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At least 1,027 records · Page 57
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Correlating microstructure and mechanical properties of harvested high dose Zorita light water reactor internals

Here, in this study, microstructural studies and micro-mechanical testing of an ex-plant material harvested from the decommissioned pressurized water reactor (PWR) is carried out. Irradiated 304 stainless steel (SS) components were harvested by the Electric Power Research Institute, U.S. Nuclear Regulatory Commission, and members of the José Cabrera Nuclear Power Station (Zorita) in Spain. The bi-crystalline micro-tensile specimens, atom probe tomography (APT) tips, and transmission electron microscopy (TEM) lamellae were fabricated from the baffle plate materials irradiated to 0.05, 15 and 50 dpa to elucidate microstructural, microchemical, and local mechanical properties changes as a function of dose. TEM and APT studies reveal radiation induced Ni, Cr, and Si rich precipitates in the 15 dpa sample that become smaller and partially redissolve into the matrix of the 50 dpa sample (decreasing size and number density). Dislocation loop and cavity number density and size were quantified as a function of dose as well as swelling. Intergranular Ni and Si enrichments with concomitant Fe and Cr depletion were observed in the 15 dpa sample and were more pronounced in the 50 dpa sample. Micro-tensile testing performed in the scanning electron microscope (SEM) at room temperature and 300 °C shows that the material's local yield strength and ultimate tensile strength decreases with increased dose and elevated test temperature and provides further insights via localized strain mapping. Current and previous mechanical data was compared with calculated values using the dispersed barrier hardening model with inputs of dislocation loops, precipitates, and cavities from microstructural characterization.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Microstructural evolution of rapidly solidified hypoeutectic Al 10Cu alloy during non-isothermal annealing transients induced by nano-second laser pulses

The evolution of characteristic nonequilibrium features presenting in morphologically distinct regions of rapid solidification (RS) microstructures in a hypoeutectic Al—10Cu (atomic %) in response to non-isothermal annealing transients has been studied by transmission electron microscopy (TEM). The capabilities of the Movie-Mode Dynamic TEM (MM-DTEM) instrument were used to expose select regions of the RS microstructure to sequences of rapid heating and cooling transients induced by nanosecond laser pulses while permitting in-situ observation. Partial melting, microstructural scale coarsening, morphological changes of the nonequilibrium features in the multi-phase RS microstructure, and solid-state phase transformation were observed. Heterogeneous nucleation of nanoscale θ-Al 2 Cu phase involved metastable supersaturated α-Al and the θ'-Al 2 Cu phases, establishing different sets of orientation relationships for the stable θ-Al 2 Cu and α-Al phases. Replacement of banded morphology grains that formed under conditions driven farthest from equilibrium by an equiaxed nanocrystalline structure comprised of α-Al phase, the primary solidification product, and an intergranular network of Al 2 Cu crystals has been attributed to local remelting. Here the experimental approach explored, permitted discovery of mechanistic details of location-specific transformation pathways activated in the multi-phase RS microstructure of hypoeutectic Al—Cu during subsequent nonisothermal transients.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Probing microstructure and phase evolution of α-MoO 3 nanobelts for sodium-ion batteries by in situ transmission electron microscopy

The fundamental electrochemical reaction mechanisms and the phase transformation pathways of layer-structured α-MoO 3 nanobelt during the sodiation/desodiation process to date remain largely unknown. In this study, to observe the real-time sodiation/desodiaton behaviors of α-MoO 3 during electrochemical cycling, we construct a MoO 3 anode sodium-ion battery inside a transmission electron microscope (TEM). Utilizing in situ TEM and electron diffraction pattern (EDP) observation, α-MoO 3 nanobelts are found to undergo a unique multi-step phase transformation. Upon the first sodiation, α-MoO 3 nanobelts initially form amorphous Na x MoO3 phase and are subsequently sodiated into intermediate phase of crystalline NaMoO 2 , finally resulting in the crystallized Mo nanograins embedded within the Na 2 O matrix. During the first desodiation process, Mo nanograins are firstly re-oxidized into intermediate phase NaMoO 2 that is further transformed into amorphous Na 2 MoO 3 , resulting in an irreversible phase transformation. Upon subsequent sodiation/desodiation cycles, however, a stable and reversible phase transformation between crystalline Mo and amorphous Na2MoO 3 phases has been revealed. In conclusion, our work provides an in-deepth understanding of the phase transformation pathways of α-MoO 3 nanobelts upon electrochemical sodiation/desodiation processes, with the hope of assistance in designing sodium-ion batteries with enhanced performance.

36 MATERIALS SCIENCE↗
DOE OSTI2021

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↗
DOE OSTI2013

Identification of Fragile Microscopic Structures during Mineral Transformations in Wet Supercritical CO2

In this study we examine the nature of highly fragile reaction products that form in low water content super critical carbon dioxide (scCO2) using a combination of scanning electron microscopy/focus ion beam (SEM/FIB), confocal Raman spectroscopy, helium ion microscopy (HeIM), and transmission electron microscopy (TEM). HeIM images show these precipitates to be fragile rosettes that can readily decompose even under slight heating from an electron beam. Using the TEM revealed details on the interfacial structure between the newly formed surface precipitates and the underlying initial solid phases. The detailed microscopic analysis revealed that the growth of the precipitates either followed a tip growth mechanism with precipitates forming directly on the forsterite surface if the initial solid was non-porous (natural forsterite) or growth from the surface of the precipitates where fluid was conducted through the porous (nanoforsterite) agglomerates to the growth center. The mechanism of formation of the hydrated/hydroxylated magnesium carbonate compound (HHMC) phases offers insight into the possible mechanisms of carbonate mineral formation from scCO2 solutions which has recently received a great deal of attention as the result of the potential for CO2 to act as an atmospheric greenhouse gas and impact overall global warming. The techniques used here to examine these fragile structures an also be used to examine a wide range of fragile material surfaces. SEM and FIB technologies have now been brought together in a single instrument, which represents a powerful combination for the studies in biological, geological and materials science.

carbon↗
DOE OSTI2016

High cycle fatigue in the transmission electron microscope

One of the most common causes of structural failure in metals is fatigue induced by cyclic loading. Historically, microstructure-level analysis of fatigue cracks has primarily been performed post mortem. However, such investigations do not directly reveal the internal structural processes at work near micro- and nanoscale fatigue cracks and thus do not provide direct evidence of active microstructural mechanisms. In this paper, the tension–tension fatigue behavior of nanocrystalline Cu was monitored in real time at the nanoscale by utilizing a new capability for quantitative cyclic mechanical loading performed in situ in a transmission electron microscope (TEM). Controllable loads were applied at frequencies from one to several hundred hertz, enabling accumulations of 10 6 cycles within 1 h. The nanometer-scale spatial resolution of the TEM allows quantitative fatigue crack growth studies at very slow crack growth rates, measured here at ~10 –12 m·cycle –1 . This represents an incipient threshold regime that is well below the tensile yield stress and near the minimum conditions for fatigue crack growth. Evidence of localized deformation and grain growth within 150 nm of the crack tip was observed by both standard imaging and precession electron diffraction orientation mapping. Finally, these observations begin to reveal with unprecedented detail the local microstructural processes that govern damage accumulation, crack nucleation, and crack propagation during fatigue loading in nanocrystalline Cu.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Unraveling Kinetically-Driven Mechanisms of Gold Nanocrystal Shape Transformations Using Graphene Liquid Cell Electron Microscopy

Mechanisms of kinetically driven nanocrystal shape transformations were elucidated by monitoring single particle etching of gold nanocrystals using in situ graphene liquid cell transmission electron microscopy (TEM). By systematically changing the chemical potential of the oxidative etching and then quantifying the facets of the nanocrystals, nonequilibrium processes of atom removal could be deduced. Etching at sufficiently high oxidation potentials, both cube and rhombic dodecahedra (RDD)-shaped gold nanocrystals transform into kinetically stable tetrahexahedra (THH)-shaped particles. Whereas {100}-faceted cubes adopt an { hko }-faceted THH intermediate where h/k depends on chemical potential, {110}-faceted RDD adopt a {210}-faceted THH intermediate regardless of driving force. For cube reactions, Monte Carlo simulations show that removing 6-coordinate edge atoms immediately reveals 7-coordinate interior atoms. The rate at which these 6- and 7-coordinate atoms are etched is sensitive to the chemical potential, resulting in different THH facet structures with varying driving force. Conversely, when RDD are etched to THH, removal of 6-coordinate edge atoms reveals 6-coordinate interior atoms. Thus, changing the driving force for oxidation does not change the probability of edge atom versus interior atom removal, leading to a negligible effect on the kinetically stabilized intermediate shape. These fundamental insights, facilitated by single-particle liquid-phase TEM imaging, provide important atomic-scale mechanistic details regarding the role of kinetics and chemical driving force in dictating shape transformations at the nanometer length scale.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2019

Interpreting Electrochemical and Chemical Sodiation Mechanisms and Kinetics in Tin Antimony Battery Anodes Using in Situ Transmission Electron Microscopy and Computational Methods

Intermetallic compounds such as SnSb are promising anode materials for sodium ion batteries; however, their nanoscale sodiation mechanisms are not well understood. Here, we used a combination of in situ transmission electron microscopy (TEM), first-principles electronic structure calculations, computational thermodynamic modeling, and phase-field simulations to reveal the sodiation mechanisms and to quantify microstructural effects contributing to the underlying reaction kinetics in SnSb electrodes. During in situ sodiation experiments, the nanocrystalline SnSb thin films underwent a rapid amorphous phase transformation upon sodiation, as determined by in situ TEM and electron diffraction experiments. The Na + diffusion coefficients were measured with and without an external electrical bias, and the data showed that an applied potential increased Na + diffusion by an order of magnitude compared to solid-state diffusion. Furthermore, there was a distinct decrease in sodium diffusion upon the formation of the amorphous phase that resulted from a change in the local structure and grain boundaries. To further understand how the Na + transport mechanism correlated with the changes observed in the SnSb thin films, phase-field modeling was used, which considered sodium diffusion within the grain boundaries together with their evolution and stress–strain state. As a result, these findings enhance our understanding of sodiation mechanisms within intermetallic anode materials for sodium ion battery applications.

25 ENERGY STORAGE↗
DOE OSTI2022

Unveiling the Degradation Mechanism of High-Temperature Superconductor Bi 2 Sr 2 CaCu 2 O 8+δ in Water-Bearing Environments

We report the physical properties of copper oxide high-temperature superconductors have been studied extensively, such as its band structure, and doping effects of Bi 2 Sr 2 CaCu 2 O 8+δ (Bi-2212). However, some chemical-related properties of these superconductors are rarely reported, such as their stability in air. Here, we report experiments combined with ab initio calculations that address the effects of water in contact with Bi-2212. The evolution of Bi-2212 flake with exposure to water for different time intervals were tested and characterized by optical microscopy (OM), atomic force microscopy (AFM), Raman spectroscopy, transmission electron microscopy (TEM) and electrical measurements. The thickness of Bi-2212 flakes is gradually decreased in water, and some thin flakes can be completely etched away after a few days. The stability of Bi-2212 in other solvents is also evaluated, including alcohol, acetone, HCl and KOH. The morphology of Bi-2212 flakes is relatively stable in organic solvents. However, the flakes are etched relatively quick in HCl and KOH, especially in acidic environment. Our results imply that hydrogen ion is primarily responsible for the deterioration of their properties. Both TEM and calculation results demonstrate that the atoms in Bi-O plane is relatively stable when compared to the inner atoms in Sr-O, Ca-O and Cu-O planes. This work contributes towards understanding the chemical stability of Bi-2212 superconducting device in environmental medium, which is important for both fundamental studies and practical applications of copper oxide high-temperature superconductors.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2021

Discovery of Gold Nanoparticles in Marcellus Shale

A high density of gold (Au) nanoparticles has been observed on the surfaces of the coexisting opal nanospheres in kerogen-bearing shales from the Marcellus Formation. Our analyses of the Au nanoparticles and associated minerals indicate that this represents a new formation type of colloidal gold nanoparticles. Additionally, the opal nanospheres are a new kind of natural opal-A that is characteristic of the mesoporous texture formed through oil-in-water emulsion processes. High-resolution transmission electron microscopy (TEM) combined with energy-dispersive X-ray spectroscopy analysis directly reveals spherical gold nanoparticles and gold nanorods associated with mesoporous opal nanospheres. Our newly found textures indicate that opal nanospheres may have facilitated the co-precipitation of pure gold nanoparticles in organic-bearing, reduced environments. Furthermore, our TEM observations provide distinct images of the initial phase of colloidal gold and silica, which may contribute to the formation of Au deposits involving "invisible" gold, secondary supergene enrichments, or high-grade gold accumulations. Finally, the discovery of Au nanoparticles in hydrocarbon-rich shale formations such as Marcellus (which contains 0.6-4.1 wt % gold/opal) suggests a potential for co-production of both gas/oil and gold-two valuable commodities.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

In Situ Transmission Electron Microscopy of Oxide Shell-Induced Pore Formation in (De)lithiated Silicon Nanowires

Silicon (Si) nanowires with a silicon oxide (SiOx) shell were observed in situ during lithiation and delithiation using transmission electron microscopy (TEM). The oxide shell constrains the volume expansion, which prevents full lithiation of the nanowire and retention of a crystalline Si core. Pores form in the amorphized silicon upon the first delithiation. We propose that this is caused by a high barrier to vacancy migration in the SiOx shell, which prevents vacancies formed during delithiation from transporting through the shell to the nanowire surface. These in situ studies demonstrate the importance of the direct observation of structural changes that occur in a material during cycling upon the addition of a coating.

Adkins, Emily R.↗
DOE OSTI2026

Structural and Mechanical Analysis of Individual Mineralized Collagen Fibrils Using In Situ Transmission Electron Microscopy

Bone serves as an example of nature’s architectured material with its characteristic blend of strength and toughness, all at a lightweight design. Given the hierarchical nature of these materials, it is essential to understand the governing mechanisms and organization of their constituents across length scales for bioinspired structural design. Despite recent advances in transmission electron microscopy (TEM) that have allowed us to witness the hierarchical arrangement of bone at micro-down to the nanoscale, we are still missing the details about the structural organization and mechanical properties of the main building blocks of bone─mineralized collagen fibrils (MCFs). Here, we present a method to extract individual MCFs from nature’s model material, mineralized turkey leg tendon, using a dropcasting procedure. By isolating the MCFs onto TEM supporting grids, we visualized the arrangement of organic and mineral phases within individual MCFs at the nanoscale. Using a four-dimensional scanning transmission electron microscopy (4D-STEM) approach, the orientation of individual mineral crystals within the MCFs was examined. Furthermore, we conducted in situ tensile experiments, revealing exceptional tensile strains of at least 8%, demonstrating the intricate relationship between structural organization and the mechanical behavior of MCFs. These insights into the ultrastructure of mineralized tissue building blocks, as well as the proposed sample-extraction method compatible with in situ mechanical testing, provide a strong basis for research into nature-inspired material design.

4D-STEM↗
DOE OSTI2018

In situ microscopy across scales for the characterization of crystal growth mechanisms: The case of europium oxalate

A better understanding of how production pathway affects the final product is required in order to produce targeted syntheses, but many of the classical ex situ techniques used for studying nanoparticle growth are unsuitable as stand-alone methods for identifying and characterizing growth mechanisms. Using a combination of high resolution transmission electron microscopy (TEM), cryogenic TEM, and fluid cell scanning electron microscopy, we monitor europium oxalate growth over the range of nanometers to tens of micrometers and identify potential crystal growth pathways. We also compare the effects of stirring during crystal growth as an example of how changing processing conditions changes growth mechanisms.

in situ SEM, Cryo TEM, lanthanide, crystal growth↗
DOE OSTI2019

Brownmillerite Phase Formation and Evolution in Epitaxial Strontium Ferrite Heterostructures

By controlling the synthesis and process conditions, we show that the oxygen vacancy channels (OVCs) of Brownmillerite-structured SrFeO2.5+? (0=??0.5) thin films can be oriented differently on the same LaAlO3(001) substrate due to either a bottom up or top down synthesis route. The brownmillerite structure formation and evolution processes yield distinctively different optical and electronic properties, owing to the difference in the oxygen content and OVC configuration in the resultant films. Moreover, we also show that in situ transmission electron microscopy (TEM) can induce oxygen loss and drive a phase transition from perovskite SrFeO3 to brownmillerite SrFeO2.5+? with mixed horizontally and vertically aligned OVCs. The dimensionality change during the TEM sample preparation makes the bottom up and top down model not applicable. Our results offer further insight into the phase stability and oxygen-diffusion mechanisms, which is important for the predictive synthesis of novel functional materials.

SrFeO3-d, compressive strain, oxygen vacancy chann↗
DOE OSTI2019

Ion exchange selectivity in clay is controlled by nanoscale chemical–mechanical coupling

Ion exchange in nanoporous clay-rich media plays an integral role in water, nutrient, and contaminant storage and transport. In montmorillonite (MMT), a common clay mineral in soils, sediments, and muds, the swelling and collapse of clay particles through the addition or removal of discrete molecular layers of water alters cation exchange selectivities in a poorly understood way. Here, we show that ion exchange is coupled to the dynamic delamination and restacking of clay layers, which creates a feedback between the hydration state of the exchanging cation and the composition of the clay interlayer. Particles with different hydration states are distinct phases with unique binding selectivities. Surprisingly, equilibrium achieved through thermal fluctuations in cation concentration and hydration state leads to the exchange of both ions and individual MMT layers between particles, a process we image directly with high-resolution transmission electron microscopy at cryogenic conditions (cryo-TEM). We introduce an exchange model that accounts for the binding selectivities of different phases, which is likely applicable to many charged colloidal or macromolecular systems in which the structural conformation is correlated with the activities of water and counterions within spatially confined compartments.

Whittaker, Michael L.↗
DOE OSTI2016

Creep deformation mechanism mapping in nickel base disk superalloys

We investigated the creep deformation mechanisms at intermediate temperature in ME3, a modern Ni-based disk superalloy, using diffraction contrast imaging. Both conventional transmission electron microscopy (TEM) and scanning TEM were utilised. Distinctly different deformation mechanisms become operative during creep at temperatures between 677-815 °C and at stresses ranging from 274 to 724 MPa. Both polycrystalline and single-crystal creep tests were conducted. The single-crystal tests provide new insight into grain orientation effects on creep response and deformation mechanisms. Creep at lower temperatures (≤760 °C) resulted in the thermally activated shearing modes such as microtwinning, stacking fault ribbons and isolated superlattice extrinsic stacking faults. In contrast, these faulting modes occurred much less frequently during creep at 815 °C under lower applied stresses. Instead, the principal deformation mode was dislocation climb bypass. In addition to the difference in creep behaviour and creep deformation mechanisms as a function of stress and temperature, it was also observed that microstructural evolution occurs during creep at 760 °C and above, where the secondary coarsened and the tertiary precipitates dissolved. Based on this work, a creep deformation mechanism map is proposed, emphasising the influence of stress and temperature on the underlying creep mechanisms.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Heat pulse propagation and anomalous electron heat transport measurements on the optimized stellarator W7-X

The optimized stellarator Wendelstein 7-X (W7-X) is designed to have an approximately quasi-isodynamic magnetic configuration with reduced neoclassical transport in comparison to a classical stellarator, and turbulent transport is expected to be a significant source of anomalous heat transport across the plasma minor radius. The ion temperature gradient driven mode and the trapped electron mode (TEM) are thought to be responsible for the ion-scale turbulence in W7-X plasmas with volume averaged pressure below 1%. In this work, the electron temperature gradient driven turbulence is shown to be a good candidate for the explanation of the observed electron heat flux, in the inner plasma region where the density gradient is weak (in the outer region, a relatively stronger density gradient would drive additional TEM turbulence). Further, the experimental electron heat transport measured during electron cyclotron resonant heating power and plasma density scans is compared to neoclassical predictions, and the stiffness in the electron heat transport measured during transient transport experiments is presented in three common magnetic configurations of W7-X. In low-(β) plasma discharges, the stiffness in the electron heat flux, quantified by the ratio of the heat pulse to power balance diffusivity, ${\chi }_{\mathrm{e}}^{\mathrm{H}\mathrm{P}}/{\chi }_{\mathrm{e}}^{\mathrm{P}\mathrm{B}}$, is measured to be less than 2, and trend downwards with increasing collisionality.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗