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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 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Differential multi-probe thermal transport measurements of multi-walled carbon nanotubes grown by chemical vapor deposition

Carbon nanotubes (CNTs) are quasi-one dimensional nanostructures that display both high thermal conductivity for potential thermal management applications and intriguing low-dimensional phonon transport phenomena. In comparison to the advances made in the theoretical calculation of the lattice thermal conductivity of CNTs, thermal transport measurements of CNTs have been limited by either the poor temperature sensitivity of Raman thermometry technique or the presence of contact thermal resistance errors in sensitive two-probe resistance thermometry measurements. Here we report advances in a multi-probe measurement of the intrinsic thermal conductivity of individual multi-walled CNT samples that are transferred from the growth substrate onto the measurement device. The sample-thermometer thermal interface resistance is directly measured by this multi-probe method and used to model the temperature distribution along the contacted sample segment. The detailed temperature profile helps to eliminate the contact thermal resistance error in the obtained thermal conductivity of the suspended sample segment. A differential electro-thermal bridge measurement method is established to enhance the signal-to-noise ratio and reduce the measurement uncertainty by over 40%. The obtained thermal resistances of multiple suspended segments of the same MWCNT samples increase nearly linearly with increasing length, revealing diffusive phonon transport as a result of phonon-defect scattering in these MWCNT samples. The measured thermal conductivity increases with temperature and reaches up to 390 ± 20 W m –1 K –1 at room temperature for a 9-walled MWCNT. In conclusion, theoretical analysis of the measurement results suggests submicron phonon mean free paths due to extrinsic phonon scattering by extended defects such as grain boundaries. The obtained thermal conductivity is decreased by a factor of 3 upon electron beam damage and surface contamination of the CNT sample.

42 ENGINEERING↗
DOE OSTI2020

Investigation of synchrotron X-ray induced oxidation of Ag–Cu thin-film

Combinatorial Ag-Cu thin-films were irradiated by synchrotron X-ray in air to investigate the beam damage on the surface of the thin-film. The main effect was found to be oxidation with the oxidation state primarily depending on film composition: CuO formed on the pure Cu film, whereas Cu 2 O formed in the presence of Ag. Meanwhile, formation of crystalline Ag 2 O 2 was favored and preferentially in the Ag-rich area. Lastly, these results are of great importance in studying the oxidation of noble metal nano-film, and in the characterization of nano-films using synchrotron X-ray.

36 MATERIALS SCIENCE↗
DOE OSTI2021

High-Resolution Imaging of Unstained Polymer Materials

Electron microscopy has played an important role in polymer characterization. Traditionally, electron diffraction is used to study crystalline polymers while transmission electron microscopy is used to study microphase separation in stained block copolymers and other multiphase systems. We describe developments that eliminate the barrier between these two approaches - it is now possible to image polymer crystals with atomic resolution. The focus of this Review is on high-resolution imaging (30 Å and smaller) of unstained polymers. Recent advances in hardware allow for capturing numerous (as many as 105) low-dose images from an unperturbed specimen; beam damage is a significant barrier to high-resolution electron microscopy of polymers. Machine-learning-based software is then used to sort and average the images to retrieve pristine structural information from a collection of noisy images. Acknowledging the heterogeneity in polymer samples prior to averaging is essential. Molecular conformations in a wide range of amphiphilic block copolymers, polymerized ionic liquids, and conjugated polymers can be gleaned from two-dimensional projections (2D), three-dimensional (3D) tomograms, and four-dimensional (4D) scanning transmission electron microscopy (STEM) data sets where 2D diffraction patterns are taken as a function of position. Some methods such as phase contrast STEM have been used to image closely related materials such as metal-organic frameworks but not polymers. With improvements in hardware and software, such methods may soon be applied to polymers. Our goal is to provide a comprehensive understanding of the strategies toward the high-resolution imaging of radiation sensitive polymer materials at different length scales.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Evidence of Morphological Change in Sulfur Cathodes upon Irradiation by Synchrotron X-rays

While the development of lithium–sulfur battery cathodes has benefited substantially from the use of in situ and ex situ X-ray absorption studies, the degree of undesired influence from synchrotron radiation has not been studied. In this study, we present evidence of severe beam damage on sulfur cathodes under irradiation by synchrotron X-rays. Specifically, X-ray fluorescence mapping with relatively low dosage was conducted to observe the morphological changes after conducting X-ray absorption spectroscopy (XAS). Under open-circuit conditions, the morphology of the sulfur spontaneously changes and tends to migrate out of the region of XAS sampling. Our work indicates that effort should be placed in first obtaining a no-change/stable open-circuit baseline when attempting to conduct in operando studies of lithium–sulfur batteries using synchrotron radiation with an energy of <7.7 keV and a flux of >6 × 10 12 photons s –1 .

25 ENERGY STORAGE↗
DOE OSTI2024

Digital twins and deep learning segmentation of defects in monolayer MX 2 phases

Developing methods to understand and control defect formation in nanomaterials offers a promising route for materials discovery. Monolayer MX 2 phases represent a particularly compelling case for defect engineering of nanomaterials due to the large variability in their physical properties as different defects are introduced into their structure. However, effective identification and quantification of defects remain a challenge even as high-throughput scanning transmission electron microscopy methods improve. This study highlights the benefits of employing first principles calculations to produce digital twins for training deep learning segmentation models for defect identification in monolayer MX 2 phases. Around 600 defect structures were obtained using density functional theory calculations, with each monolayer MX 2 structure being subjected to multislice simulations for the purpose of generating the digital twins. Several deep learning segmentation architectures were trained on this dataset, and their performances evaluated under a variety of conditions such as recognizing defects in the presence of unidentified impurities, beam damage, grain boundaries, and with reduced image quality from low electron doses. Further, this digital twin approach allows benchmarking different deep learning architectures on a theory dataset, which enables the study of defect classification under a broad array of finely controlled conditions. It thus opens the door to resolving the underpinning physical reasons for model shortcomings and potentially chart paths forward for automated discovery of materials defect phases in experiments.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Wehnelt photoemission in an ultrafast electron microscope: Stability and usability

We tested and compared the stability and usability of three different cathode materials and configurations in a thermionic-based ultrafast electron microscope: (1) on-axis thermionic and photoemission from a custom 100 μm diameter LaB 6 source with a graphite guard ring, (2) off-axis photoemission from the Ni aperture surface of the Wehnelt electrode, and (3) on-axis thermionic and photoemission from a custom 200 μm diameter polycrystalline Ta source. For each cathode type and configuration, including the Ni Wehnelt aperture, we illustrate how the photoelectron beam-current stability is deleteriously impacted by simultaneous cooling of the source following thermionic heating. Furthermore, we demonstrate usability via collection of parallel- and convergent-beam electron diffraction patterns and by formation of the optimum probe size. We find that usability of the off-axis Ni Wehnelt-aperture photoemission is at least comparable to on-axis LaB 6 thermionic emission, as well as to on-axis photoemission [the heretofore conventional approach to ultrafast electron microscopy (UEM) in thermionic-based instruments]. However, the stability and achievable beam currents for off-axis photoemission from the Wehnelt aperture were superior to that of the other cathode types and configurations, regardless of the electron-emission mechanism. Beam-current stability for this configuration was found to be ±1% (one standard deviation from the mean) for 70 min (longest duration tested), and steady-state beam current was reached within the sampling-time resolution used here (~1 s) for 15 pA beam currents (i.e., 460 electrons per packet for a 200 kHz repetition rate). Repeatability and robustness of the steady-state condition were also found to be within ±1% of the mean. We discuss the implications of these findings for UEM imaging and diffraction experiments, for pulsed-beam damage measurements, and for practical switching between optimum conventional TEM and UEM operation within the same instrument.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2020

Development of low temperature fuel cell holders for Operando x-ray micro and nano computed tomography to visualize water distribution

Abstract Synchrotron x-ray imaging techniques, like x-ray computed tomography (CT) and radiography have proven instrumental in expanding the communities knowledge of complex transport and reaction kinetics in electrochemical devices such as fuel cells and electrolyzers. This work presents the development of novel x-ray CT imaging techniques for operando visualization of water within low temperature fuel cells at spatial resolutions spanning the micro and nano scales. The design of operando sample holders, for both micro x-ray CT and nano CT experiments is described in depth, and prototypes of these sample holders were evaluated across a set of requirements, the most important of which are x-ray transmissibility, electrical conductivity and mechanical stability. Water segmentation from micro x-ray CT data was enabled by an image subtraction method, where the image without water is subtracted from the one with water. Through iterative experimentations, the operando nano CT cell was developed to optimize mechanical compression, electric conductivity and gas flow. While three-dimensional fuel cell reconstructions were shown possible, there remain challenges to overcome at typical lower energies (8 keV) due to beam damage, whereas it is not as significant for higher energies (>17.5 keV).

Kulkarni, Devashish↗
DOE OSTI2025

X-ray absorption spectroscopy of lanmodulin-derived peptides bound to rare earth elements

A sustainable and robust supply chain of rare earth elements (REEs) is necessary to meet our consumer, national security and clean energy goals. However, current intra-REE separation technologies (e.g. solvent extraction) are costly and carry a heavy environmental burden. Therefore, the development of new aqueous based ligands that are selective for individual REEs will be integral in future REE production systems. To develop these ligands, an understanding of how ligand coordination structure relates to selectivity is imperative. We used X-ray absorption spectroscopy (XAS) to observe the local structure around four lanthanide (Ln) ions (La, Ce, Pr and Nd) complexed by water and several relevant chelating ligands [lanmodulin EF-hand 1 peptides (LanM1), ethyl­enedi­amine­tetra­acetic acid (EDTA), amino­tris­(methyl­ene­phospho­nic acid) (ATMP) and citric acid]. To collect these liquid-phase XAS spectra, we developed a new flow cell that prevents bubble interference and beam damage to the samples. In the X-ray absorption near-edge structure (XANES), we observed energy shifts in the white line, white line broadening and differences in the white line intensity of different Ln–ligand complexes between ligands. In the extended X-ray absorption fine structure (EXAFS), we distinguished differences in peak intensity and distance between coordinating ligands. Differences in the local coordination structure between Ln–LanM1 peptide complexes were more subtle compared with the other ligands (La–water, La–EDTA, La–ATMP and La–citric acid complexes). Further XANES and EXAFS studies, in combination with modelling and other techniques, could greatly improve our structural knowledge of how these aqueous ligands bind Ln ions and how they can be used to design more selective ligands for more efficient and sustainable REE separations.

EDTA↗
DOE OSTI2020

Understanding Measurement Artifacts Causing Inherent Cation Gradients in Depth Profiles of Perovskite Photovoltaics with TOF-SIMS

Time-of-flight secondary-ion mass spectrometry (TOF-SIMS) is one of the few techniques that can obtain chemical information from the hybrid organic-inorganic perovskite solar cells (PSCs) in one dimension (standard depth profiling), two dimensions (high-resolution 100-nm imaging), as well as three dimensions (tomography combining high-resolution imaging with depth profiling). We have very recently developed thermo-mechanical methods to cleave perovskite samples at the back transparent conducting oxide/PSC interface. This allowed for depth-profiling from the back of the device to the front. The resultant profiles answered the lingering question of the apparent A-site cation gradient typically seen in TOF-SIMS depth profiles. In fact, this gradient is a measurement artifact due to beam damage that the community should be informed of as TOF-SIMS data become more commonly employed. Methods of mitigating this artifact by altering the measurement conditions are also presented.

14 SOLAR ENERGY↗
DOE OSTI2024

High‐speed 4‐dimensional scanning transmission electron microscopy using compressive sensing techniques

Abstract Here we show that compressive sensing allows 4‐dimensional (4‐D) STEM data to be obtained and accurately reconstructed with both high‐speed and reduced electron fluence. The methodology needed to achieve these results compared to conventional 4‐D approaches requires only that a random subset of probe locations is acquired from the typical regular scanning grid, which immediately generates both higher speed and the lower fluence experimentally. We also consider downsampling of the detector, showing that oversampling is inherent within convergent beam electron diffraction (CBED) patterns and that detector downsampling does not reduce precision but allows faster experimental data acquisition. Analysis of an experimental atomic resolution yttrium silicide dataset shows that it is possible to recover over 25 dB peak signal‐to‐noise ratio in the recovered phase using 0.3% of the total data. Lay abstract : Four‐dimensional scanning transmission electron microscopy (4‐D STEM) is a powerful technique for characterizing complex nanoscale structures. In this method, a convergent beam electron diffraction pattern (CBED) is acquired at each probe location during the scan of the sample. This means that a 2‐dimensional signal is acquired at each 2‐D probe location, equating to a 4‐D dataset. Despite the recent development of fast direct electron detectors, some capable of 100kHz frame rates, the limiting factor for 4‐D STEM is acquisition times in the majority of cases, where cameras will typically operate on the order of 2kHz. This means that a raster scan containing 256^2 probe locations can take on the order of 30s, approximately 100‐1000 times longer than a conventional STEM imaging technique using monolithic radial detectors. As a result, 4‐D STEM acquisitions can be subject to adverse effects such as drift, beam damage, and sample contamination. Recent advances in computational imaging techniques for STEM have allowed for faster acquisition speeds by way of acquiring only a random subset of probe locations from the field of view. By doing this, the acquisition time is significantly reduced, in some cases by a factor of 10‐100 times. The acquired data is then processed to fill‐in or inpaint the missing data, taking advantage of the inherently low‐complex signals which can be linearly combined to recover the information. In this work, similar methods are demonstrated for the acquisition of 4‐D STEM data, where only a random subset of CBED patterns are acquired over the raster scan. We simulate the compressive sensing acquisition method for 4‐D STEM and present our findings for a variety of analysis techniques such as ptychography and differential phase contrast. Our results show that acquisition times can be significantly reduced on the order of 100‐300 times, therefore improving existing frame rates, as well as further reducing the electron fluence beyond just using a faster camera.

Robinson, Alex W.↗
NASA NTRS1990

A probe for real-time images of particle beams and their analyses in a merged-beams apparatus

A real-time charged particle beam probe was developed, which can be used both as a beam diagnostic (beam tuning) and to quantitatively determine the three-dimensional density distribution of a beam. The probe consists of a microchannel plate, an aluminized phosphor screen deposited on a fiber-optic faceplate, a flexible fiber-optic bundle, and a charge injection device (CID) in tandem. Digital or analog video output of the CID is fed into a computer or oscilloscope, respectively, for analysis or observation. The probe can be moved continuously along the beams' paths to obtain 'pictures' of the beam at any desired interval, thus giving three-dimensional form factors. The beams, singly or simultaneously, may be observed on the monitor facilitating the task of beam adjustment for optimum overlap. The digital output is used for quantitative computation of the beam overlaps. The device is linear with beam intensity, but the performance degrades with time due to beam damage of the microchannel plate.

Forand, J. L.↗
NASA NTRS1992

Optical and TEM study of shock metamorphism from the Sedan test site

Thus far, detailed petrologic studies of shock metamorphism have been performed on samples recovered from laboratory experiments and on a few natural impactites. The loading history of these samples is quite different: In particular, laboratory experiments spend only a short time (less than 1 microsec) at peak pressure, whereas natural impactites may have stress pulses from 0.1 - 1 ms. On the other hand, laboratory experiments have known stress histories; natural impactites do not. Natural samples are also subjected to thousands or millions of years of postshock annealing and/or weathering. A useful intermediate case is that of nuclear detonation. Stress pulses for these events can reach 0.1 ms or higher, and samples are obtained in pristine condition. All three types of loading produce stresses of hundreds of kilobars. Samples studied were taken from the Sedan nulcear test site, and consist of a coarse-grained granodiorite containing quartz, K-feldspar, cordierite, and hornblende. Samples were studied optically in this section, then were thinned with an ion mill and studied by transmission electron microscopy (TEM). Optically, quartz and K-feldspar displayed numerous sets of planar deformation features (PDF's) identical to the nondecorated PDF's seen in laboratory samples and many natural impactites. TEM study showed that the PDF's in quartz and feldspar corresponded to densely packed wide transformation lamellae identical to those described in laboratory studies. The transformation lamellae in both minerals were amorphous, with no sign of high-pressure phases. In the case of K-feldspar only, narrow sublamellae extended outward from some wide lamellae. Quartz, which was more abundant and studied more extensively, contained no shock-induced dislocations. Some planar features were also seen in cordierite, but could not be identified due to rapid beam damage. No shock defects were seen in hornblende in TEM. The shock-induced defects present at the Sedan site are very similar to those seen in shock recovery experiments, and also to those present at certain natural events (e.g., Meteor Crater). This suggests that shock deformation in quartz is not strongly dependent on shock pulse duration, and that laboratory recovery experiments are useful simulations of natural impact events.

Gratz, A. J.↗
NASA NTRS1999

Delamination Modeling of Composites for Improved Crash Analysis

Finite element crash modeling of composite structures is limited by the inability of current commercial crash codes to accurately model delamination growth. Efforts are made to implement and assess delamination modeling techniques using a current finite element crash code, MSC/DYTRAN. Three methods are evaluated, including a straightforward method based on monitoring forces in elements or constraints representing an interface; a cohesive fracture model proposed in the literature; and the virtual crack closure technique commonly used in fracture mechanics. Results are compared with dynamic double cantilever beam test data from the literature. Examples show that it is possible to accurately model delamination propagation in this case. However, the computational demands required for accurate solution are great and reliable property data may not be available to support general crash modeling efforts. Additional examples are modeled including an impact-loaded beam, damage initiation in laminated crushing specimens, and a scaled aircraft subfloor structures in which composite sandwich structures are used as energy-absorbing elements. These examples illustrate some of the difficulties in modeling delamination as part of a finite element crash analysis.

Fleming, David C.↗
NASA NTRS1999

Delamination Modeling of Composites for Improved Crash Analysis

Finite element crash modeling of composite structures is limited by the inability of current commercial crash codes to accurately model delamination growth. Efforts are made to implement and assess delamination modeling techniques using a current finite element crash code, MSC/DYTRAN. Three methods are evaluated, including a straightforward method based on monitoring forces in elements or constraints representing an interface; a cohesive fracture model proposed in the literature; and the virtual crack closure technique commonly used in fracture mechanics. Results are compared with dynamic double cantilever beam test data from the literature. Examples show that it is possible to accurately model delamination propagation in this case. However, the computational demands required for accurate solution are great and reliable property data may not be available to support general crash modeling efforts. Additional examples are modeled including an impact-loaded beam, damage initiation in laminated crushing specimens, and a scaled aircraft subfloor structures in which composite sandwich structures are used as energy-absorbing elements. These examples illustrate some of the difficulties in modeling delamination as part of a finite element crash analysis.

Fleming, David C.↗
NASA NTRS2013

Stardust Interstellar Preliminary Examination III: Infrared Spectroscopic Analysis of Interstellar Dust Candidates

Under the auspices of the Stardust Interstellar Preliminary Examination, picokeystones extracted from the Stardust Interstellar Dust Collector were examined with synchrotron Fourier transform infrared (FTIR) microscopy to establish whether they contained extraterrestrial organic material. The picokeystones were found to be contaminated with varying concentrations and speciation of organics in the native aerogel, which hindered the search for organics in the interstellar dust candidates. Furthermore, examination of the picokeystones prior to and post X-ray microprobe analyses yielded evidence of beam damage in the form of organic deposition or modification, particularly with hard X-ray synchrotron X-ray fluorescence. From these results, it is clear that considerable care must be taken to interpret any organics that might be in interstellar dust particles. For the interstellar candidates examined thus far, however, there is no clear evidence of extraterrestrial organics associated with the track and/or terminal particles. However, we detected organic matter associated with the terminal particle in Track 37, likely a secondary impact from the Al-deck of the sample return capsule, demonstrating the ability of synchrotron FTIR to detect organic matter in small particles within picokeystones from the Stardust interstellar dust collector.

Interstellar↗
DOE OSTI2022

Plasma Processing for In-Situ Field Emission Mitigation of Superconducting Radiofrequency (SRF) Cryomodules

Field emission (FE) is one of the main limiting factors of superconducting radio-frequency (SRF) cavities operating in accelerators and it occurs whenever contaminants, like dust, metal flakes or even absorbates, are present on the surface of the cavity high electric field region. Field emission reduces the maximum achievable accelerating field and generates free electrons that may interact with the beam, damage or activate the beamline. One practical method that can be used to mitigate this problem is in-situ plasma cleaning, or plasma processing. The development of a processing that can be applied in-situ is extremely advantageous, since it enables the recovery of the cryomodule performance without the need of disassembling the whole cryomodule, which is an extremely expensive and time-consuming process. On the other hand, plasma processing only requires the cryomodule warm-up to room-temperature and the subsequent processing of the contaminated cavities. The entire process is reasonably quick and involves a limited number of personnel. For these reasons we would like to advocate for continuing to invest in the R&D of plasma processing to optimize its applicability in cryomodules and for extending the technique to other frequency ranges and cavities geometries.

43 PARTICLE ACCELERATORS↗
NASA NTRS1998

Potential for EMU Fabric Damage by Electron Beam and Molten Metal During Space Welding for the International Space Welding Experiment

As a consequence of preparations concerning the International Space Welding Experiment (ISWE), studies were performed to better understand the effect of molten metal contact and electron beam impingement with various fabrics for space suit applications. The question arose as to what would occur if the electron beam from the Ukrainian Universal Hand Tool (UHT) designed for welding in space were to impinge upon a piece of Nextel AF-62 ceramic cloth designed to withstand temperatures up to 1427 C. The expectation was that the electron beam would lay down a static charge pattern with no damage to the ceramic fabric. The electron beam is capable of spraying the fabric with enough negative charge to repel further electrons from the fabric before significant heating occurs. The static charge pattern would deflect any further charge accumulation except for a small initial amount of leakage to the grounded surface of the welder. However, when studies were made of the effect of the electron beam on the insulating ceramic fabric it was surprisingly found that the electron beam did indeed burn through the ceramic fabric. It was also found that the shorter electron beam standoff distances had longer burnthrough times than did some greater electron beam standoff distances. A possible explanation for the longer burnthrough times for the small electron beam standoff distance would be outgassing of the fabric which caused the electron beam hand-tool to cycle on and off to provide some protection for the cathodes. The electron beam hand tool was observed to cycle off at the short standoff distance of two inches likely due to vapors being outgassed. During the electron beam welding process there is an electron leakage, or current leakage, flow from the fabric. A static charge pattern is initially laid down by the electron beam current flow. The static charge makes up the current leakage flow which initially slightly heats up the fabric. The initially laid down surface charge leaks a small amount of current. The rate at which the current charge leaks from the fabric controls how fast the fabric heats up. As the ceramic fabric is heated it begins to outgass primarily from contamination/impurities atoms or molecules on and below the fabric surface. The contaminant gases ionize to create extra charge carriers and multiply a current of electrons. The emitted gas which ionized in the electron leakage flow promotes further leakage. Thus, the small leakage of charge from the fabric surface is enhanced by outgassing. When the electron beam current makes up the lost current, the incoming electrons heat the fabric and further enhance the outgassing. The additional leakage promotes additional heating up of the ceramic fabric. The electrons bound to the ceramic fabric surface leak off more and more as the surface gets hotter promoting even greater leakage. The additional electrons that result also gain energy in the field and produce further electrons. Eventually the process becomes unstable and accelerates to the point where a hole is burned through the fabric.

Fragomeni, James M.↗