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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Fabrication of a Point-Like Transmission Target for Reducing Computed Tomography Imaging Artifacts

In this study, we address the challenge of enhancing image quality and spatial resolution in computed tomography (CT) imaging by introducing simulation and fabrication of high aspect ratio, point-like transmission targets. Utilizing advanced electroplating techniques, traditionally employed in the fabrication of Through Substrate Via (TSV) interconnects for CMOS circuitry, we successfully embed copper targets within silicon substrates. This method allows us to create high-aspect-ratio features specifically designed for X-ray transmission targets, resulting in micro targets that exhibit a volume increase compared to conventional evaporated surface targets. Furthermore, we present simulation results of the X-ray spectrum generated by these targets, demonstrating their potential to significantly improve both image quality and spatial resolution in CT applications. Our findings suggest that leveraging advanced fabrication techniques can open new avenues for the development of enhanced imaging technologies in medical diagnostics and beyond.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

Deep Learning for Spectroscopic X-ray Nano-Imaging Denoising

Synchrotron transmission X-ray microscopy with absorption near edge structure (TXM-XANES) is a powerful tool for investigating the structure and composition of materials at nano- to meso-scales. It is, however, often challenged by high levels of noise that obscure critical details at the single-pixel level. To address this issue, a deep learning-based algorithm is developed for suppressing the image noise, grounded in self-supervised learning principles. In contrast to traditional image denoising methods, this approach successfully enhances the visibility of fine details while significantly reducing the noise in the X-ray images. Through this advancement, the potential of the approach for improving the accuracy and interpretability of the TXM-XANES data is demonstrated, thereby enabling more precise detection of nanoscale phenomena such as inhomogeneous cation redox and metal segregation in battery cathode materials. This technique offers an effective new avenue for harnessing the full potential of synchrotron TXM-XANES imaging, paving the way for a range of exciting new studies in materials science and beyond.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Chemical Heterogeneity in PAN/LLZTO Composite Electrolytes by Synchrotron Imaging

Solid polymer/ceramic composite electrolytes are promising for batteries due to their attractive thermal stability and mechanical properties. Chemical heterogeneity in solid composite electrolytes, such as the inhomogeneity in the ceramic phase and salt distribution at the polymer/ceramic interface, is critical to the performance of solid composite electrolytes. However, such heterogeneity has not been well understood yet. In this work, we use Synchrotron-based X-ray fluorescence imaging (XRF) and Transmission X-ray Microscope (TXM) to image nanoscale chemical heterogeneity in polyacrylamide/Li 7+x La 3 Zr 2–x Ta x O 12 (LLZTO) composite electrolytes and investigate the effects of lithium salt, salt concentration, and plasticizer. We find that LLZTO particles show strong inter- and intra-particles chemical heterogeneities, and the off-stoichiometry of Zr in an LLZTO particle is unlikely to be only balanced by Ta substitution. Moreover, statistical analysis suggests that LiI tends to accumulate at the ceramic/polymer interface at a low concentration of 5 wt%, but no such tendency was observed in samples with 10 wt% LiI. However, composite electrolytes with LiTFSI show interfacial accumulation at both 5 wt% and 10 wt%. Furthermore, this report provides insight into element distributions in solid composite electrolytes, and we hope further researches can shed light on the connections between chemical heterogeneity and ionic transport pathway inside.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Atomic Resolution Imaging of Light Elements in a Crystalline Environment using Dynamic Hollow-Cone Illumination Transmission Electron Microscopy

Multiple electron scattering and the nonintuitive nature of image formation with coherent radiation complicate the interpretation of conventional transmission electron microscopy images. Precession of the illuminating beam in transmission electron microscopy (TEM) can lead to more robust and interpretable images with some penalty to image contrast, a technique known as dynamic hollow-cone illumination TEM. Here, we demonstrate direct and robust imaging of light and heavy atoms in a crystalline environment with this technique. This method is similar to the annular bright-field technique in scanning transmission electron microscopy, via the principle of reciprocity. Dynamic hollow-cone illumination TEM is challenging in practice due to sensitivity to the misalignment of the precession axis, microscope objective aperture, and crystal zone axis.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2021

Use of Transmission Electron Microscopy for Analysis of Aerosol Particles and Strategies for Imaging Fragile Particles

For over 25 years, transmission electron microscopy (TEM) has provided a method for the study of aerosol particles with sizes from below the optical diffraction limit to several microns, resolving the particles as well as smaller features. The wide use of this technique to study aerosol particles has contributed important insights about environmental aerosol particle samples and model atmospheric systems. TEM produces an image that is a 2D projection of aerosol particles that have been impacted onto grids and, through associated techniques and spectroscopies, can contribute additional information such as the determination of elemental composition, crystal structure, and 3D particle structures. Soot, mineral dust, and organic/inorganic particles have all been analyzed using TEM and spectroscopic techniques. TEM, however, has limitations that are important to understand when interpreting data including the ability of the electron beam to damage and thereby change the structure and shape of particles, especially in the case of particles composed of organic compounds and salts. In this paper, we concentrate on the breadth of studies that have used TEM as the primary analysis technique. Another focus is on common issues with TEM and cryogenic-TEM. Insights for new users on best practices for fragile particles, that is, particles that are easily susceptible to damage from the electron beam, with this technique are discussed. Tips for readers on interpreting and evaluating the quality and accuracy of TEM data in the literature are also provided and explained.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Femtosecond multimodal imaging with a laser-driven X-ray source

Laser-plasma accelerators are compact linear accelerators based on the interaction of high-power lasers with plasma to form accelerating structures up to 1000 times smaller than standard radiofrequency cavities, and they come with an embedded X-ray source, namely betatron source, with unique properties: small source size and femtosecond pulse duration. A still unexplored possibility to exploit the betatron source comes from combining it with imaging methods able to encode multiple information like transmission and phase into a single-shot acquisition approach. In this work, we combine edge illumination-beam tracking (EI-BT) with a betatron X-ray source and present the demonstration of multimodal imaging (transmission, refraction, and scattering) with a compact light source down to the femtosecond timescale. The advantage of EI-BT is that it allows multimodal X-ray imaging technique, granting access to transmission, refraction and scattering signals from standard low-coherence laboratory X-ray sources in a single shot.

43 PARTICLE ACCELERATORS↗
DOE OSTI2021

Thermodynamics of order and randomness in dopant distributions inferred from atomically resolved imaging

Abstract Exploration of structure-property relationships as a function of dopant concentration is commonly based on mean field theories for solid solutions. However, such theories that work well for semiconductors tend to fail in materials with strong correlations, either in electronic behavior or chemical segregation. In these cases, the details of atomic arrangements are generally not explored and analyzed. The knowledge of the generative physics and chemistry of the material can obviate this problem, since defect configuration libraries as stochastic representation of atomic level structures can be generated, or parameters of mesoscopic thermodynamic models can be derived. To obtain such information for improved predictions, we use data from atomically resolved microscopic images that visualize complex structural correlations within the system and translate them into statistical mechanical models of structure formation. Given the significant uncertainties about the microscopic aspects of the material’s processing history along with the limited number of available images, we combine model optimization techniques with the principles of statistical hypothesis testing. We demonstrate the approach on data from a series of atomically-resolved scanning transmission electron microscopy images of Mo x Re 1- x S 2 at varying ratios of Mo/Re stoichiometries, for which we propose an effective interaction model that is then used to generate atomic configurations and make testable predictions at a range of concentrations and formation temperatures.

25 ENERGY STORAGE↗
DOE OSTI2021

Quantitative insights into the dislocation source behavior of twin boundaries suggest a new dislocation source mechanism

Pop-in statistics from nanoindentation with spherical indenters are used to determine the stress required to activate dislocation sources in twin boundaries (TBs) in copper and its alloys. The TB source activation stress is smaller than that needed for bulk single crystals, irrespective of the indenter size, dislocation density and stacking fault energy. Because an array of pre-existing Frank partial dislocations is present at a TB, we propose that dislocation emission from the TB occurs by the Frank partials splitting into Shockley partials moving along the TB plane and perfect lattice dislocations, both of which are mobile. The proposed mechanism is supported by recent high resolution transmission electron microscopy images in deformed nanotwinned (NT) metals and may help to explain some of the superior properties of nanotwinned metals (e.g. high strength and good ductility), as well as the process of detwinning by the collective formation and motion of Shockley partial dislocations along TBs.

36 MATERIALS SCIENCE↗
DOE OSTI2026

INR-TEM: Robust cavity detection in multifocus TEM images via implicit neural representations

When characterizing materials using transmission electron microscopy (TEM) images, detecting and quantifying small features in microstructures, such as cavities, pose significant challenges. Off-the-shelf object detection models, including YOLOv8, show considerable performance degradation, particularly when images vary in resolution and the objects of interest possess a low percentage of the total image region of interest. In this study, we introduce a novel detection pipeline that incorporates an implicit neural representation (INR)-based detection method, INR-TEM, and two-modality imaging (e.g., under-focused and over-focused images typically acquired during materials characterization) to improve object detection performance. The INR-TEM method incorporates a pixel-wise prediction principle inspired by pixel-wise centerness weighting. INR-TEM demonstrates superior robustness to resolution variability, maintaining high detection accuracy even at low image resolutions compared to YOLOv8. To leverage INR-TEM effectively in real-world two-modality characterization applications, we further integrate a two-stage motion correction pipeline designed explicitly for aligning multifocus TEM images. The alignment process, comprising keypoint (based on scale-invariant feature transform, SIFT) and intensity matching, significantly mitigates the adverse effects of perceived motion-induced image degradation during through-focal TEM imaging, directly enhancing INR-TEM’s detection capability over conventional single-focus images. Our integrated INR-TEM cavity detection framework notably improves performance across various cavity sizes, outperforming off-the-shelf YOLOv8 detections that rely on a single image modality.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2020

mpfit: a robust method for fitting atomic resolution images with multiple Gaussian peaks

The standard technique for sub-pixel estimation of atom positions from atomic resolution scanning transmission electron microscopy images relies on fitting intensity maxima or minima with a two-dimensional Gaussian function. While this is a widespread method of measurement, it can be error prone in images with non-zero aberrations, strong intensity differences between adjacent atoms or in situations where the neighboring atom positions approach the resolution limit of the microscope. Here we demonstrate mpfit, an atom finding algorithm that iteratively calculates a series of overlapping two-dimensional Gaussian functions to fit the experimental dataset and then subsequently uses a subset of the calculated Gaussian functions to perform sub-pixel refinement of atom positions. Based on both simulated and experimental datasets presented in this work, this approach gives lower errors when compared to the commonly used single Gaussian peak fitting approach and demonstrates increased robustness over a wider range of experimental conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Stroboscopic ultrafast imaging using RF strip-lines in a commercial transmission electron microscope

The development of ultrafast electron microscopy (UEM), specifically stroboscopic imaging, has brought the study of structural dynamics to a new level by overcoming the spatial limitations of ultrafast spectroscopy and the temporal restrictions of traditional TEM simultaneously. Combining the concepts governing both techniques has enabled direct visualization of dynamics with spatiotemporal resolutions in the picosecond-nanometer regime. Here, in this study, we push the limits of imaging using a pulsed electron beam via RF induced transverse deflection based on the newly developed 200 keV frequency-tunable strip-line pulser. We demonstrate 0.2 nm spatial resolution at high magnifications and elucidation of Lorentz imaging using the phase-microscopy method. We also present beam coherence measurements and expand our study using the breathing modes of a silicon interdigitated comb under RF excitation which achieves improved temporal synchronization between the electron pulse-train and electric field. A new RF holder has also been developed with impedance matching to the RF signal to minimize transmission power loss to samples and its performance is compared with a conventional sample holder.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Development of liquid cells for high resolution imaging and chemical analysis in situ with Transmission Electron Microscopy

The development of liquid cells for transmission electron microscopy (TEM) have enabled breakthroughs in the study of nanoscale structural, morphological, or chemical changes during materials growth and applications [1]. The challenges of achieving high resolution imaging and chemical analysis through liquids often arise from the liquid cells being too thick. Making ultra-thin freestanding membranes and controlling the liquid thickness are some of the key attributes to the recent liquid cell developments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

4D-STEM of Beam-Sensitive Materials

We report that a scanning electron nanobeam diffraction, or 4D-STEM (four-dimensional scanning transmission electron microscopy), is a flexible and powerful approach to elucidate structure from "soft" materials that are challenging to image in the transmission electron microscope because their structure is easily damaged by the electron beam. In a 4D-STEM experiment, a converged electron beam is scanned across the sample, and a pixelated camera records a diffraction pattern at each scan position. This four-dimensional data set can be mined for various analyses, producing maps of local crystal orientation, structural distortions, crystallinity, or different structural classes. Holding the sample at cryogenic temperatures minimizes diffusion of radicals and the resulting damage and disorder caused by the electron beam. The total fluence of incident electrons can easily be controlled during 4D-STEM experiments by careful use of the beam blanker, steering of the localized electron dose, and by minimizing the fluence in the convergent beam thus minimizing beam damage. This technique can be applied to both organic and inorganic materials that are known to be beam-sensitive; they can be highly crystalline, semicrystalline, mixed phase, or amorphous. One common example is the case for many organic materials that have a π-π stacking of polymer chains or rings on the order of 3.4-4.2 Å separation. If these chains or rings are aligned in some regions, they will produce distinct diffraction spots (as would other crystalline spacings in this range), though they may be weak or diffuse for disordered or weakly scattering materials. We can reconstruct the orientation of the π-π stacking, the degree of π-π stacking in the sample, and the domain size of the aligned regions. This Account summarizes illumination conditions and experimental parameters for 4D-STEM experiments with the goal of producing images of structural features for materials that are beam-sensitive. We will discuss experimental parameters including sample cooling, probe size and shape, fluence, and cameras. 4D-STEM has been applied to a variety of materials, not only as an advanced technique for model systems, but as a technique for the beginning microscopist to answer materials science questions. It is noteworthy that the experimental data acquisition does not require an aberration-corrected TEM but can be produced on a variety of instruments with the right attention to experimental parameters.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Multi-modal tomographic imaging system for poolside characterization of nuclear test fuels: Design considerations and studies

Testing and qualification of advanced nuclear fuels involves an iterative process of prototyping, in-pile irradiation testing, and in-situ or ex-situ examination. Fuel restructuring and fission product migration during burnup are among the most important aspects of fuel evolution that affect several important performance characteristics such as heat removal, accident tolerance, and fission product retention. Pool-side non-destructive characterization techniques provide fuel developers with tools to understand fuel evolution at different points of burnup. A design for a compact, submersible, and multi-modal gamma-ray tomography system for imaging irradiated nuclear fuel is presented here. Detector selection, collimator geometry and fabrication, mechanical design, imaging protocol and acquisition speed are discussed. Modeling calculations show that sub-millimeter resolution can be achieved in both transmission computed tomography images as well as in emission computed tomography images in a matter of hours. Several design compromises and fabrication challenges are discussed which should be taken into consideration for future submersible gamma-ray tomography instruments.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

Direct imaging of electron density with a scanning transmission electron microscope

Abstract Recent studies of secondary electron (SE) emission in scanning transmission electron microscopes suggest that material’s properties such as electrical conductivity, connectivity, and work function can be probed with atomic scale resolution using a technique known as secondary electron e-beam-induced current (SEEBIC). Here, we apply the SEEBIC imaging technique to a stacked 2D heterostructure device to reveal the spatially resolved electron density of an encapsulated WSe 2 layer. We find that the double Se lattice site shows higher emission than the W site, which is at odds with first-principles modelling of valence ionization of an isolated WSe 2 cluster. These results illustrate that atomic level SEEBIC contrast within a single material is possible and that an enhanced understanding of atomic scale SE emission is required to account for the observed contrast. In turn, this suggests that, in the future, subtle information about interlayer bonding and the effect on electron orbitals could be directly revealed with this technique.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Characterization of Mn 5 Ge 3 Contacts on a Shallow Ge/SiGe Heterostructure

Mn 5 Ge 3 is a ferromagnetic phase of the Mn-Ge system that is a potential contact material for efficient spin injection and detection. Here, we investigate the creation of Mn 5 Ge 3 -based contacts on a Ge/SiGe quantum well heterostructure via solid-state synthesis. X-ray diffraction spectra fitting indicates the formation of Mn 5 Ge 3 -based contacts on bulk Ge and Ge/SiGe. High-resolution scanning transmission electron microscopy imaging and energy dispersive X-ray spectroscopy verify the correct Mn 5 Ge 3 -based phase formation. Schottky diode measurements, transmission line measurements, and Hall measurements reveal that Mn 5 Ge 3 -based contacts serve as good p-type contacts for Ge/SiGe quantum well heterostructures due to having a low Schottky barrier height of 0.10 eV (extracted from a Mn 5 Ge 3 /n-Ge analogue) and a contact resistance in the order of 1 kΩ. Furthermore, we show that these electrical characteristics have a gate-voltage dependence, thereby providing tunability.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Plasmonic nanorod probes’ journey inside plant cells for in vivo SERS sensing and multimodal imaging

Nanoparticle-based platforms are gaining strong interest in plant biology and bioenergy research to monitor and control biological processes in whole plants. However, in vivo monitoring of biomolecules using nanoparticles inside plant cells remains challenging due to the impenetrability of the plant cell wall to nanoparticles beyond the exclusion limits (5-20 nm). To overcome this physical barrier, we have designed unique bimetallic silver-coated gold nanorods (AuNR@Ag) capable of entering plant cells, while conserving key plasmonic properties in the near-infrared (NIR). To demonstrate cellular internalization and tracking of the nanorods inside plant tissue, we used a comprehensive multimodal imaging approach that included transmission electron microscopy (TEM), confocal fluorescence microscopy, two-photon luminescence (TPL), X-ray fluorescence microscopy (XRF), and photoacoustics imaging (PAI). We successfully acquired SERS signals of nanorods in vivo inside plant cells of tobacco leaves. On the same leaf samples, we applied orthogonal imaging methods, TPL and PAI techniques for in vivo imaging of the nanorods. This study first demonstrates the intracellular internalization of AuNR@Ag inside whole plant systems for in vivo SERS analysis in tobacco cells. This work demonstrates the potential of this nanoplatform as a new nanotool for intracellular in vivo biosensing for plant biology.

Cupil-Garcia, Vanessa↗