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Results for “nano-tomography”

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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18 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Visualizing time-dependent microstructural and chemical evolution during molten salt corrosion of Ni-20Cr model alloy using correlative quasi in situ TEM and in situ synchrotron X-ray nano-tomography

In situ monitoring of corrosion processes is important to fundamentally understand the kinetics and evolution of materials in harsh environments. A quasi in situ transmission electron microscopy technique was utilized to study microstructural and chemical evolution of a Ni-20Cr disc sample 6 exposed to molten KCl-MgCl 2 salt for 60 s in consecutive 20 s iterations. In situ synchrotron X-ray nano-tomography was performed to characterize the morphological evolution of a Ni-20Cr microwire exposed to molten KCl-MgCl 2 . Here, both techniques captured key corrosion events and revealed mechanisms at different time and length scales, potentially bringing greater insights and 10 deeper understanding beyond conventional analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Heterogeneous 3D Morphological Evolution of Ni Microparticles in Molten Salts: Visualized by Operando Synchrotron X-ray Nano-tomography

Ni-based superalloys are promising materials for high-temperature molten salt (MS) energy generation and storage. Studying morphological and chemical evolution of pure Ni in MS provides fundamental knowledge for MS technologies and corrosion mitigation. Here, in this study, real-time 3D morphological changes of Ni microparticles in molten KCl-MgCl 2 were studied by operando synchrotron X-ray nano-tomography at 700°C. Rapid Ni particle agglomeration occurred, without significant chemical reactions, such as oxide or chloride formation. The morphological growth evolved differently from classical coarsening or sintering behaviors and occurred nonuniformly, with other regions showing slight dissolution of Ni. Ni nanoparticles were found to be dispersed in many areas of the samples, either from microparticle dissolution or other radiation-induced nanoparticle formation mechanisms. This study discusses important factors, i.e., thermal gradient, amounts of salt and metals, and radiation effect, that influence morphological changes of materials in MS, critical for fundamental understanding of material–MS interactions as well as for practical applications.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Formation of three-dimensional bicontinuous structures via molten salt dealloying studied in real-time by in situ synchrotron X-ray nano-tomography

Abstract Three-dimensional bicontinuous porous materials formed by dealloying contribute significantly to various applications including catalysis, sensor development and energy storage. This work studies a method of molten salt dealloying via real-time in situ synchrotron three-dimensional X-ray nano-tomography. Quantification of morphological parameters determined that long-range diffusion is the rate-determining step for the dealloying process. The subsequent coarsening rate was primarily surface diffusion controlled, with Rayleigh instability leading to ligament pinch-off and creating isolated bubbles in ligaments, while bulk diffusion leads to a slight densification. Chemical environments characterized by X-ray absorption near edge structure spectroscopic imaging show that molten salt dealloying prevents surface oxidation of the metal. In this work, gaining a fundamental mechanistic understanding of the molten salt dealloying process in forming porous structures provides a nontoxic, tunable dealloying technique and has important implications for molten salt corrosion processes, which is one of the major challenges in molten salt reactors and concentrated solar power plants.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Sub-10 second fly-scan nano-tomography using machine learning

Abstract X-ray computed tomography is a versatile technique for 3D structure characterization. However, conventional reconstruction algorithms require that the sample not change throughout the scan, and the timescale of sample dynamics must be longer than the data acquisition time to fulfill the stable sample requirement. Meanwhile, concerns about X-ray-induced parasite reaction and sample damage have driven research efforts to reduce beam dosage. Here, we report a machine-learning-based image processing method that can significantly reduce data acquisition time and X-ray dose, outperforming conventional approaches like Filtered-Back Projection, maximum-likelihood, and model-based maximum-a-posteriori probability. Applying machine learning, we achieve ultrafast nano-tomography with sub-10 second data acquisition time and sub-50 nm pixel resolution in a transmission X-ray microscope. We apply our algorithm to study dynamic morphology changes in a lithium-ion battery cathode under a heating rate of 50 o C min −1 , revealing crack self-healing during thermal annealing. The proposed method can be applied to various tomography modalities.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Distributed Optimization for Nonrigid Nano-Tomography

Resolution level and reconstruction quality in nano-computed tomography (nano-CT) are in part limited by the stability of microscopes, because the magnitude of mechanical vibrations during scanning becomes comparable to the imaging resolution, and the ability of the samples to resist radiation induced deformations during data acquisition. In such cases, there is no incentive in recovering the sample state at different time steps like in time-resolved reconstruction methods, but instead the goal is to retrieve a single reconstruction at the highest possible spatial resolution and without any imaging artifacts. Here we propose a distributed optimization solver for tomographic imaging of samples at the nanoscale. Our approach solves the tomography problem jointly with projection data alignment, nonrigid sample deformation correction, and regularization. Projection data consistency is regulated by dense optical flow estimated by Farneback's algorithm, leading to sharp sample reconstructions with less artifacts. Synthetic data tests show robustness of the method to Poisson and low-frequency background noise. We accelerated the solver on multi-GPU systems and validated the method on three nano-imaging experimental data sets.

97 MATHEMATICS AND COMPUTING↗
NASA NTRS2024

X-Ray Micro- and Nano-Tomography Analysis of Bennu Samples: A Preliminary Report

X-ray tomography (XCT) is an effective technique for obtaining the 3D structures of returned samples. XCT using synchrotron radiation provides high-resolution CT images with quantitative information. The XCT systems at SPring-8, an SR facility in Japan, have been used to analyze samples returned from the asteroids Itokawa and Ryugu. In this study, we plan to apply SR-XCT to samples returned from the asteroid Bennu.

A Tsuchiyama↗
DOE OSTI2022

Evolution of micro-pores in Ni–Cr alloys via molten salt dealloying

Porous materials with high specific surface area, high porosity, and high electrical conductivity are promising materials for functional applications, including catalysis, sensing, and energy storage. Molten salt dealloying was recently demonstrated in microwires as an alternative method to fabricate porous structures. The method takes advantage of the selective dissolution process introduced by impurities often observed in molten salt corrosion. This work further investigates molten salt dealloying in bulk Ni–20Cr alloy in both KCl–MgCl 2 and KCl–NaCl salts at 700 °C, using scanning electron microscopy, energy dispersive spectroscopy, and X-ray diffraction (XRD), as well as synchrotron X-ray nano-tomography. Micro-sized pores with irregular shapes and sizes ranging from sub-micron to several microns and ligaments formed during the process, while the molten salt dealloying was found to progress several microns into the bulk materials within 1–16 h, a relatively short reaction time, enhancing the practicality of using the method for synthesis. The ligament size increased from ~ 0.7 μm to ~ 1.3 μm in KCl–MgCl 2 from 1 to 16 h due to coarsening, while remaining ~ 0.4 μm in KCl–NaCl during 16 h of exposure. The XRD analysis shows that the corrosion occurred primarily near the surface of the bulk sample, and Cr 2 O 3 was identified as a corrosion product when the reaction was conducted in an air environment (controlled amount sealed in capillaries); thus surface oxides are likely to slow the morphological coarsening rate by hindering the surface diffusion in the dealloyed structure. 3D-connected pores and grain boundary corrosion were visualized by synchrotron X-ray nano-tomography. This study provides insights into the morphological and chemical evolution of molten salt dealloying in bulk materials, with a connection to molten salt corrosion concerns in the design of next-generation nuclear and solar energy power plants.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Elucidating a dissolution–deposition reaction mechanism by multimodal synchrotron X-ray characterization in aqueous Zn/MnO 2 batteries

Aqueous Zn/MnO 2 batteries with their environmental sustainability and competitive cost, are becoming a promising, safe alternative for grid-scale electrochemical energy storage. Here, presented as a promising design principle to deliver a higher theoretical capacity, this work offers fundamental understanding of the dissolution–deposition mechanism of Zn/β-MnO 2 . A multimodal synchrotron characterization approach including three operando X-ray techniques (powder diffraction, absorption spectroscopy, and fluorescence microscopy) is coupled with elementally resolved synchrotron X-ray nano-tomography. Together they provide a direct correlation between structural evolution, reaction chemistry, and 3D morphological changes. Operando synchrotron X-ray diffraction and spectroscopy show a crystalline-to-amorphous phase transition. Quantitative modeling of the operando data by Rietveld refinement for X-ray diffraction and multivariate curve resolution (MCR) for X-ray absorption spectroscopy are used in a complementary fashion to track the structural and chemical transitions of both the long-range (crystalline phases) and short-range (including amorphous phases) ordering upon cycling. Scanning X-ray microscopy and full-field nano-tomography visualizes the morphology of electrodes at different electrochemical states with elemental sensitivity to spatially resolve the formation of the Zn- and Mn-containing phases. Overall, this work critically indicates that for Zn/MnO 2 aqueous batteries, the reaction pathways involving Zn–Mn complex formation upon cycling become independent of the polymorphs of the initial electrode and sheds light on the interplay among structural, chemical, and morphological evolution for electrochemically driven phase transitions.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Nano-laminography with a transmission X-ray microscope

Nano-laminography combines the penetrating power of hard X-rays with a tilted rotational geometry to deliver high-resolution, three-dimensional images of laterally extended, flat specimens that are otherwise incompatible with, or difficult to image using, conventional nano-tomography. In this work, we demonstrate a full-field, X-ray nano-laminography system implemented with the transmission X-ray microscope at beamline 32-ID of the upgraded Advanced Photon Source at Argonne National Laboratory, USA. By rotating the sample around an axis inclined by 20° to the incident beam, the technique minimizes the long optical path lengths that would otherwise generate excessive artifacts when planar samples are imaged edge-on. The efficiency of the technique is demonstrated with 50 nm spatial resolution and minute-scale temporal resolution 3D imaging of a planar integrated circuit sample and targeted imaging of an individual particle within a powder sample, where mounting procedures are typically challenging in regular nano-tomography. The sample mounting strategy, data acquisition, and reconstruction method will also be discussed.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2021

Deep-learning-based image registration for nano-resolution tomographic reconstruction

Nano-resolution full-field transmission X-ray microscopy has been successfully applied to a wide range of research fields thanks to its capability of non-destructively reconstructing the 3D structure with high resolution. Due to constraints in the practical implementations, the nano-tomography data is often associated with a random image jitter, resulting from imperfections in the hardware setup. Without a proper image registration process prior to the reconstruction, the quality of the result will be compromised. Here a deep-learning-based image jitter correction method is presented, which registers the projective images with high efficiency and accuracy, facilitating a high-quality tomographic reconstruction. This development is demonstrated and validated using synthetic and experimental datasets. We report the method is effective and readily applicable to a broad range of applications. Together with this paper, the source code is published and adoptions and improvements from our colleagues in this field are welcomed.

deep learning↗
DOE OSTI2025

Impacts of the Conductive Networks on Solid‐State Battery Operation

The micromorphology of composite cathodes is known to play a vital role in determining all-solid-state battery (ASSB) performance. However, much of our current understanding is derived from empirical observations, lacking a deeper mechanistic foundation. The “rocking chair” concept of battery chemistry requires maintaining charge neutrality, emphasizing the necessity of examining electrode micromorphology from the perspective of conductive networks. This study systematically investigates the microscopic electrochemical impacts of conductive network micromorphology by varying the Li + -to-e − channel ratio in cathodes comprising LiNbO 3 -coated LiNi 0.8 Co 0.1 Mn 0.1 O 2 , Li 6 PS 5 Cl, and carbon fibers. Utilizing multiscale synchrotron-based spectro-microscopy, we unravel that unbalanced Li + and e − conducting channels intensify charge polarization within active cathode particles and accelerate their degradation. A further model system with X-ray nano-tomography resolved e − and Li + channels indicates that spatially uniform and well-paired Li + and e − conducting channels are highly desirable as they could promote more uniform lithiation/delithiation, mitigating microscopic electrochemical polarization. Electrode-scale X-ray holotomography analysis reveals that the impact of conductive networks is particle-size-dependent, with smaller cathode particles being more significantly affected. These findings provide mechanistic insights into the interplay between conductive networks and all-solid-state battery operation, laying the groundwork for rational design and optimization of cathode architectures in future solid-state battery technologies.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Dynamic in situ imaging of methane hydrate formation in coal media

Fast 3D X-ray imaging has proved to provide crucial insights into multi-phase dynamic processes in various geomaterials. In particular, many in situ imaging experiments have been made to study gas-hydrate formation in porous sandy samples. Such imaging is challenging for the methane gas-hydrate formation in coal samples because of the coal micro-porosity structure and lower X-ray contrast. Here we present results of the first dynamic in situ micro-computed tomography experiment of methane-hydrate formation in coal samples. Synchrotron phase-contrast tomography techniques allowed to achieve necessary contrast levels to separate all the materials of interest (gas, water, coal, and gas hydrate) in reconstructed images with high spatial and temporal resolution. The imaging results are compared to the ones from a similar tomographic experiment with sand samples. Methane-hydrate formation is accompanied by the water movements caused by cryogenic water suction that happens in sequences of short fast movements with longer equilibrium states in between. Only one type of the hydrate formation was observed in coal (growth as shells on grain boundaries) as opposed to three types in sand (shells, growth into gas pockets, and inside water volumes). In particular, this leads to a slower hydrateformation speed in coal. For the coal sample, we also observed water extraction from grains, and interpreted it as competitive sorption of methane. Lastly, we visualized the dynamic behavior of this water extraction via microchannels inside the coal grains, and performed nano-tomography imaging of these channels for a better understanding of this phenomenon.

58 GEOSCIENCES↗
DOE OSTI2020

Nanofabrication of synthetic nanoporous geomaterials: from nanoscale-resolution 3D imaging to nano-3D-printed digital (shale) rock

Abstract Advances in imaging have made it possible to view nanometer and sub-nanometer structures that are either synthesized or that occur naturally. It is believed that fluid dynamic and thermodynamic behavior differ significantly at these scales from the bulk. From a materials perspective, it is important to be able to create complex structures at the nanometer scale, reproducibly, so that the fluid behavior may be studied. New advances in nanoscale-resolution 3D-printing offer opportunities to achieve this goal. In particular, additive manufacturing with two-photon polymerization allows creation of intricate structures. Using this technology, a creation of the first nano-3D-printed digital (shale) rock is reported. In this paper, focused ion beam-scanning electron microscopy (FIB-SEM) nano-tomography image dataset was used to reconstruct a high-resolution digital rock 3D model of a Marcellus Shale rock sample. Porosity of this 3D model has been characterized and its connected/effective pore system has been extracted and nano-3D-printed. The workflow of creating this novel nano-3D-printed digital rock 3D model is described in this paper.

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

Design nanoporous metal thin films via solid state interfacial dealloying

Thin-film solid-state interfacial dealloying (thin-film SSID) is an emerging technique to design nanoarchitecture thin films. The resulting controllable 3D bicontinuous nanostructure is promising for a range of applications including catalysis, sensing, and energy storage. Using a multiscale microscopy approach, we combine X-ray and electron nano-tomography to demonstrate that besides dense bicontinuous nanocomposites, thin-film SSID can create a very fine (5–15 nm) nanoporous structure. Not only is such a fine feature among one of the finest fabrications by metal-agent dealloying, but a multilayer thin-film design enables creating nanoporous films on a wider range of substrates for functional applications. Through multimodal synchrotron diffraction and spectroscopy analysis with which the materials’ chemical and structural evolution in this novel approach is characterized in details, we further deduce that the contribution of change in entropy should be considered to explain the phase evolution in metal-agent dealloying, in addition to the commonly used enthalpy term in prior studies. Here, the discussion is an important step leading towards better explaining the underlying design principles for controllable 3D nanoarchitecture, as well as exploring a wider range of elemental and substrate selections for new applications.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Exploring Cr and molten salt interfacial interactions for molten salt applications

Molten salts play an important role in various energy-related applications such as high-temperature heat transfer fluids and reaction media. However, the extreme molten salt environment causes the degradation of materials, raising safety and sustainability challenges. A fundamental understanding of material–molten salt interfacial evolution is needed. This work studies the transformation of metallic Cr in molten 50/50 mol% KCl–MgCl 2 via multi-modal in situ synchrotron X-ray nano-tomography, diffraction and spectroscopy combined with density functional theory (DFT) and ab initio molecular dynamics (AIMD) simulations. Notably, in addition to the dissolution of Cr in the molten salt to form porous structures, a δ-A15 Cr phase was found to gradually form as a result of the metal–salt interaction. This phase change of Cr is associated with a change in the coordination environment of Cr at the interface. DFT and AIMD simulations provide a basis for understanding the enhanced stability of δ-A15 Cr vs. bcc Cr, by revealing their competitive phase thermodynamics at elevated temperatures and probing the interfacial behavior of the molten salt at relevant facets. This study provides critical insights into the morphological and chemical evolution of metal–molten salt interfaces. Finally, the combination of multimodal synchrotron analysis and atomic simulation also offers an opportunity to explore a broader range of systems critical to energy applications.

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

Surface coating by mechanofusion modulates bulk charging pathways and battery performance of Ni-rich layered cathodes

Ni-rich layered oxides as high-capacity battery cathodes suffer from degradation at high voltages. Here, we utilize a dry surface modification method, mechanofusion (MF), to achieve enhanced battery stability. The simplicity, high yield, and flexibility make it cost-effective and highly attractive for processing at the industrial scale. The underlying mechanisms responsible for performance improvement are unveiled by a systematic study combining multiple probes, e.g., 3D nano-tomography, spectroscopic imaging, in situ synchrotron diffraction, and finite element analysis (FEA). MF affects the bulk crystallography by introducing partially disordered structure, microstrain, and local lattice variation. Furthermore, the crack initiation and propagation pattern during delithiation are regulated and the overall mechanical fracture is reduced after such surface coating. We validate that MF can alter the bulk charging pathways. Such a synergic effect between surface modification and bulk charge distribution is fundamentally important for designing next-generation battery cathode materials.

25 ENERGY STORAGE↗
DOE OSTI2023

3D and Multimodal X‐Ray Microscopy Reveals the Impact of Voids in CIGS Solar Cells

Small voids in the absorber layer of thin-film solar cells are generally suspected to impair photovoltaic performance. They have been studied on Cu(In,Ga)Se 2 cells with conventional laboratory techniques, albeit limited to surface characterization and often affected by sample-preparation artifacts. Here, synchrotron imaging is performed on a fully operational as-deposited solar cell containing a few tens of voids. By measuring operando current and X-ray excited optical luminescence, the local electrical and optical performance in the proximity of the voids are estimated, and via ptychographic tomography, the depth in the absorber of the voids is quantified. Besides, the complex network of material-deficit structures between the absorber and the top electrode is highlighted. Despite certain local impairments, the massive presence of voids in the absorber suggests they only have a limited detrimental impact on performance.

14 SOLAR ENERGY↗