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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 OSTI2021

Redox Mediated Control of Electrochemical Potential in Liquid Cell Electron Microscopy

Liquid cell electron microscopy enables the study of nanoscale transformations in solvents with high spatial and temporal resolution, but for the technique to achieve its potential requires a new level of control over the reactivity caused by radical generation under electron beam irradiation. An understanding of how to control electron-solvent interactions is needed to further advance the study of structural dynamics for complex materials at the nanoscale. Additionally, we developed an approach that scavenges radicals with redox species that form well-defined redox couples and control the electrochemical potential in situ . This approach enables the observation of electrochemical structural dynamics at near-atomic resolution with precise control of the liquid environment. Analysis of nanocrystal etching trajectories indicates that this approach can be generalized to several chemical systems. The ability to simultaneously observe heterogeneous reactions at near-atomic resolution and precisely control the electrochemical potential enables the fundamental study of complex nanoscale dynamics with unprecedented detail.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Atom-resolved imaging with a silicon tip integrated into an on-chip scanning tunneling microscope

Limited throughput is a shortcoming of the Scanning Tunneling Microscope (STM), particularly when used for atomically precise lithography. To address this issue, we have developed an on-chip STM based on Microelectromechanical-Systems (MEMS) technology. The device reported here has one degree of freedom, replacing the Z axis in a conventional STM. The small footprint of the on-chip STM provides a great opportunity to increase STM throughput by incorporating a number of on-chip STMs in an array to realize parallel STM. The tip methodology adopted for the on-chip STM presented here, which is a batch-fabricated Si tip, makes our design conducive to this goal. In this work, we investigate the capability of this on-chip STM with an integrated Si tip for STM imaging. We integrate the on-chip STM into a commercial ultrahigh-vacuum STM system and perform imaging with atomic resolution on par with conventional STMs but at higher scan speeds due to the higher sensitivity of the MEMS actuator relative to a piezotube. The results attest that it is possible to achieve a parallel and high-throughput STM platform, which is a fully batch-fabricated MEMS STM nanopositioner capable of performing atomic-resolution STM imaging.

Instruments & Instrumentation↗
DOE OSTI2022

Ingrained: An Automated Framework for Fusing Atomic-Scale Image Simulations into Experiments

To fully leverage the power of image simulation to corroborate and explain patterns and structures in atomic resolution microscopy, an initial correspondence between the simulation and experimental image must be established at the outset of further high accuracy simulations or calculations. Furthermore, if simulation is to be used in context of highly automated processes or high-throughput optimization, the process of finding this correspondence itself must be automated. In this work, "ingrained," an open-source automation framework which solves for this correspondence and fuses atomic resolution image simulations into the experimental images to which they correspond, is introduced. Here, the overall "ingrained" workflow, focusing on its application to interface structure approximations, and the development of an experimentally rationalized forward model for scanning tunneling microscopy simulation are described.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Cryogen-free modular scanning tunneling microscope operating at 4-K in high magnetic field on a compact ultra-high vacuum platform

One of the daunting challenges in modern low temperature scanning tunneling microscopy (STM) is the difficulty of combining atomic resolution with cryogen-free cooling. Further functionality needs, such as ultra-high vacuum (UHV), high magnetic field (HF), and compatibility with μm-sized samples, pose additional challenges to an already ambitious build. We present the design, construction, and performance of a cryogen-free, UHV, low temperature, and high magnetic field system for modular STM operation. An internal vibration isolator reduces vibrations in this system, allowing for atomic resolution STM imaging while maintaining a low base temperature of ∼4 K and magnetic fields up to 9 T. Samples and tips can be conditioned in situ utilizing a heating stage, an ion sputtering gun, an e-beam evaporator, a tip treater, and sample exfoliation. In situ sample and tip exchange and alignment are performed in a connected UHV room temperature stage with optical access. Multisite operation without breaking vacuum is enabled by a unique quick-connect STM head design. A novel low-profile vertical transfer mechanism permits transferring the STM between room temperature and the low temperature cryostat.

Instruments & Instrumentation↗
DOE OSTI2022

From ground to excited electronic state dynamics of electron and ion irradiated graphene nanomaterials

Microscopes utilizing convergent electron and ion beams are emerging as powerful tools for both imaging and manipulating two-dimensional materials with atomic resolution, allowing the ultimate limits of nanofabrication to be realized. In this chapter, we detail the use of time-dependent electronic structure theory to determine the excited state properties and reactivity of functionalized graphene nanostructures. A time-dependent density functional theory treatment of electronic excitations of materials is presented, with specific emphasis on predicting the position-dependent electronic response of two-dimensional nanomaterials to electron beams. The method is demonstrated in a study highlighting the important role that electronic excitation can play in opening reaction pathways relevant to atomically precise defect manipulation in graphene. Finally, we provide some perspective on future development directions for methods of simulating nonequilibrium electronic and vibrational dynamics induced by electron/ion beams.

Lingerfelt, David↗
DOE OSTI2022

Imaging atomic-scale chemistry from fused multi-modal electron microscopy

Efforts to map atomic-scale chemistry at low doses with minimal noise using electron microscopes are fundamentally limited by inelastic interactions. Here, fused multi-modal electron microscopy offers high signal-to-noise ratio (SNR) recovery of material chemistry at nano- and atomic-resolution by coupling correlated information encoded within both elastic scattering (high-angle annular dark-field (HAADF)) and inelastic spectroscopic signals (electron energy loss (EELS) or energy-dispersive x-ray (EDX)). By linking these simultaneously acquired signals, or modalities, the chemical distribution within nanomaterials can be imaged at significantly lower doses with existing detector hardware. In many cases, the dose requirements can be reduced by over one order of magnitude. This high SNR recovery of chemistry is tested against simulated and experimental atomic resolution data of heterogeneous nanomaterials.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Quantifying the dislocation content of atomically resolved grain boundary line defects using the Nye tensor

The Nye tensor, which quantifies the density of Burgers vector for a given dislocation line direction, can be effectively used to characterize dislocation content in bulk crystals from atomic-resolution transmission electron microscopy images. The Nye tensor can be calculated from these images, in part because the reference state is simply defined by the lattice of the perfect crystal. The application of the Nye tensor to interfacial line defects, for which the natural reference state is the dichromatic pattern of the two grains in their reference orientation, poses additional challenges. In this work, we present a method that employs the Nye tensor to characterize the edge dislocation content of line defects at grain boundaries from atomic-resolution images. This approach enables us to rapidly characterize all edge dislocation content along a grain boundary. Additionally, the Nye tensor provides information about line defect core structure. Finally, we demonstrate this method on two exemplar defects: a twin boundary disconnection and a facet junction in face-centered cubic Au.

Crystallographic defects↗
DOE OSTI2023

The N‐terminal intrinsically disordered region of Ncb5or docks with the cytochrome b 5 core to form a helical motif that is of ancient origin

Abstract NADH cytochromeb 5 oxidoreductase (Ncb5or) is a cytosolic ferric reductase implicated in diabetes and neurological conditions. Ncb5or comprises cytochromeb 5 (b 5 ) and cytochromeb 5 reductase (b 5 R) domains separated by a CHORD‐Sgt1 (CS) linker domain. Ncb5or redox activity depends on proper inter‐domain interactions to mediate electron transfer from NADH or NADPH via FAD to heme. While full‐length human Ncb5or has proven resistant to crystallization, we have succeeded in obtaining high‐resolution atomic structures of theb 5 domain and a construct containing the CS andb 5 R domains (CS/b 5 R). Ncb5or also contains an N‐terminal intrinsically disordered region of 50 residues that has no homologs in other protein families in animals but features a distinctive, conserved L 34 MDWIRL 40 motif also present in reduced lateral root formation (RLF) protein in rice and increased recombination center 21 in baker's yeast, all attaching to ab 5 domain. After unsuccessful attempts at crystallizing a human Ncb5or construct comprising the N‐terminal region naturally fused to theb 5 domain, we were able to obtain a high‐resolution atomic structure of a recombinant rice RLF construct corresponding to residues 25–129 of human Ncb5or (52% sequence identity; 74% similarity). The structure reveals Trp 120 (corresponding to invariant Trp 37 in Ncb5or) to be part of an 11‐residue α‐helix (S 116 QMDWLKLTRT 126 ) packing against two of the four helices in theb 5 domain that surround heme (α2 and α5). The Trp 120 side chain forms a network of interactions with the side chains of four highly conserved residues corresponding to Tyr 85 and Tyr 88 (α2), Cys 124 (α5), and Leu 47 in Ncb5or. Circular dichroism measurements of human Ncb5or fragments further support a key role of Trp 37 in nucleating the formation of the N‐terminal helix, whose location in the N/b 5 module suggests a role in regulating the function of this multi‐domain redox enzyme. This study revealed for the first time an ancient origin of a helical motif in the N/b 5 module as reflected by its existence in a class of cytochromeb 5 proteins from three kingdoms among eukaryotes.

Biochemistry & Molecular Biology↗
NASA NTRS1993

Scanning tunneling microscopy studies of diamond films and optoelectronic materials

In this report, we report on progress achieved from 12/1/92 to 10/1/93 under the grant entitled 'Scanning Tunneling Microscopy Studies of Diamond Films and Optoelectronic Materials'. We have set-up a chemical vapor deposition (CVD) diamond film growth system and a Raman spectroscopy system to study the nucleation and growth of diamond films with atomic resolution using scanning tunneling microscopy (STM). A unique feature of the diamond film growth system is that diamond films can be transferred directly to the ultrahigh vacuum (UHV) chamber of a scanning tunneling microscope without contaminating the films by exposure to air. The University of North Texas (UNT) provided $20,000 this year as matching funds for the NASA grant to purchase the diamond growth system. In addition, UNT provided a Coherent Innova 90S Argon ion laser, a Spex 1404 double spectrometer, and a Newport optical table costing $90,000 to set-up the Raman spectroscopy system. The CVD diamond growth system and Raman spectroscopy system will be used to grow and characterize diamond films with atomic resolution using STM as described in our proposal. One full-time graduate student and one full-time undergraduate student are supported under this grant. In addition, several graduate and undergraduate students were supported during the summer to assist in setting-up the diamond growth and Raman spectroscopy systems. We have obtained research results concerning STM of the structural and electronic properties of CVD grown diamond films, and STM and scanning tunneling spectroscopy of carbon nanotubes. In collaboration with the transmission electron microscopy (TEM) group at UNT, we have also obtained results concerning the optoelectronic material siloxene. These results were published in refereed scientific journals, submitted for publication, and presented as invited and contributed talks at scientific conferences.

Perez, Jose M.↗
DOE OSTI2024

Secondary-electron imaging of bulk crystalline specimens in an aberration corrected $\text{STEM}$

Atomic-scale electron microscopy traditionally probes thin specimens, with thickness below 100 nm, and its feasibility for bulk samples has not been documented. Here in this study, we explore the practicality of scanning transmission electron microscope (STEM) imaging with secondary electrons (SE), using a silicon-wedge specimen having a maximum thickness of 18 μm. We find that the atomic structure is present in the entire thickness range of the SE images although the background intensity increases moderately with thickness. The consistent intensity of secondary electron (SE) images at atomic positions and the modest increase in intensity in between (background) observed in silicon suggest a limited contribution from SEs generated by backscattered electrons, a conclusion supported by our multislice calculations. We conclude that achieving atomic resolution in SE imaging for bulk specimens is indeed attainable using aberration-corrected STEM and that an aberration-corrected scanning electron microscope (SEM) may have the capacity for atomic-level resolution, holding great promise for future strides in materials research.

25 ENERGY STORAGE↗
DOE OSTI2020

Atomic structures determined from digitally defined nanocrystalline regions

Nanocrystallography has transformed our ability to interrogate the atomic structures of proteins, peptides, organic molecules and materials. By probing atomic level details in ordered sub-10 nm regions of nanocrystals, scanning nanobeam electron diffraction extends the reach of nanocrystallography and in principle obviates the need for diffraction from large portions of one or more crystals. Scanning nanobeam electron diffraction is now applied to determine atomic structures from digitally defined regions of beam-sensitive peptide nanocrystals. Using a direct electron detector, thousands of sparse diffraction patterns over multiple orientations of a given crystal are recorded. Each pattern is assigned to a specific location on a single nanocrystal with axial, lateral and angular coordinates. This approach yields a collection of patterns that represent a tilt series across an angular wedge of reciprocal space: a scanning nanobeam diffraction tomogram. Using this diffraction tomogram, intensities can be digitally extracted from any desired region of a scan in real or diffraction space, exclusive of all other scanned points. Intensities from multiple regions of a crystal or from multiple crystals can be merged to increase data completeness and mitigate missing wedges. It is demonstrated that merged intensities from digitally defined regions of two crystals of a segment from the OsPYL/RCAR5 protein produce fragment-based ab initio solutions that can be refined to atomic resolution, analogous to structures determined by selected-area electron diffraction. In allowing atomic structures to now be determined from digitally outlined regions of a nanocrystal, scanning nanobeam diffraction tomography breaks new ground in nanocrystallography.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Atom Identification in Bilayer Moiré Materials with Gomb-Net

Moiré patterns in van der Waals bilayer materials complicate the analysis of atomic-resolution images, hindering the atomic-scale insight typically attainable with scanning transmission electron microscopy. Here, we report a method to detect the positions and identities of atoms in each of the individual layers that compose twisted bilayer heterostructures. We developed a deep learning model, Gomb-Net, which identifies the coordinates and atomic species in each layer, deconvoluting the moiré pattern. This enables layer-specific mapping of atomic positions and dopant distributions, unlike other commonly used segmentation models which struggle with moiré-induced complexity. Using this approach, we explored the Se atom substitutional site distribution in a twisted fractional Janus WS 2 -WS 2(1–x) Se 2x heterostructure and found that layer-specific implantation sites are unaffected by the moiré pattern’s local energetic or electronic modulation. In conclusion, this advancement enables atom identification within material regimes where it was not possible before, opening new insights into previously inaccessible material physics.

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

In Situ Observation of Domain Wall Lateral Creeping in a Ferroelectric Capacitor

As a promising candidate for next-generation nonvolatile memory devices, ferroelectric oxide films exhibit many emergent phenomena with functional applications, making understanding polarization switching and domain evolution behaviors of fundamental importance. However, tracking domain wall motion in ferroelectric oxide films with high spatial resolution remains challenging. Here, in this study, an in situ biasing approach for direct atomic-scale observations of domain nucleation and sideways motion is presented. By accurately controlling the applied electric field, the lateral translational speed of the domain wall can decrease to less than 2.2 Å s −1 , which is observable with atomic resolution STEM imaging. In situ observations on a capacitor structured PbZr 0.1 Ti 0.9 O 3 /La 0.7 Sr 0.3 MnO 3 heterojunction demonstrate the unique creeping behavior of a domain wall under a critical electric field, with the atomic structure of the creeping domain wall revealed. Moreover, the evolution of the metastable domain wall forms an elongated morphology, which contains a large proportion of charged segments. Phase-field simulations unveil the competition between gradient, elastic, and electrostatic energies that decide this unique domain wall creeping and morphology variation. This work paves the way toward a complete fundamental understanding of domain wall physics and potential modulations of domain wall properties in real devices.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Multislice Electron Tomography Using Four-Dimensional Scanning Transmission Electron Microscopy

Electron tomography offers useful three-dimensional (3D) structural information, which cannot be observed by two-dimensional imaging. By combining annular dark-field scanning transmission electron microscopy (ADF STEM) with aberration correction, the resolution of electron tomography has reached atomic resolution. However, tomography based on ADF STEM inherently suffers from several issues, including a high electron-dose requirement, poor contrast for light elements, and artifacts from image-contrast nonlinearity. Here, we develop an alternative method called multislice electron tomography (MSET) based on four-dimensional STEM tilt series. In this study, our simulations show that multislice-based 3D reconstruction can effectively reduce undesirable reconstruction artifacts from the nonlinear contrast, allowing precise determination of atomic structures with improved sensitivity for low-Z elements, at considerably low electron-dose conditions. We expect that the MSET method can be applied to a wide variety of materials, including radiation-sensitive samples and materials containing light elements whose 3D atomic structures have never been fully elucidated due to electron-dose limitations or nonlinear imaging contrast.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2023

Oxidized structure and Compositional properties of 1144 phase FBS by analytical electron microscopy

The 1144 phase (Ae1A1Fe4As4) shows a strong advantage of engineering fabrication among Fe Iron)-based superconductor (FBS) family due to the robustness of its superconducting properties with respect to chemical inhomogeneities, granted by its uniform crystalline-layered structure. This regularity is furthermore associated to crystalline defects capable of acting as efficient pinning centers, which high critical currents achieved at high fields for these superconductors. Like other FBS phases, its lossless current-carrying capability can be remarkably degraded by distractions at grain boundaries (GBs). GB oxidation is an issue of upmost importance to the realization of the practical FBS application for high field (> 20T) magnet. In this study, we explore oxidized grain boundary and intrinsic grain structural properties of 1144 polycrystalline samples by applying analytical electron microscopy such as atomic resolution scanning transmission electron microscopy and atom probe tomography. These structural properties of samples produced by a mechanochemically assisted synthesis are evaluated following the degradation of superconducting properties due to oxidation. We observe a strong correlation between the contamination at grain boundaries and the decrease of transport properties of the bulk sample, while the crystallin structure seems to be not affected by the oxidation.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2023

Evidence of Xe-incorporation in the bubble superlattice in irradiated U-Mo fuel

For years, researchers have reported competing ideas on the formation of fission gas bubble super lattices in metallic fuels, which was postulated to be comprised of elemental xenon (Xe) atoms. However, the chemical and physical arrangement of these elements within this gas bubble superlattice has not been verified. In this contribution, Xe was chemically profiled using atomic resolution scanning transmission electron microscopy (STEM) and atom probe tomography (APT) techniques in irradiated uranium-molybdenum (U-Mo) fuels. These complementary techniques provide conclusive evidence of Xe presence in bubble superlattice up to fission densities of 4.5×10 21 fissions/cm 3 and provide quantitative assessment of Xe content within the bubble superlattice. Based on the results of simultaneous imaging and spectroscopy using STEM, the chemical composition of the Xe bubble superlattice present in fission densities less than 4.5x10 21 fissions/cm 3 in U-Mo fuel was measured and found to be up to 8±1.3 atomic %. APT data complements STEM findings on Xe distribution in irradiated U-Mo fuel sample. APT showed a chemical composition of 0.7±0.1 atomic%. Finally, this study concludes by providing conclusive evidence that Xe is not only present within an atomically arranged bubble superlattice but provides fundamental insight the physical state of Xe in low enriched U-Mo monolithic fuel.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Direct growth of crystalline SiGe nanowires on superconducting NbTiN thin films

Novel heterostructures created by coupling one-dimensional semiconductor nanowires with a superconducting thin film show great potential toward next-generation quantum computing. Here, by growing high-crystalline SiGe nanowires on a NbTiN thin film, the resulting heterostructure exhibits Ohmic characteristics as well as a shift of the superconducting transition temperature (T c ). The structure was characterized at atomic resolution showing a sharp SiGe/NbTiN interface without atomic interdiffusion. Lattice spacing, as calculated from large-area x-ray diffraction experiments, suggests a potential preferred d-spacing matching between (200) NbTiN and (110) SiGe grains. The observed out-of-plane compressive strain within the NbTiN films coupled with SiGe nanowires explains the downward shift of the superconductivity behavior. The presented results post scientific insights toward functional heterostructures by coupling multi-dimensional materials, which could enable tunable superconductivity that benefits the quantum science applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗