Search NASA⌕ Search

SEARCH · Search NASA

Results for “Dynamic TEM”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 451 records · Page 25

Direct Mapping of Charge Distribution during Lithiation of Ge Nanowires Using Off-Axis Electron Holography

The successful operation of rechargeable batteries relies on reliable insertion/ extraction of ions into/from the electrodes. The battery performance and the response of the electrodes to such ion insertion and extraction are directly related to the spatial distribution of the charge and its dynamic evolution. However, it remains unclear how charge is distributed in the electrodes during normal battery operation. In this work, we have used offaxis electron holography to measure charge distribution during lithium ion insertion into a Ge nanowire (NW) under dynamic operating conditions. We discovered that the surface region of the Ge core is negatively charged during the core-shell lithiation of the Ge NW, which is counterbalanced by positive charge on the inner surface of the lithiated LixGe shell. The remainder of the lithiated LixGe shell is free from net charge, consistent with its metallic characteristics. The present work provides a vivid picture of charge distribution and dynamic evolution during Ge NW lithiation and should form the basis for tackling the response of these and related materials under real electrochemical conditions.

25 ENERGY STORAGE↗

Kinetic phase evolution of spinel cobalt oxide during lithiation

Spinel cobalt oxide has been proposed to undergo a multiple-step reaction during the electrochemical lithiation process. Understanding the kinetics of the lithiation process in this compound is crucial to optimize its performance and cyclability. In this work, we have utilized a low-angle annular dark-field scanning transmission electron microscopy method to visualize the dynamic reaction process in real time and study the reaction kinetics at different rates. We show that the particles undergo a two-step reaction at the single-particle level, which includes an initial intercalation reaction followed by a conversion reaction. At low rates, the conversion reaction starts after the intercalation reaction has fully finished, consistent with the prediction of density functional theoretical calculations. At high rates, the intercalation reaction is overwhelmed by the subsequently nucleated conversion reaction, and the reaction speeds of both the intercalation and conversion reactions are increased. Phase-field simulations show the crucial role of surface diffusion rates of lithium ions in controlling this process. Furthermore, this work provides microscopic insights into the reaction dynamics in non-equilibrium conditions and highlights the effect of lithium diffusion rates on the overall reaction homogeneity as well as the performance.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗

Probing the role of local tunnel variations in early-stage lithiation of α-MnO₂ nanowires via in situ TEM

Understanding lithium-ion transport in tunnel-structured manganese oxides is essential for designing high-performance lithium-ion battery electrode materials. Here, we elucidate the early-stage lithiation mechanism of potassium-stabilized α-MnO 2 nanowires using in situ transmission electron microscopy (TEM) coupled with electron energy-loss spectroscopy (EELS), high-resolution TEM (HRTEM), and geometric phase analysis (GPA). Real-time TEM imaging reveals clear volume expansion at the reaction front, while EELS analysis uncovers lithium-ion diffusion far beyond this region, where no visible expansion is observed, indicating fast, defect-assisted transport. GPA and HRTEM analyses show that localized tensile and compressive strain fields, originating from pre-existing local tunnel structural variations, persist after lithiation. The tensile-strained regions enable lithium-ion insertion with minimal lattice distortion, offering additional free volume that facilitates rapid lithium-ion accommodation ahead of the structural transformation. Our results demonstrate a local tunnel variation-mediated fast diffusion pathway that precedes bulk reaction, underscoring the critical role of local strain in enabling early-stage lithium transport. Given the structural versatility of MnO 2 and its ability to accommodate diverse atomic arrangements beyond the well-known tunnel phases (β-, γ-, δ-, λ-, R-phases), our findings highlight the importance of understanding and engineering local structural environments. This work provides fundamental insights into the interplay between defects, strain, and ion dynamics, and presents defect engineering as a promising approach to enhance both rate performance and structural stability in manganese-based cathodes.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Grain growth of nanocrystalline aluminum under tensile deformation: A combined in situ TEM and atomistic study

Nanocrystalline Al thin films have been strained in situ in a transmission electron microscope using two separate nanomechanical techniques involving a push-to-pull device and a microelectromechanical system (MEMS) device. Deformation-induced grain growth was observed to occur via stress-assisted grain boundary migration with extensive grain growth occurring in the necked region, indicating that the increase in local stress drives the boundary migration. Under applied tensile stresses close to the ultimate tensile strength of 450 MPa for a nanocrystalline Al specimen, measured boundary migration speeds are 0.2 – 0.7 nm s -1 for grains outside necked region and increases to 2.5 nm s -1 for grains within the necked region where the local estimated tensile stresses are elevated to around 630 MPa. By tracking grain boundary motion over time, molecular dynamics simulations showed qualitative agreement in terms of pronounced grain boundary migration with the experimental observations. The combined in situ observation and molecular dynamics simulation results underscore the important role of stress-driven grain growth in plastically deforming nanocrystalline metals, leading to intergranular fracture through predominant grain boundary sliding in regions with large localized deformation.

36 MATERIALS SCIENCE↗

Improving the cycle stability of LiCoPO{sub 4} nanocomposites as 4.8 V cathode: Stepwise or synchronous surface coating and Mn substitution

Nanostructured LiCo{sub 1−x}Mn{sub x}PO{sub 4}/C (x = 0 and 0.05) materials were successfully produced as superior quality cathodes by combined sol-gel and carbothermal reduction methods. X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HR-TEM), energy dispersive spectroscopy (EDS), fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), inductively coupled plasma (ICP), cyclic voltammetry (CV) and galvanostatic measurements were applied to determine the phase purity, morphology and electrochemical qualifications. HR-TEM analysis reveals that the thickness of the surface carbon layer of 5 to 10 nm range with the uniform distribution. LiCo{sub 0·95}Mn{sub 0·05}PO{sub 4}/C particles were between 40 and 80 nm and the same material exhibits a higher and stable reversible capacity (140 mA h g{sup −1}) with the long voltage plateau (4.76 V). Substitution of Co{sup 2+} with Mn{sup 2+} in LiCoPO{sub 4}/C has an influence on the initial discharge capacity and excellent cycling behaviour. The obtained results have attributed that production dynamics in nano-synthesis, the coating process with proper carbon source and an effective doping represent three parameters to prepare favorable cathode materials. - Highlights: • Structural, morphological and electrochemical effects of Mn doped LiCo{sub 1−x}Mn{sub x}PO{sub 4}–C electrodes are investigated. • Cheap, effective and simple sol-gel assisted carbothermal reduction approach is used. • After 60th cycle, capacity retention is almost 92% for LiCo{sub 0·95}Mn{sub 0.05}PO{sub 4}–C electrode. • Mn-doped sample exhibits distinctive oxidation (4.76 V and 4.12 V) peaks.

36 MATERIALS SCIENCE↗

Modeling thermal spike driven reactions at low temperature and application to zirconium carbide radiation damage

The development of TEM-visible damage in materials under irradiation at cryogenic temperatures cannot be explained using classical rate theory modeling with thermally activated reactions since at low temperatures thermal reaction rates are too low. Although point defect mobility approaches zero at low temperature, the thermal spikes induced by displacement cascades enable some atom mobility as it cools. In this work a model is developed to calculate “athermal” reaction rates from the atomic mobility within the irradiation-induced thermal spikes, including both displacement cascades and electronic stopping. The athermal reaction rates are added to a simple rate theory cluster dynamics model to allow for the simulation of microstructure evolution during irradiation at cryogenic temperatures. The rate theory model is applied to in-situ irradiation of ZrC and compares well at cryogenic temperatures. The results show that the addition of the thermal spike model makes it possible to rationalize microstructure evolution in the low temperature regime.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Microstructure development during rapid alloy solidification

Abstract Solidification processing of structural alloys can take place over an extremely wide range of solid–liquid interface velocities spanning six orders of magnitude, from the low-velocity constitutional supercooling limit of microns/s to the high-velocity absolute stability limit of m/s. In between these two limits, the solid–liquid interface is morphologically unstable and typically forms cellular-dendritic microstructures, but also other microstructures that remain elusive. Rapid developments in additive manufacturing have renewed the interest in modeling the high-velocity range, where approximate analytical theories provide limited predictions. In this article, we discuss recent advances in phase-field modeling of rapid solidification of metallic alloys, including a brief description of state-of-the-art experiments used for model validation. We describe how phase-field models can cope with the dual challenge of carrying out simulations on experimentally relevant length- and time scales and incorporating nonequilibrium effects at the solid–liquid interface that become dominant at rapid rates. We present selected results, illustrating how phase-field simulations have yielded unprecedented insights into high-velocity interface dynamics, shedding new light on both the absolute stability limit and the formation of banded microstructures that are a hallmark of rapid alloy solidification near this limit. We also discuss state-of-the-art experiments used to validate those insights. Graphical abstract

36 MATERIALS SCIENCE↗

Synthesis of magnesiowüstite nanocrystallites embedded in an amorphous silicate matrix via low energy multiple ion implantations

The synthesis process is presented for experimentally simulating modifications in cosmic dust grains using sequential ion implantations or irradiations followed by thermal annealing. Cosmic silicate dust analogues were prepared via implantation of 20–80 keV Fe - , Mg - , and O - ions into commercially available p-type silicon (100)wafers. The as-implanted analogues are amorphous with a Mg/(Fe+Mg) ratio of 0.5 tailored to match theoretical abundances in circumstellar dusts. Before the ion implantations were performed, Monte-Carlo-based ion-solid interaction codes were used to model the dynamic redistribution of the implanted atoms in the silicon substrate. 600 keV helium ion irradiation was performed on one of the samples before thermal annealing. Two samples were thermally annealed at a temperature appropriate for an M-class stellar wind, 1000 K, for 8.3 h in a vacuum chamber with a pressure of 1 x 10 -7 torr. The elemental depth profiles were extracted utilizing Rutherford Backscattering Spectrometry (RBS) in the samples before and after thermal annealing. X-ray diffraction (XRD)analysis was employed for the identification of various phases in crystalline minerals in the annealed analogues. Transmission electron microscopy (TEM) analysis was utilized to identify specific crystal structures. RBS analysis shows redistribution of the implanted Fe, Mg, and O after thermal annealing due to incorporation into the crystal structures for each sample type. XRD patterns along with TEM analysis showed nanocrystalline Mg and Fe oxides with possible incorporation of additional silicate minerals.

79 ASTRONOMY AND ASTROPHYSICS↗

Unraveling Spatio-Temporal Chemistry Evolution in Laser Ablation Plumes and Its Relation to Initial Plasma Conditions

The chemistry evolution in a laser ablation plume depends strongly on its initial physical conditions. In this article, we investigate the impact of plasma generation conditions on the interrelated phenomena of expansion dynamics, plasma chemistry, and physical conditions. Plasmas are produced from a uranium metal target in air using nanosecond, femtosecond, and femtosecond filament-assisted laser ablation. Time-resolved two-dimensional spectral imaging was performed for evaluating the spatio-temporal evolu-tion of atoms, diatoms, polyatomic molecules, and nanoparticles in situ. Emission spectral features reveal that molecular formation occurs at early times in both femtosecond and filament ablation plumes, although with different temporal decay. In contrast, mo-lecular formation is found to occur at much later times in nanosecond plasma evolution. Spectral modeling is used to infer tem-poral behavior of plasma excitation temperature, and results highlighted that nanosecond plume temperatures decay rapidly while plumes generated by filament ablation show slowest decay. In this work, we find U atoms and UO molecules co-exist in ultrafast laser produced plasmas even at early times after plasma onset owing to favorable temperatures for molecular formation. Regardless of irradiation conditions, plume emission features showed presence of higher oxides (i.e. UxOy), although with different temporal histories. Our study provides insight into the impact of plasma generation conditions on chemistry evolution in plasmas produced from traditional focused femtosecond, nanosecond, and filament-assisted laser ablation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Three-Dimensional Engineered High Fidelity Normal Human Lung Tissue-Like Assemblies (TLA) as Targets for Human Respiratory Virus Infections

Unlike traditional two-dimensional (2D) cell cultures, three-dimensional (3D) tissue-like assemblies (TLA) (Goodwin et aI, 1992, 1993, 2000 and Nickerson et aI. , 2001,2002) offer high organ fidelity with the potential to emulate the infective dynamics of viruses and bacteria in vivo. Thus, utilizing NASA micro gravity Rotating Wall Vessel (RWV) technology, in vitro human broncho-epithelial (HBE) TLAs were engineered to mimic in vivo tissue for study of human respiratory viruses. These 3D HBE TLAs were propagated from a human broncho-tracheal cell line with a mesenchymal component (HBTC) as the foundation matrix and either an adult human broncho-epithelial cell (BEAS-2B) or human neonatal epithelial cell (16HBE140-) as the overlying element. Resulting TLAs share several characteristic features with in vivo human respiratory epithelium including tight junctions, desmosomes and cilia (SEM, TEM). The presence of epithelium and specific lung epithelium markers furthers the contention that these HBE cells differentiate into TLAs paralleling in vivo tissues. A time course of infection of these 3D HBE TLAs with human respiratory syncytial virus (hRSV) wild type A2 strain, indicates that virus replication and virus budding are supported and manifested by increasing virus titer and detection of membrane-bound F and G glycoproteins. Infected 3D HBE TLAs remain intact for up to 12 days compared to infected 2D cultures that are destroyed in 2-3 days. Infected cells show an increased vacuolation and cellular destruction (by transmission electron microscopy) by day 9; whereas, uninfected cells remain robust and morphologically intact. Therefore, the 3D HBE TLAs mimic aspects of human respiratory epithelium providing a unique opportunity to analyze, for the first time, simulated in vivo viral infection independent of host immune response.

Goodwin, T. J.↗

Atomic-scale imaging of ultrafast materials dynamics

The advent of short-pulse electron and x-ray sources has enabled pump-probe approaches for elucidating ultrafast materials dynamics. From such studies, a comprehensive picture of the time-dependent evolution of the initial steps of energy deposition, propagation, relaxation, and conversion in a wide range of materials can be generated. In this article, we provide an overview of the capabilities of femtosecond electron and x-ray scattering for resolving structural dynamics of materials. With such approaches, time resolutions are ultimately limited by the durations of the electron and x-ray pulses, and dynamics can be studied at length scales spanning atomic to mesoscale dimensions. The articles in this issue represent a cross section of the vigorous activity occurring in the study of light-induced ultrafast materials dynamics as it relates to charge carriers, surfaces and interfaces, lattice-coupling mechanisms, coherent structural motions, and next-generation instrument development. Here, the approaches highlighted here are leading to new physical insights, new possibilities for engineering the properties of matter, and ultimately, a new understanding of materials functionality on ultrasmall and ultrashort spatiotemporal scales.

36 MATERIALS SCIENCE↗

Dynamic Analysis of Recalescence Process and Interface Growth of Eutectic Fe{sub 82}B{sub 17}Si{sub 1} Alloy

By employing the glass fluxing technique in combination with cyclical superheating, the microstructural evolution of the undercooled Fe{sub 82}B{sub 17}Si{sub 1} alloy in the obtained undercooling range was studied. With increase in undercooling, a transition of cooling curves was detected from one recalescence to two recalescences, followed by one recalescence. The two types of cooling curves were fitted by the break equation and the Johnson–Mehl–Avrami–Kolmogorov model. Based on the cooling curves at different undercoolings, the recalescence rate was calculated by the multi-logistic growth model and the Boettinger–Coriel–Trivedi model. Both the recalescence features and the interface growth kinetics of the eutectic Fe{sub 82}B{sub 17}Si{sub 1} alloy were explored. The fitting results that were obtained using TEM (SAED), SEM and XRD were consistent with the changing rule of microstructures. Finally, the relationship between the microstructure and hardness was also investigated.

36 MATERIALS SCIENCE↗

In-situ monitoring of atomically dispersed Pt sites supported on OMS-2 during CO 2 activation

Atomically dispersed catalysts have drawn great interest lately, as they showcase a high density of active sites, selectivity, and high turnover frequencies in oxidation chemistry due to labile oxygen activation. In contrast, the applications of these catalysts have lagged in reduction reactions due to the ambiguity caused by the sintering and restructuring of active sites. To bridge this gap, the evolution of Pt 4+ isomorphically substituted into an octahedral molecular sieve structure (OMS-2) under reductive conditions was correlatively characterized using multiple in-situ analytical techniques such as ambient pressure X-ray photoelectron spectroscopy, environmental transmission electron microscopy, and solid-state nuclear magnetic resonance. The surface dynamics of the Pt single atoms were revealed during the Reverse Water Gas Shift (RWGS) reaction, where the active sites were identified as two-coordinated platinum single atoms. Under reaction, we show nonbinding atoms adjacent to the single atoms restructured the motif of the single atoms to Pt 2+ via ion mobility of potassium, increasing the activation energy by 25.6 kJ/mol. Here, this work also highlights the potential for increased stability of the single atom sites via isomorphic substitution of the metal oxide support, since the Pt-OMS-2 catalyst retained activity for about 33 h before deactivation, after which nanoparticles were observed in TEM images. This work offers a new perspective in single atom synthesis using the metal oxide as the host for the single atom site, instead of adatoms on the surface

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Dynamic recrystallization kinetics and microstructure evolution of an AZ91D magnesium alloy during hot compression

Highlights: • DRX kinetic model is developed for the aged AZ91D magnesium alloy. • The DRX behavior in different strained regions was investigated. • Four morphologies of the second phase were proposed during the hot compression tests. • The nucleation mechanisms of the DRX grains were clarified. - Abstract: The flow behavior of as-cast AZ91D magnesium alloy was evaluated by isothermal compression tests within the temperatures of 220 °C, 260 °C, 300 °C, 340 °C, and 380 °C, and the strain rates of 0.001, 0.01, 0.1, 1 and 10s{sup −1}. Based on the stress-strain curve and hyperbolic sine function, the thermal activation energy and the strain rate sensitivity of the material were determined to be 142.2726 kJ·mol{sup −1} and 0.142, respectively. The S type evolution of the dynamic recrystallization with the increasing strain that dynamic recrystallization (DRX) model obtained from stress and strain data. There was a good consistency between the proposed DRX kinetics model and microstructure observation results. Combining isothermal compression specimens with finite element and scanning electron microscopy (SEM) analysis indicated that the sample can be divided into rarely recrystallized region, partially recrystallized region and completely recrystallized region, which falls within the dense deformation zone, free deformation zone and severe deformation zone, respectively. The different forms of the β-Mg{sub 17}Al{sub 12} phase induced by compression tests were confirmed by SEM. Nucleation mechanisms of the DRX were discussed with reference to the transmission electron microscope (TEM) analysis results.

36 MATERIALS SCIENCE↗

Revealing the synergistic effects of sequential and simultaneous dual beam irradiations in tungsten via in-situ TEM

Elucidating the synergistic effects of different energetic beams on the radiation response of nuclear materials is critical for developing an improved methodology for their evaluation when exposed to extreme environments. This article describes in-situ sequential (He implantation followed by Kr irradiation and vice-versa) and simultaneous (heavy ion Kr irradiation and He implantation) dual beam irradiations performed on tungsten at 1223 K. Dislocation loop density, average area, and total loop damage as a function of irradiation history and dose/fluence are quantified. The loop Burgers vectors and cavity damage (cavity density, size and total change in volume) are also determined at the final maximum dose for each condition. The loop damage evolution was different in all cases, with the smallest loop damage observed in the simultaneous experiment. Annihilation of Kr generated dislocation loops during He implantation in the Kr + He experiment was an unanticipated observation that may be explained by the dynamic evolution of dislocation loop sink strengths and time-dependent defect fluxes. Dislocation loop raft formation, denuded zones near extended defects, and cavity damage are compared across the different conditions. The phenomena observed and discussed in this work will stimulate further experimental and computational modeling activities leading to improved fundamental understanding of the irradiation response of nuclear materials under reactor-similar environments.

36 MATERIALS SCIENCE↗

In situ observation of self-assembled Fe{sub 13}Ge{sub 8} nanowires growth on anisotropic Ge (1 1 0) surface

Highlights: Black-Right-Pointing-Pointer Epitaxial Fe{sub 13}Ge{sub 8} nanowries growth and shape evolution on Ge (1 1 0) studied by in situ UHV-TEM. Black-Right-Pointing-Pointer Single type of morphology and unique orientation of nanowires formed at elevated temperatures. Black-Right-Pointing-Pointer Uniform control of the nanowires morphology at different temperatures can be succeeded. -- Abstract: Self-assembled iron germanide nanowires (NWs) were grown by directly depositing Fe onto a Ge (1 1 0) substrate, in an in situ ultra-high vacuum transmission electron microscope from 430 to 500 Degree-Sign C. All observed NWs had a similar length/width aspect ratio ({approx}8:1) at all deposition temperatures, as well as the same elongation orientation with respect to the underlying Ge (1 1 0) substrate. The growth dynamics was investigated by real time observations of NWs growth at elevated temperatures. It is elucidated that the formation of NWs in similar shape at all deposited temperatures is attributed to the similar activation energy barriers in length and width of NWs, which can result in the constant growth rate independent of growth temperatures. Furthermore, the difference in pre-exponential factor along the length and width of growing islands arose due to the anisotropic constraint of the Ge (1 1 0) substrate, leading to the unique elongation of NWs. This growth dynamics suggests the possibility of uniform control of the morphology of self-assembled NWs, as well as other morphologies of bottom-up fabricated devices, at different deposition temperatures.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

A correlation between grain boundary character and deformation twin nucleation mechanism in coarse-grained high-Mn austenitic steel

Abstract In polycrystalline materials, grain boundaries are known to be a critical microstructural component controlling material’s mechanical properties, and their characters such as misorientation and crystallographic boundary planes would also influence the dislocation dynamics. Nevertheless, many of generally used mechanistic models for deformation twin nucleation in fcc metal do not take considerable care of the role of grain boundary characters. Here, we experimentally reveal that deformation twin nucleation occurs at an annealing twin (Σ3{111}) boundary in a high-Mn austenitic steel when dislocation pile-up at Σ3{111} boundary produced a local stress exceeding the twining stress, while no obvious local stress concentration was required at relatively high-energy grain boundaries such as Σ21 or Σ31. A periodic contrast reversal associated with a sequential stacking faults emission from Σ3{111} boundary was observed by in-situ transmission electron microscopy (TEM) deformation experiments, proving the successive layer-by-layer stacking fault emission was the deformation twin nucleation mechanism, different from the previously reported observations in the high-Mn steels. Since this is also true for the observed high Σ-value boundaries in this study, our observation demonstrates the practical importance of taking grain boundary characters into account to understand the deformation twin nucleation mechanism besides well-known factors such as stacking fault energy and grain size.

36 MATERIALS SCIENCE↗

Effects of Fe atoms on hardening of a nickel matrix: Nanoindentation experiments and atom-scale numerical modeling

Significant hardening effect due to Fe concentrations in Ni-based alloys with face-centered-cubic structure has been studied by using a combined experimental and atomistic-based computational approach via nanoindentation tests. The obtained experimental load–displacement data for the [0 0 1] crystal orientation reached a qualitative good agreement with molecular dynamics simulations results, leading to strong evidence that the main strengthening factors are associated to sluggish dislocation diffusion, reduced defect sizes and the nucleation of tetrahedral stacking faults. Here, interstitial type prismatic dislocation loops mainly formed by $\frac{1}{6}$$\langle$1 1 2$\rangle$ Shockley dislocations are nucleated during the loading process, where their interaction leads to the formation of pyramidal shaped stacking fault which are mainly created by $\frac{1}{3}$$\langle$1 0 0$\rangle$ Hirth dislocations lines. Observing both types of defects coexisting in the same plastic deformation zone by both approaches. Reported mechanical data, measured experimentally and interpreted numerically, are also in accordance with microstructural SEM and TEM investigations.

36 MATERIALS SCIENCE↗