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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 847 records · Page 47
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

An in situ ambient and cryogenic transmission electron microscopy study of the effects of temperature on dislocation behavior in CrCoNi-based high-entropy alloys with low stacking-fault energy

Temperature is known to affect deformation mechanisms in metallic alloys. As temperature decreases, the stacking-fault energy in many face-centered cubic (fcc) alloys decreases, resulting in a change of deformation mode from dislocation slip to deformation twinning. Such an impact of temperature can be more complex in compositionally heterogeneous microstructures that exhibit, for example, local concentration fluctuation such as that in multi-principal element alloys. In this work, we compare the dislocation behavior and mechanical properties of a fcc Cr 20 Mn 10 Fe 30 Co 30 Ni 10 high-entropy alloy at ambient and liquid-nitrogen temperatures. We find that a network of stacking faults is formed by uniformly extended dislocations at ambient temperatures with low stacking-fault energy, whereas at lower temperatures, uneven dissociation of dislocations becomes significant, which results in severe dislocation pile-ups together with their pronounced entanglement. Our findings indicate that as the stacking-fault energy decreases with decreasing temperature, the heterogeneity of the distribution of elements becomes more dominant in tuning the local variation of lattice resistance. As a result, the change in dislocation behavior at low temperatures strongly affects microstructural evolution and consequently leads to significantly more pronounced work hardening.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Invariant discovery of features across multiple length scales: Applications in microscopy and autonomous materials characterization

Physical imaging is a foundational characterization method in areas from condensed matter physics and chemistry to astronomy and spans length scales from atomic to universe. Images encapsulate crucial data regarding atomic bonding, materials microstructures, and dynamic phenomena such as microstructural evolution and turbulence, among other phenomena. The challenge lies in effectively extracting and interpreting this information. Variational Autoencoders (VAEs) have emerged as powerful tools for identifying the underlying factors of variation in image data, providing a systematic approach to distilling meaningful patterns from complex data sets. However, a significant hurdle in their application is the definition and selection of appropriate descriptors reflecting local structures. Here, we introduce the scale-invariant VAE approach (SI-VAE) based on the progressive training of the VAE with the descriptors sampled at different length scales. The SI-VAE allows the discovery of the length scale-dependent factors of variation in the system. Here, we illustrate this approach using the ferroelectric domain images and generalize it to the movies of the electron-beam induced phenomena in graphene and topography evolution across combinatorial libraries. This approach can further be used to initialize the decision making in automated experiments including structure–property discovery and can be applied across a broad range of imaging methods. This approach is universal and can be applied to any spatially resolved data including both experimental imaging studies and simulations, and can be particularly useful for exploration of phenomena such as turbulence and scale-invariant transformation fronts.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Origin of reduced efficiency in GaN-based micro-LEDs studied by scanning near-field optical microscopy

The quantum efficiency of micro-light emitting diodes (micro-LEDs) is lower than that of large area LEDs. This efficiency reduction is typically attributed to the nonradiative Shockley–Read–Hall recombination at the surface defects and current leakage through the sidewall region without a clear distinction between these effects. In this work, we attempt to find out which of these phenomena is most critical for the reduced efficiency of micro-LEDs. This has been done by mapping electroluminescence (EL) and photoluminescence (PL) and measuring PL dynamics in blue GaN micro-LEDs fabricated by dry etching. It has been found that in the as-etched device, the EL intensity is much lower than in devices with KOH etching and atomic layer deposition of SiO 2 . This effect is especially pronounced close to the sidewalls. On the other hand, PL decay times are similar in as-etched and passivated devices, both in their center and at the sidewalls. This allows concluding that the main mechanism of the reduced efficiency of micro-LEDs fabricated by dry etching is the current leakage in the sidewall region and not the nonradiative recombination. The KOH etching has been found to be the most efficient means to eliminate the current leakage.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Three-colour digital holographic microscopy based on a Mach – Zender interferometer and a solid-state RGB laser

We have developed a facility for recording colour digital holograms involving a Mach – Zender interferometer and a pulsed solid-state RGB laser, which radiates simultaneously at three wavelengths: 451, 532, and 634 nm. These wavelengths are obtained in the conversion of the radiation of a pulsed Nd{sup 3+} : YAG laser (1064 nm), which operates in the regime of intracavity parametric oscillation at a wavelength of 1570 nm, with the subsequent conversion of its frequencies to the red, green, and blue spectral regions in nonlinear KTP-crystal elements. The combination of this three-wavelength pulsed light source with the Mach – Zender interferometer provides the simultaneous recording of three spectral digital holograms with one matrix RGB radiation detector. Pulsed three-colour digital holography shows promise for the analysis of fast processes and rapidly varying colour phase objects. (paper)

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2020

The cryoelectron microscopy structure of the human CDK-activating kinase

The human CDK-activating kinase (CAK), a complex composed of cyclin-dependent kinase (CDK) 7, cyclin H, and MAT1, is a critical regulator of transcription initiation and the cell cycle. It acts by phosphorylating the C-terminal heptapeptide repeat domain of the RNA polymerase II (Pol II) subunit RPB1, which is an important regulatory event in transcription initiation by Pol II, and it phosphorylates the regulatory T-loop of CDKs that control cell cycle progression. Here, we have determined the three-dimensional (3D) structure of the catalytic module of human CAK, revealing the structural basis of its assembly and providing insight into CDK7 activation in this context. The unique third component of the complex, MAT1, substantially extends the interaction interface between CDK7 and cyclin H, explaining its role as a CAK assembly factor, and it forms interactions with the CDK7 T-loop, which may contribute to enhancing CAK activity. We have also determined the structure of the CAK in complex with the covalently bound inhibitor THZ1 in order to provide insight into the binding of inhibitors at the CDK7 active site and to aid in the rational design of therapeutic compounds.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Structural transitions in the GTP cap visualized by cryo-electron microscopy of catalytically inactive microtubules

Microtubules (MTs) are nonequilibrium polymers that switch between states of growth and shrinkage. This property is critical for their function and is a consequence of GTP hydrolysis in the MT. The structure of the stable GTP part of the MT (the GTP cap) has previously been inferred from MTs polymerized with nonhydrolyzable GTP analogs. Here, we report high-resolution structures of MTs truly containing GTP, polymerized from mutated, hydrolysis-deficient tubulins. We find that GTP-MTs have an “expanded lattice” and a “closed seam,” structural characteristics possibly responsible for stabilizing the GTP cap. These results provide insight into the structural transitions at growing MT ends, furthering our understanding of the bistable nature of MTs.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Closing the loop between microstructure and charge transport in conjugated polymers by combining microscopy and simulation

A grand challenge in materials science is to identify the impact of molecular composition and structure across a range of length scales on macroscopic properties. We demonstrate a unified experimental–theoretical framework that coordinates experimental measurements of mesoscale structure with molecular-level physical modeling to bridge multiple scales of physical behavior. Here we apply this framework to understand charge transport in a semiconducting polymer. Spatially-resolved nanodiffraction in a transmission electron microscope is combined with a self-consistent framework of the polymer chain statistics to yield a detailed picture of the polymer microstructure ranging from the molecular to device relevant scale. Using these data as inputs for charge transport calculations, the combined multiscale approach highlights the underrepresented role of defects in existing transport models. Short-range transport is shown to be more chaotic than is often pictured, with the drift velocity accounting for a small portion of overall charge motion. Local transport is sensitive to the alignment and geometry of polymer chains. At longer length scales, large domains and gradual grain boundaries funnel charges preferentially to certain regions, creating inhomogeneous charge distributions. While alignment generally improves mobility, these funneling effects negatively impact mobility. The microstructure is modified in silico to explore possible design rules, showing chain stiffness and alignment to be beneficial while local homogeneity has no positive effect. This combined approach creates a flexible and extensible pipeline for analyzing multiscale functional properties and a general strategy for extending the accesible length scales of experimental and theoretical probes by harnessing their combined strengths.

42 ENGINEERING↗
DOE OSTI2024

An In Situ transmission electron microscopy study on the synergistic effects of Au-ion irradiation and high temperature on nuclear graphite microstructure

Abstract The combined effects of high-temperature and heavy-ion irradiation on Mrozowski cracks (MC) and nuclear graphite crystallographic dimensions have been studied using in situ heating and in situ ion-irradiation in the transmission electron microscope (TEM). Electron transparent lamella of nuclear graphite, IG-110, was irradiated using a 2.8 MeV Au beam at an ion flux of 3.991 ×10 10 ion cm −2 s −1 for 70 min at 800 °C. Upon high-temperature irradiation, Mrozowski crack closure was studied quantitatively. The analysis showed linear, positive expansion of nuclear graphite which is significantly different from the dimensional changes previously reported for low-dose neutron irradiation of nuclear graphite in which the material undergoes negative to positive expansion via a turnaround radiation dose. The trend of the thermal expansion coefficient (CTE) of pristine IG-110 in this study is consistent with previous reports in the 100 °C–800 °C temperature region in which the dimensional change ranges from negative to positive values.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Machine Learning-Enabled Image Classification for Automated Electron Microscopy

Abstract Traditionally, materials discovery has been driven more by evidence and intuition than by systematic design. However, the advent of “big data” and an exponential increase in computational power have reshaped the landscape. Today, we use simulations, artificial intelligence (AI), and machine learning (ML) to predict materials characteristics, which dramatically accelerates the discovery of novel materials. For instance, combinatorial megalibraries, where millions of distinct nanoparticles are created on a single chip, have spurred the need for automated characterization tools. This paper presents an ML model specifically developed to perform real-time binary classification of grayscale high-angle annular dark-field images of nanoparticles sourced from these megalibraries. Given the high costs associated with downstream processing errors, a primary requirement for our model was to minimize false positives while maintaining efficacy on unseen images. We elaborate on the computational challenges and our solutions, including managing memory constraints, optimizing training time, and utilizing Neural Architecture Search tools. The final model outperformed our expectations, achieving over 95% precision and a weighted F-score of more than 90% on our test data set. This paper discusses the development, challenges, and successful outcomes of this significant advancement in the application of AI and ML to materials discovery.

Materials Science↗
DOE OSTI2023

Evaluating Stage Motion for Automated Electron Microscopy

Abstract Precise control is an essential and elusive quality of emerging self-driving transmission electron microscopes (TEMs). It is widely understood these instruments must be capable of performing rapid, high-volume, and arbitrary movements for practical self-driving operation. However, stage movements are difficult to automate at scale, owing to mechanical instability, hysteresis, and thermal drift. Such difficulties pose major barriers to artificial intelligence-directed microscope designs that require repeatable, precise movements. To guide design of emerging instruments, it is necessary to understand the behavior of existing mechanisms to identify rate limiting steps for full autonomy. Here, we describe a general framework to evaluate stage motion in any TEM. We define metrics to evaluate stage degrees of freedom, propose solutions to improve performance, and comment on fundamental limits to automated experimentation using present hardware.

47 OTHER INSTRUMENTATION↗
DOE OSTI2023

Design of Electrostatic Aberration Correctors for Scanning Transmission Electron Microscopy

Abstract In a scanning transmission electron microscope (STEM), producing a high-resolution image generally requires an electron beam focused to the smallest point possible. However, the magnetic lenses used to focus the beam are unavoidably imperfect, introducing aberrations that limit resolution. Modern STEMs overcome this by using hardware aberration correctors comprised of many multipole elements, but these devices are complex, expensive, and can be difficult to tune. We demonstrate a design for an electrostatic phase plate that can act as an aberration corrector. The corrector is comprised of annular segments, each of which is an independent two-terminal device that can apply a constant or ramped phase shift to a portion of the electron beam. We show the improvement in image resolution using an electrostatic corrector. Engineering criteria impose that much of the beam within the probe-forming aperture be blocked by support bars, leading to large probe tails for the corrected probe that sample the specimen beyond the central lobe. We also show how this device can be used to create other STEM beam profiles such as vortex beams and probes with a high degree of phase diversity, which improve information transfer in ptychographic reconstructions.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2020

3D Nanotomography of calcium silicate hydrates by transmission electron microscopy

Calcium silicate hydrate (C-S-H), is the principal hydration product of Portland cement that mainly contributes to the physical and mechanical properties of concrete. This paper aims to investigate the three-dimensional structure of C-S-H with Ca/Si ratios of 1.0 and 1.6 at the nanoscale using electron tomography. The 3D reconstructions and selected region of interest analysis confirm that the morphology of both C-S-H materials are foil-like structures. Additionally, the difference between the two materials is the density of elongated structures. C-S-H with Ca/Si ratio 1.6 is clearly composed of denser particles compared to the other C-S-H material due to overlapping of the foil-like structure. Pore analysis shows that C-S-H 1.0 and C-S-H 1.6 have porosities 69.2% and 49.8% respectively. Pore size distribution also reveals that C-S-H 1.0 has pore size range between 0-250 nm and C-S-H 1.6 between 0-100 nm. The pore network's size of C-S-H 1.0 is significantly larger than 1.6. This study illustrates the capability of using electron tomography to determine the 3D nanoscale structure of cementitious products and to distinguish between C-S-H 1.0 and 1.6.

42 ENGINEERING↗
DOE OSTI2025

Orientation microscopy–assisted grain boundary analysis for protonic ceramic cell electrolytes

Abstract Grain boundaries in protonic ceramic cell (PCC) electrolytes hinder proton transport, reducing interfacial conductivity. In multicomponent PCC electrolytes, the inclusion of sintering aids further accentuates the complexity of grain boundaries. In this study, we synthesize nanocrystalline BaCe 0.4 Zr 0.4 Y 0.1 Yb 0.1 O 3− δ thin films via pulsed laser deposition and analyze their grain boundary character distributions using orientation data collected by precession electron diffraction technique. The results reveal an anisotropic distribution of grain boundary characters, with notably high populations of 180°‐tilt and twist grain boundaries. These findings provide critical insights into identifying the predominant grain boundaries in this PCC electrolyte material, assessing the vast five‐dimensional grain boundary space.

Patel, Sooraj [School of Aerospace and Mechanical ↗
DOE OSTI2020

Field emission microscopy of carbon nanotube fibers: Evaluating and interpreting spatial emission

In this work, the authors quantify field emission properties of cathodes made from carbon nanotube (CNT) fibers. The cathodes were arranged in different configurations to determine the effect of cathode geometry on the emission properties. Various geometries were investigated including (1) flat cut fiber tip, (2) folded fiber, (3) looped fiber, and (4) fibers wound around a cylinder. The authors employ a custom field emission microscope to quantify I-V characteristics in combination with laterally resolved field-dependent electron emission area. Additionally, they look at the very early emission stages, first when a CNT fiber is turned on for the first time, which is then followed by multiple ramp-up/down runs. Upon the first turn on, all fibers demonstrated limited and discrete emission area. During ramping runs, all CNT fibers underwent multiple (minor and/or major) breakdowns, which improved emission properties in that turn-on field decreased and field enhancement factor and emission area both increased. It is proposed that breakdowns are responsible for removing initially undesirable emission sites caused by stray fibers higher than average. This initial breakdown process gives way to a larger emission area that is created when the CNT fiber subcomponents unfold and align with the electric field. Overall, the authors' results form the basis for careful evaluation of CNT fiber cathodes for dc or low frequency pulsed power systems in which large uniform area emission is required or for narrow beam high frequency applications in which high brightness is a must.

Image processing↗
DOE OSTI2022

Fast scanning in x-ray microscopy: the effects of offset in the central stop position

Scanning of lightweight circular diffractive optics, separate from central stops and apertures, is emerging as an approach to exploit advances in synchrotron x-ray sources. We consider the effects in a scanning microscope of offsets between the optic and its central stop and find that scan ranges of up to about half the diameter of the optic are possible with only about a 10% increase in the focal spot width. Finally, for large scanning ranges, we present criteria for the working distance between the last aperture and the specimen to be imaged.

47 OTHER INSTRUMENTATION↗
DOE OSTI2023

Reconstruction of simulated electrostatic potentials by automatic differentiation-based phase retrieval in electron microscopy imaging

Measuring interfacial electrostatic potentials is vital to understanding many fundamental materials properties. A variety of TEM methods exist for measuring electric potentials from the phase shift produced on an electron wave as it passes through a sample. However, most are either experimentally challenging or poorly suited to resolving nanoscale features. Here, we demonstrate the viability of a simple, automatic differentiation-based exit wave reconstruction from a focal series of images to accurately measure nanoscale electric potentials. Here, the analysis suggests that under optimal measurement conditions, electric potentials can be resolved to less than 0.06 V in magnitude and less than 1 nm in spatial extent.

36 MATERIALS SCIENCE↗