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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 181 records · Page 10
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Imaging Photonic Resonances within an All‐Dielectric Metasurface via Photoelectron Emission Microscopy

Dielectric metasurfaces, through volume‐type photonic resonances, enable precise control of light‐matter interactions for applications including imaging, holography, and sensing. The application space of dielectric metasurfaces has extended from infrared to visible wavelengths by incorporating high refractive index materials, such as titanium dioxide (TiO 2 ). Understanding the fundamental and fabrication limits for these applications requires metrology with nanoscale resolution, sensitivity to electromagnetic fields within the meta‐atom volume, and far‐field excitation. In this work, photoelectron emission microscopy (PEEM) is used to image field distributions of photonic resonances in a TiO 2 metasurface excited with far‐field, visible‐wavelength illumination. The local volumetric field variations within the meta‐atoms are analyzed as a function of illumination angle and polarization by comparing photoelectron images to finite‐difference time‐domain simulations. This study determines the inelastic mean free path of very low‐energy (<1 eV) photoelectrons to be 35 ± 10 nm, which is comparable to the meta‐atom height thereby highlighting PEEM sensitivity to resonances within the volume. Additionally, the simulations reveal high sensitivity of PEEM images to an in‐plane component of the illumination k ‐vector. These results demonstrate that photoelectron imaging with subwavelength resolution offers unique advantages for examining light‐matter interactions in volume‐type (as opposed to surface) photonic modes within dielectric nanophotonic structures.

electron inelastic mean free path↗
DOE OSTI2025

Effect of Stoichiometry on the Structure and Polarization of BaTiO 3

Barium titanate (BaTiO 3 ) is a material of interest for photonic device applications due to its strong optical non-linearity. However, BaTiO 3 -based devices have not found widespread adoption, in part due to the challenges associated with synthesizing high quality thin-films. Here, high-resolution scanning transmission electron microscope (STEM) imaging is used to investigate the atomic structure of both on- and off-stoichiometric BaTiO 3 synthesized by molecular beam epitaxy (MBE). Here, this investigation reveals an asymmetry in the way the BaTiO 3 atomic lattice accommodates off-stoichiometry growth and unveils features beyond what is expected from diffraction or surface characterization techniques. Excess titanium incorporates into the BaTiO 3 lattice to form pervasive defects despite titanium-rich films having a low surface roughness and high-quality appearance in diffraction. Excess barium forms a rough, water-soluble surface layer but does not significantly impact the quality of the BaTiO 3 lattice. STEM is used to map titanium atom displacement in real-space. The average displacement distance is 30–60 pm in the strained thin-films, higher than the <20 pm displacement in bulk BaTiO 3 . Additionally, the titanium atom displacement direction deviates from the c-axis of the unit cell, which may have implications for the material's electro-optic tensor and thus for electro-optic device design.

Cavanagh, Ashley E. [Harvard Univ., Cambridge, MA ↗
DOE OSTI2025

Wafer-scale waveguide sidewall roughness scattering loss characterization by image processing

Photonic integrated circuits (PICs) are vital for developing affordable, high-performance optoelectronic devices that can be manufactured at an industrial scale, driving innovation and efficiency in various applications. Optical loss of modes in thin film waveguides and devices is a critical measure of their performance. Thin film growth, lithography, masking, and etching processes are imperfect processes that introduce significant sidewall and top-surface roughness and cause dominating optical losses in waveguides and photonic structures. This roughness, as perturbations couple light from guided to far-field radiation modes, leads to scattering losses that can be estimated from theoretical models. Typically, with UV-based lithography, sidewall roughness is significantly larger than wafer-top surface roughness. Atomic force microscopy (AFM) imaging measurement gives a 3D and high-resolution roughness profile, but the measurement is inconvenient, costly, and unscalable for large-scale PICs and at wafer-scale. Here, we evaluate the sidewall roughness profile based on 2D high-resolution scanning electron microscope (SEM) imaging. We characterized the loss on two homemade nitride and oxide films on 3-inch silicon wafers with 12 waveguide devices on each and correlated the scattering loss estimated from a 2D image-based sidewall profile and theoretical Payne model. The lowest loss of guided fundamental transverse electric (TE 0 ) mode is found at 0.075 dB/cm at 633 nm across 24 devices, a record at visible wavelength. Our work shows 100% success (edge continuity span exceeding 95% of image width/height) in edge detection in image processing of all images to estimate autocorrelation function and optical mode loss. These demonstrations offer valuable insights into waveguide sidewall roughness and a comparison of experimental and 2D SEM image processing based loss estimations with applications in loss characterization at wafer-scale PICs.

Khurana, Mohit (ORCID:0000000207898672)↗
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 OSTI2020

Intra- and Intermolecular Self-Assembly of a 20-nm-Wide Supramolecular Hexagonal Grid.

For the past three decades, the coordination-driven self-assembly of three-dimensional structures has undergone rapid progress; however, parallel efforts to create large discrete two-dimensional architectures-as opposed to polymers-have met with limited success. The synthesis of metallo-supramolecular systems with well-defined shapes and sizes in the range of 10-100 nm remains challenging. Here we report the construction of a series of giant supramolecular hexagonal grids, with diameters on the order of 20 nm and molecular weights greater than 65 kDa, through a combination of intra- and intermolecular metal-mediated self-assembly steps. The hexagonal intermediates and the resulting self-assembled grid architectures were imaged at submolecular resolution by scanning tunnelling microscopy. Characterization (including by scanning tunnelling spectroscopy) enabled the unambiguous atomic-scale determination of fourteen hexagonal grid isomers.

Zhang, Zhe↗
DOE OSTI2022

In vitro investigation of protein assembly by combined microscopy and infrared spectroscopy at the nanometer scale

The nanoscale structure and dynamics of proteins on surfaces has been extensively studied using various imaging techniques, such as transmission electron microscopy and atomic force microscopy (AFM) in liquid environments. These powerful imaging techniques, however, can potentially damage or perturb delicate biological material and do not provide chemical information, which prevents a fundamental understanding of the dynamic processes underlying their evolution under physiological conditions. Here, we use a platform developed in our laboratory that enables acquisition of infrared (IR) spectroscopy and AFM images of biological material in physiological liquids with nanometer resolution in a cell closed by atomically thin graphene membranes transparent to IR photons. In this work, we studied the self-assembly process of S-layer proteins at the graphene-aqueous solution interface. The graphene acts also as the membrane separating the solution containing the proteins and Ca 2+ ions from the AFM tip, thus eliminating sample damage and contamination effects. The formation of S-layer protein lattices and their structural evolution was monitored by AFM and by recording the amide I and II IR absorption bands, which reveal the noncovalent interaction between proteins and their response to the environment, including ionic strength and solvation. Our measurement platform opens unique opportunities to study biological material and soft materials in general.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

First-principles simulation of light-ion microscopy of graphene

The extreme sensitivity of 2D materials to defects and nanostructure requires precise imaging techniques to verify presence of desirable and absence of undesirable features in the atomic geometry. Helium-ion beams have emerged as a promising materials imaging tool, achieving up to 20 times higher resolution and 10 times larger depth-of-field than conventional or environmental scanning electron microscopes. Here, we offer first-principles theoretical insights to advance ion-beam imaging of atomically thin materials by performing real-time time-dependent density functional theory simulations of single impacts of 10–200 keV light ions in free-standing graphene. Here we predict that detecting electrons emitted from the back of the material (the side from which the ion exits) would result in up to three times higher signal and up to five times higher contrast images, making 2D materials especially compelling targets for ion-beam microscopy. This predicted superiority of exit-side emission likely arises from anisotropic kinetic emission. The charge induced in the graphene equilibrates on a sub-fs time scale, leading to only slight disturbances in the carbon lattice that are unlikely to damage the atomic structure for any of the beam parameters investigated here.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Single-shot imaging with randomized structured illumination at a free electron laser

Stroboscopic nanoscale imaging with free electron laser light is revolutionizing our understanding of fast dynamics in heterogeneous systems. The short wavelength of X-ray and extreme ultraviolet radiation makes it possible to achieve nanoscale resolution, while resonance with atomic transitions gives access to electronic and magnetic degrees of freedom. Here, we report on our implementation of a recently developed imaging method, randomized probe imaging, at a free electron laser. The advantage of randomized probe imaging over existing methods is its compatibility with extended and strongly scattering samples. Our implementation delivers robust single-shot reconstructions at up to a full-pitch resolution of 400 nm over a field of view with a 40 µm diameter. We also demonstrate single-shot imaging of magnetic domain structures using circular dichroism at resonance, paving the way to future time-resolved studies of magnetic dynamics, shock physics, and the dynamics of collective electronic phases.

47 OTHER INSTRUMENTATION↗
DOE OSTI2025

PhaseT3M: 3D imaging at 1.6 Å resolution via electron cryo-tomography with nonlinear phase retrieval

Electron cryo-tomography (cryo-ET) enables 3D imaging of complex, radiation-sensitive structures with molecular detail. However, image contrast from the interference of scattered electrons is nonlinear with atomic density and multiple scattering further complicates interpretation. These effects degrade resolution, particularly in conventional reconstruction algorithms, which assume linearity. Particle averaging can reduce such issues but is unsuitable for heterogeneous or dynamic samples ubiquitous in biology, chemistry, and materials sciences. Here, we develop a phase retrieval-based cryo-ET method, PhaseT3M. We experimentally demonstrate its application to an approximately 7 nm Co3O4 nanoparticle on an approximately 30 nm carbon substrate, achieving a maximum resolution of 1.6 Å, surpassing conventional limits using standard cryo-TEM equipment. PhaseT3M uses a multislice model for multiple scattering and Bayesian optimization for alignment and computational aberration correction, with a positivity constraint to recover ‘missing wedge’ information. Applied directly to biological particles, it enhances reconstruction quality and reduces artifacts, establishing a standard for routine 3D imaging with phase contrast.

Biophysics↗
DOE OSTI2023

Facile hermetic TEM grid preparation for molecular imaging of hydrated biological samples at room temperature

Abstract Although structures of vitrified supramolecular complexes have been determined at near-atomic resolution, elucidating in situ molecular structure in living cells remains a challenge. Here, we report a straightforward liquid cell technique, originally developed for real-time visualization of dynamics at a liquid-gas interface using transmission electron microscopy, to image wet biological samples. Due to the scattering effects from the liquid phase, the micrographs display an amplitude contrast comparable to that observed in negatively stained samples. We succeed in resolving subunits within the protein complex GroEL imaged in a buffer solution at room temperature. Additionally, we capture various stages of virus cell entry, a process for which only sparse structural data exists due to their transient nature. To scrutinize the morphological details further, we used individual particle electron tomography for 3D reconstruction of each virus. These findings showcase this approach potential as an efficient, cost-effective complement to other microscopy technique in addressing biological questions at the molecular level.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2021

Deep Bayesian local crystallography

Abstract The advent of high-resolution electron and scanning probe microscopy imaging has opened the floodgates for acquiring atomically resolved images of bulk materials, 2D materials, and surfaces. This plethora of data contains an immense volume of information on materials structures, structural distortions, and physical functionalities. Harnessing this knowledge regarding local physical phenomena necessitates the development of the mathematical frameworks for extraction of relevant information. However, the analysis of atomically resolved images is often based on the adaptation of concepts from macroscopic physics, notably translational and point group symmetries and symmetry lowering phenomena. Here, we explore the bottom-up definition of structural units and symmetry in atomically resolved data using a Bayesian framework. We demonstrate the need for a Bayesian definition of symmetry using a simple toy model and demonstrate how this definition can be extended to the experimental data using deep learning networks in a Bayesian setting, namely rotationally invariant variational autoencoders.

36 MATERIALS SCIENCE↗
DOE OSTI2023

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

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

36 MATERIALS SCIENCE↗
DOE OSTI2025

X-ray and Neutron Radiography for Quantitative Material Reconstructions

Radiography is a powerful tool to determine the interior structure of objects. X-ray radiography is widely used and provides high-resolution images, though X-rays have limited transmission through materials of high atomic number (Z) and density. In contrast, neutrons can penetrate many materials that are heavily attenuating to X-rays, such as metals, providing contrast in the inner layers of highly attenuating items. Past work has shown the value in using both X-ray and neutron radiography for estimating material thicknesses, though that work was limited to simulated data. Here, we demonstrate quantitative material reconstructions using experimental X-ray and neutron radiography data from lab-based systems, accurately modeling radiography system responses to within a few percent to enable quantitative measures of material thickness. We demonstrate the utility of neutron radiography and X-ray radiography for these quantitative reconstructions and introduce methods for using their complementarity to improve image quality and optimize experimental design.

Gilbert, Andrew J.↗
DOE OSTI2021

High signal-to-noise ratio differential conductance spectroscopy

The scanning tunneling microscope (STM) has enabled manipulation and interrogation of surfaces with atomic-scale resolution. Electronic information about a surface is obtained by combining the imaging capability of the STM with scanning tunneling spectroscopy, i.e., measurement of current-voltage (I/V) characteristics of the surface. We propose a change in the STM feedback loop that enables capturing a higher quality dI/dV image. A high frequency dither voltage is added to the bias voltage of the sample, and the fundamental frequency component of the resulting current is demodulated. The in-phase component of this signal is then plotted along with the X and Y position data, constructing the dI/dV image. Here, we show that by incorporating notch filters in the STM feedback loop, we may utilize a high-amplitude dither voltage to significantly improve the quality of the obtained dI/dV image.

42 ENGINEERING↗
NASA NTRS1997

NASA/University Joint Venture in Space Science (JOVE)

This system has an immense complex of optical knots that extend several galactic diameters to the north and south of the main optical object. These are star forming regions, some of which are the size of small irregular galaxies. It has a nearby companion called the 'seashell' owing to its disturbed appearance. The data had been reduced and images formed; a figure is attached. The high resolution observations show that the atomic hydrogen (HI) encompasses not only the N-S complex of optical knots but it forms an incomplete ring or tail that extends approximately 3 arcmins to the west. The seashell was not detected, and the HI associated with NGC 5291 itself shows a very large velocity range. The formation mechanism for this disturbed and distorted complex is unclear. X-ray emission suggesting ram sweeping is also observed. This author favors an explanation involving an interaction between the two components, NGC 5291 and the seashell. We are witnessing the formation of tidal tails and bridges between the galaxies and the associated ejecta. Ram sweeping occurs as the system moves bodily through the medium of the cluster of galaxies, Abell 3574, to which NGC 5291 et al. belong. There are numerous concentrations of HI, mostly along the N-S star forming complexes which generally coincide with the optical knots; the larger features contain several x109 solar mass, again the magnitude of a small irregular galaxy. Each knot was compared to a set of criteria designed to test if the feature was stable against its own internal kinetic energy, and stable against the tidal forces of the host galaxy. At least one of the objects (Knot B) appears to be a bound system suggesting that it is a genuinely young dwarf irregular galaxy that has evolved from the material associated with his interacting complex. We conclude that we are witnessing the early evolution of young galaxies and that NGC 5291 and the seashell are a nursery.

Gottesman, Stephen T.↗
NASA NTRS2003

Improved Process for Fabricating Carbon Nanotube Probes

An improved process has been developed for the efficient fabrication of carbon nanotube probes for use in atomic-force microscopes (AFMs) and nanomanipulators. Relative to prior nanotube tip production processes, this process offers advantages in alignment of the nanotube on the cantilever and stability of the nanotube's attachment. A procedure has also been developed at Ames that effectively sharpens the multiwalled nanotube, which improves the resolution of the multiwalled nanotube probes and, combined with the greater stability of multiwalled nanotube probes, increases the effective resolution of these probes, making them comparable in resolution to single-walled carbon nanotube probes. The robust attachment derived from this improved fabrication method and the natural strength and resiliency of the nanotube itself produces an AFM probe with an extremely long imaging lifetime. In a longevity test, a nanotube tip imaged a silicon nitride surface for 15 hours without measurable loss of resolution. In contrast, the resolution of conventional silicon probes noticeably begins to degrade within minutes. These carbon nanotube probes have many possible applications in the semiconductor industry, particularly as devices are approaching the nanometer scale and new atomic layer deposition techniques necessitate a higher resolution characterization technique. Previously at Ames, the use of nanotube probes has been demonstrated for imaging photoresist patterns with high aspect ratio. In addition, these tips have been used to analyze Mars simulant dust grains, extremophile protein crystals, and DNA structure.

Stevens, R.↗
DOE OSTI2022

Spatial resolution in secondary-electron microscopy

Here, we first review the significance of resolution and contrast in electron microscopy, and the effect of the electron optics on these two quantities. We then outline the physics of the generation of secondary electrons (SE) and their transport and emission from the surface of a specimen. Contrast and resolution are discussed for different kinds of SE imaging in scanning (SEM) and scanning-transmission (STEM) instruments, with some emphasis on the observation of individual atoms and atomic columns in a thin specimen. The possibility of achieving atomic resolution from a bulk specimen at SEM energies is also considered.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Design and construction of a quantum matter synthesizer

The quantum matter synthesizer (QMS) is a new quantum simulation platform in which individual particles in a lattice can be resolved and re-arranged into arbitrary patterns. The ability to spatially manipulate ultracold atoms and control their tunneling and interactions at the single-particle level allows full control of a many-body quantum system. We present the design and characterization of the QMS, which integrates into a single ultra-stable apparatus a two-dimensional optical lattice, a moving optical tweezer array formed by a digital micromirror device, and site-resolved atomic imaging. We demonstrate excellent mechanical stability between the lattice and tweezer array with relative fluctuations below 10 nm, diffraction-limited imaging at a resolution of 655 nm, and high-speed real-time control of the tweezer array at a 2.52 kHz refresh rate, which will be adopted to realize fast rearrangement of atoms. The QMS also features new technologies and schemes, such as nanotextured anti-reflective windows and all-optical long-distance transport of atoms.

47 OTHER INSTRUMENTATION↗