions, and possible sources of materials that mix with other particles. Aerosol particles during the wet season were from both natural sources such as the Amazon forest, Saharan desert, Atlantic Ocean, and African biomass burning and anthropogenic sources such as Manaus and local emissions. These particles mix together at an individual particle scale. The number fractions of mineral dust and sea-salt particles increased almost 3-fold when long-range transport (LRT) from the African continent occurred. Nearly 20 % of mineral dust and primary biological aerosol particles had attached sea salts on their surfaces. Sulfates were also internally mixed with sea-salt and mineral dust particles. The TEM element mapping images showed that several components with sizes of hundreds of nanometers from different sources commonly occur within individual LRT aerosol particles. We conclude that many aerosol particles from natural sources change their compositions by mixing during transport. The compositions and mixing states of these particles after emission result in changes in their hygroscopic and optical properties and should be considered when assessing their effects on climate.

54 ENVIRONMENTAL SCIENCES↗

Mixing states of Amazon-basin aerosol particles transported over long distances using transmission electron microscopy

The Amazon basin is important for understanding the global climate both because of its carbon cycle and as a laboratory for obtaining basic knowledge of the continental background atmosphere. Aerosol particles play an important role in the climate and weather, and knowledge of their compositions and mixing states is necessary to understand their influence on the climate. For this study, we collected aerosol particles from the Amazon basin during the Green Ocean Amazon (GoAmazon2014/5) campaign (February to March 2014) at the T3 site, which locates about 70 km from Manaus, and analyzed using transmission electron microscopy (TEM). TEM has better spatial resolution than other instruments, which enables us to analyse the occurrences of components that attach to or are embedded within other particles. Based on the TEM results of more than 10,000 particles from several transport events, this study shows the occurrences of individual particles including compositions, size distributions, number fractions, and possible sources of materials that mix with other particles. Aerosol particles during the wet season were from both natural sources such as the Amazon forest, Saharan desert, Atlantic Ocean, and African biomass burning and anthropogenic sources such as Manaus and local emissions. These particles mix together at an individual particle scale. The number fractions of mineral dust and sea-salt particles increased almost three-fold when long-range transport (LRT) from the African continent occurred. Nearly 20 % of mineral dust and primary biological aerosol particles attached sea salts on their surfaces. Sulfates were also internally mixed with sea-salt and mineral dust particles. The TEM element mapping images showed that several components with sizes of hundreds of nanometres from different sources commonly occur within individual LRT aerosol particles. We conclude that many aerosol particles from natural sources change their compositions by mixing during transport. The compositions and mixing states of these particles after emission result in changes in their hygroscopic and optical properties and should be considered when assessing their effects on climate.

54 ENVIRONMENTAL SCIENCES↗

Quantifying the role of moss in terrestrial ecosystem carbon dynamics in northern high latitudes

Mosses are ubiquitous in northern terrestrial ecosystems, and play an important role in regional carbon, water and energy cycling. Current global land surface models that do not consider mosses may bias the quantification of regional carbon dynamics. Here we incorporate mosses as a new plant functional type into the process-based Terrestrial Ecosystem Model (TEM 5.0), to develop a new model (TEM_Moss). The new model explicitly quantifies the interactions between vascular plants and mosses and their competition for energy, water, and nutrients. Compared to the estimates using TEM 5.0, the new model estimates that the regional terrestrial soils currently store 132.7 Pg more C and will store 157.5 and 179.1 Pg more C under the RCP8.5 and RCP2.6 scenarios, respectively, by the end of the 21st century. Ensemble regional simulations forced with different parameters for the 21st century with TEM_Moss predict that the region will accumulate 161.1±142.1 Pg C under the RCP2.6 scenario and 186.7±166.1 Pg C under the RCP8.5 scenario over the century. Our study highlights the necessity of coupling moss into Earth system models to adequately quantify terrestrial carbon–climate feedbacks in the Arctic.

54 ENVIRONMENTAL SCIENCES↗

Microstructural Characterization of Aluminum-Lithium Alloys 1460 and 2195

Transmission electron microscopy (TEM) and differential scanning calorimetry (DSC) techniques were employed to characterize the precipitate distributions in lithium-containing aluminum alloys 1460 and 2195 in the T8 condition. TEM examinations revealed delta prime and T1 as the primary strengthening precipitates in alloys 1460 and 2195 respectively. TEM results showed a close similarity of the Russian alloy 1460 to the U.S. alloy 2090, which has a similar composition and heat treatment schedule. DSC analyses also indicate a comparable delta prime volume fraction. TEM study of a fractured tensile sample of alloy 1460 showed that delta prime precipitates are sheared by dislocations during plastic deformation and that intense stress fields arise at grain boundaries due to planar slip. Differences in fracture toughness of alloys 1460 and 2195 are rationalized on the basis of a literature review and observations from the present study.

Wang, Z. M.↗

3D Observation of GEMS by Electron Tomography

Amorphous silicates in chondritic porous interplanetary dust particles (CP-IDPs) coming from comets are dominated by glass with embedded metal and sulfides (GEMS). GEMS grains are submicron-sized rounded objects (typically 100-500) nm in diameter) with anaometer-sized (10-50 nm) Fe-Ni metal and sulfide grains embedded in an amorphous silicate matrix. Several formation processes for GEMS grains have been proposed so far, but these models are still being debated [2-5]. Bradley et al. proposed that GEMS grains are interstellar silicate dust that survived various metamorphism or alteration processes in the protoplanetary disk and that they are amorphiation products of crystalline silicates in the interstellar medium by sputter-deposition of cosmic ray irradiation, similar to space weathering [2,4]. This consideration is based on the observation of nano-sized crystals (approximately 10 nm) called relict grains in GEMS grains and their shapes are pseudomorphs to the host GEMS grains. On the other hand, Keller and Messenger proposed that most GEMS formed in the protoplanetary disk as condensates from high temperature gas [3,5]. This model is based on the fact that most GEMS grains have solar isotopic compositions and have extremely heterogeneous and non-solar elemental compositions. Keller and Messenger (2011) also reported that amorphous silicates in GEMS grains are surrounded by sulfide grains, which formed as sulfidization of metallic iron grains located on the GEMS surface. The previous studies were performed with 2D observation by using transmission electron microscopy (TEM) or scanning TEM (STEM). In order to understand the structure of GEMS grains described above more clearly, we observed 3D structure of GEMS grains by electron tomography using a TEM/STEM (JEM-2100F, JEOL) at Kyoto University. Electron tomography gives not only 3D structures but also gives higher spatial resolution (approximately a few nm) than that in conventional 2D image, which is restricted by sample thickness ) approx. or greater than 50 nm). Three cluster IDPs (L2036AA5 cluster4, L2009L8 cluster 13 and W726A2) were used for the observations. ID W726A2 was collected without silicon oil, which is ordinary used to collect IDPs, so this sample has no possibility of contaminations caused by silicon oil or solvent to rinse it [6]. The samples were embedded in epoxy risin and sliced into ultrathin sections (50-300 nm) using an ultramicotome. The sections were observed by BF-TEM and HAADF-STEM (high angle annular dark field-scanning TEM) modes. Images were obtained by rotating the sample tilt angle over a range of +/- 65 deg in 1 deg steps. The obtained images were reconstructed to slice images. Mineral phases in the slice images were estimated by comparing with a 2D elemental map obtained by an EDS (energy dispersive X-ray spectroscopy) system equipped in the TEM/STEM. Careful examination of the slice images confirmed that iron grains are embedded in the amorphous silicate matrix of the GEMS grains, but sulfide grains were mainly present on the surface of the amorphous silicate. These results are consistent with the model that GEMS grains formed as condensates [3,5], although more data are needed to conclude the origin of GEMS grains. The present study is the first successful example adapting the electron tomography to the IDPs. This type of analysis will be important for planetary material sciences in the future.

Matsuno, Junya↗

Formation and growth of cerium (III) oxalate nanocrystals by liquid-cell transmission electron microscopy

Using rare earth elements as analogs for actinide series elements enables studying the chemistry of these radioactive materials without the inherent risks. A fundamental understanding of the nucleation and growth of actinide oxalates is crucial for processing nuclear waste. Using in-situ liquid cell TEM (LC-TEM), we show particle attachment processes occurring during the nucleation and growth of cerium oxalate. The early stages of the observed non-classical growth mechanisms have important implications for particle evolution and predictions of final particle morphology. In this work, we observed particle formation via monomer-by-monomer addition or the particle aggregation pathway depending on the selected precursor concentration. At the highest precursor concentration at a high dose rate, we observed particle alignment in a branch structure is due to the interfacial instability. It was demonstrated that in-situ LC-TEM is an invaluable tool in studying the cerium oxalate formation and ultimately a path to understanding actinide chemistry.

36 MATERIALS SCIENCE↗

In situ electron microscopy: atomic-scale dynamics of metal oxidation and corrosion

Corrosion degrades metals through complex microscopic processes that traditional methods often fail to capture. In-situ transmission electron microscopy (TEM) bridges this gap by providing real-time atomic-scale imaging of oxidation and corrosion dynamics. Gas-phase TEM uncovers critical oxidation mechanisms like oxide nucleation and alloying effects, while liquid-phase TEM tracks corrosion initiation. Coupled with emerging techniques like ultrafast direct electron detection cameras, these advancements promise unprecedented resolution in understanding material degradation.

36 MATERIALS SCIENCE↗

Computer Vision Pipeline for Image Analysis for Freeze‐Fracture Electron Microscopy: Rosette Cellulose Synthase Complexes Case

In materials science, plant biology, agriculture, and environmental research, the automated analysis of high-magnification, complex microscopy images, such as those generated by freeze-fracture electron microscopy (FF-TEM), remains a critical challenge that limits the scalability of data interpretation. We present a deep learning computer vision pipeline for high-throughput detection and morphological characterization analysis of cellulose synthase complexes (CSCs, or rosettes) in FF-TEM images. The pipeline integrates preprocessing, detection, human-in-the-loop verification, and semantic segmentation to quantify features such as rosette diameter and inter-lobe spacing. The approach was trained and tested on a curated dataset of high-resolution FF-TEM micrographs of Physcomitrium patens, expanded via strategic tiling and augmentation to over 650 images. We compare YOLOv8 and YOLOv9 architectures and demonstrate that YOLOv9 achieves superior performance in both localization accuracy (mAP50-95 = 0.854) and inference speed. The resulting distributions revealed biological variability consistent with prior manual studies, validating the approach for high-throughput applications. Our results show that the pipeline achieves human-expert level accuracy while dramatically reducing analysis time, enabling scalable, reproducible structural characterization of intramembrane protein complexes. The pipeline is broadly applicable to other domains requiring precise interpretation of complex microscopy data and establishes a foundation for future artificial intelligence (AI)-assisted workflows in biological imaging.

59 BASIC BIOLOGICAL SCIENCES↗

A deep learning model for automatic analysis of cavities in irradiated materials

Transmission electron microscopy (TEM) is a commonly used technique in materials science for defect investigation. Quantitative analysis of defects is important for understanding the properties of a material, but manual analysis of TEM micrographs can be time-consuming and prone to error, especially when the defects have irregular shapes rather than spherical shapes. Many existing methods or deep learning models do not handle a wide range of sizes for the same object type within a single image. In this work, we present a framework that enables users to train an instance segmentation model called Mask R- CNN on any microstructure dataset, perform multi-detection on the same image at different scales, and obtain properties (e.g., size, area) of the objects based on the desired shape (e.g., circle, ellipse, rectangle). Additionally, we have developed a parallel detection module that uses multiple GPUs to increase the efficiency of the object detection process. We demonstrate the capabilities of our framework using a set of TEM images of cavities with different shapes, size distributions, and background contrasts. Finally, we show that the performance of our model in terms of density, size, and swelling of the cavities is comparable to the human average and that our model achieves the highest recall value compared to existing methods due to the use of image multi-rescaling.

36 MATERIALS SCIENCE↗

Structure of the pellet-cladding interaction layer of a high-burnup Zr-Nb-O nuclear fuel cladding

Here, structure of the pellet/cladding-interaction (PCI) layer of a high-burnup nuclear fuel with niobium-bearing cladding was investigated using modern transmission electron microscopy (TEM) techniques. Morphology of the PCI consisted of uniform zirconia layer on the cladding side and finger-like features towards to the ceramic fuel. The PCI layer showed a complex microstructure that constitutes three distinct zirconia layers formed by two zirconia phases. From cladding to fuel, monoclinic, tetragonal, and another tetragonal phase were determined via TEM diffraction patterns and precession electron diffraction (PED) using ASTAR microscopy platform (AMP). Characterizations showed that monoclinic and tetragonal phases close to the cladding were crack-free, but the tetragonal layer adjacent to the fuel contained cracks and pores. Presence of the monoclinic layer suggested that its formation involved the gaseous diffusion of oxygen below threshold dose of fission product damage before the fuel/cladding contact occurred. Furthermore, high-resolution TEM revealed compound phase of (U,Zr)O 2 at fringes of zirconia fingers on the fuel side.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Structural Complexities in Sodium Ion Conductive Antiperovskite Revealed by Cryogenic Transmission Electron Microscopy

Here we use low-dose cryogenic transmission electron microscopy (cryo-TEM) to investigate the atomic-scale structure of antiperovskite Na 2 NH 2 BH 4 crystals by preserving the room-temperature cubic phase and carefully monitoring the electron dose. Via quantitative analysis of electron beam damage using selected area electron diffraction, we find cryogenic imaging provides 6-fold improvement in beam stability for this solid electrolyte. Cryo-TEM images obtained from flat crystals revealed the presence of a new, long-range-ordered supercell with a cubic phase. The supercell exhibits doubled unit cell dimensions of 9.4 Å × 9.4 Å as compared to the cubic lattice structure revealed by X-ray crystallography of 4.7 Å × 4.7 Å. The comparison between the experimental image and simulated potential map indicates the origin of the supercell is a vacancy ordering of sodium atoms. This work demonstrates the potential of using cryo-TEM imaging to study the atomic-scale structure of air- and electron-beam-sensitive antiperovskite-type solid electrolytes.

36 MATERIALS SCIENCE↗

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↗

Final Technical Report for the SciDAC Center for the Study of Plasma Microturbulence

This final technical report for the SciDAC Center for the Study of Plasma Microturbulence documents contributions from MIT to the project over the period of the award (February 15, 2011 to February 14, 2020). This project focused on the development of neoclassical and gyrokinetic simulation capabilities relevant for the description of particle, momentum and energy transport in tokamak fusion plasmas. Extensive validation against experimental results from Alcator C-Mod and DIII-D experiments was performed. Overall areas of emphasis included gyrokinetic simulations, experiments, and observation of density gradient driven Trapped Electron Mode (TEM) turbulence relevant to burning plasmas; theory and gyrokinetic simulations of the parametric variation of the nonlinear upshift of the TEM critical density gradient; identification of a new mechanism for the isotope effect due to density gradient driven TEM turbulence; new synthetic diagnostics based on full-wave simulations which enabled unprecedented agreement between gyrokinetic simulations and measured fluctuation spectra with and without strong electron heating; development of new continuum pedestal neoclassical and turbulence codes; formulation and implementation of the first gyrokinetic exact Fokker-Planck collision operator in gyrokinetic turbulence simulations; development of new spectral approaches in velocity space for highly efficient treatments of collisions; new model collision operators implemented in the discontinuous Galerkin gyrokinetic edge turbulence code GKEYLL; and a new model and spectral code to study the interaction of ion- and electron-scale turbulence, which will serve as an efficient test-bed for multi-rate and multi-scale methods. These fundamental advances contribute to the development of a validated, predictive capability for turbulent and collisional particle, momentum and energy transport in both the core and edge of magnetically confined fusion plasmas.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Advanced Electron Microscopy Characterization of the Fuel-Cladding Chemical Interaction Region in a High Burnup U-10Zr Fuel

To support the development of U-10Zr metallic fuel, advanced characterization techniques have been applied to the fuel-cladding chemical interaction (FCCI) region in a Na-bonded solid U-10Zr fuel cross-section that was irradiated to a burnup of ~13.1 at.% at the Fast Flux Test Facility. 17 phases were identified in the FCCI region through a combination of high-resolution scanning transmission electron microscopy (STEM), STEM based energy dispersive X-ray spectroscopy (STEM-EDS), and TEM based selective area electron diffraction (TEM-SAED) analysis. In this talk, we will also discuss the implications of results on metallic fuel FCCI by focusing on the formation of Zr rind, fission product migration, and HT-9 cladding integrality under the investigated thermal irradiation conditions. This work complements our previous study on the TEM characterization of the fuel region of this high burnup fuel sample and serves as scientific basis to support metallic fuel development and qualification.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗