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At least 901 records · Page 50

Electron tomography of unirradiated and irradiated nuclear graphite

Graphite is the moderator material of several Generation IV nuclear reactor concepts, as well as the British Advanced Gas-cooled Reactors (AGR). Porosity can heavily influence the material properties, mechanical irradiation response, and neutron induced shrinkage or swelling of nuclear-grade graphite. Due to the sub-micron size of several types of pores found in graphite, only a high-resolution imaging technique such as electron tomography are capable of visualizing these features in three dimensions. In this research, we used electron tomography to characterize as-received and neutron irradiated samples of IG-110 nuclear-grade graphite to show for the first time the 3D structure of both native and irradiation-induced nano-cracks. This technique also reveals unique characteristics of graphite such as the structure that surrounds pores and could be used to inform molecular dynamic simulations of irradiated graphite and experimental techniques such as gas-absorption. This work also shows the utility of this technique for the study of other nuclear porous carbon-based materials.

36 MATERIALS SCIENCE↗

Dislocation Loops in Proton Irradiated Uranium-Nitrogen-Oxygen System

Here in this study, we investigated the dislocation loop types formed in the proton-irradiated uranium-nitrogen-oxygen (U-N-O) system, which involves uranium mononitride (UN), uranium sesquinitride (a-U2N3), and uranium dioxide (UO2) phases. The dislocation loop formation is examined using specimens irradiated at 400°C and 710°C. Based on the detailed transmission-based electron microscopy characterization with i) the morphology-based on-zone and ii) the invisibility-criterion based two-beam condition imaging techniques, only a single type of dislocation loop in each phase is found: a/2?110?, a/2?111?, or a/3?111? dislocation loops in UN, a-U2N3, and UO2 phases, respectively. Molecular statics calculations for the formation energy of perfect and faulted dislocation loops in UN phases indicate a critical loop size of ~ 6 nm, above which perfect loops are energetically favorable. This could explain the absence of faulted loops in the experimental observation of the irradiated UN phase at two temperatures. This work will enhance the understanding of irradiation induced microstructural evolution for uranium nitrides as advanced nuclear fuels for the next-generation nuclear reactors.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Correlative electron and ion beam analysis of the electrochemical performances of LiV 3 O 8 cathode films as a function of microstructures

Degradation mechanisms in LiV 3 O 8 cathode films (~500 nm) with different initial microstructures i.e., globular nanocrystals in amorphous matrix and needle-like nanocrystals, synthesized by annealing the cathodes at 150 °C and 300 °C for 6 h are studied by Transmission Electron Microscopy (TEM) and Auger Electron Spectroscopy (AES). In addition, a unique in-situ combination of TEM and Secondary Ion Mass Spectrometry (SIMS) imaging techniques, namely Parallel Ion and Electron beam Spectrometry (PIES) is carried out to measure the 3D distribution of V and Li with nanoscale resolution. These characterization studies focus on correlating the pre- and post-cycling microstructure to observed electrochemical performance. The LiV 3 O 8 cathode film with needle-like nanocrystals (300 °C) shows a higher initial capacity but it degrades rapidly compared to the film with globular nanocrystals embedded in amorphous matrix (150 °C). We observed that LiV 3 O 8 films with needle-like nanocrystals are more susceptible to cathode decohesion and vanadium dissolution than the films with globular nanocrystals embedded in amorphous matrix, explaining the differences in their electrochemical performance. The findings from this study have relevance to the development of thin film electrode microstructures for high capacity and cyclic stability.

25 ENERGY STORAGE↗

Cyclic plastic deformation behaviour of a directionally solidified nickel base superalloy at 850 °C: Damage micromechanisms

Highlights: • Isothermal LCF life of CM 247 DS is reduced using R = 0 instead of R = −1. • Reduction in LCF life is significant at lower values of Δε/2. • Reduction in fatigue life is attributed to the development of sustained mean stress. • Sustained mean stress prevents the slip transfer from γ-channels to γ′-precipitates. • Sustained mean stress promotes dislocation network formation and looping. - Abstract: Dislocation based deformation micromechanisms during low cycle fatigue deformation of nickel base superalloy CM 247 DS LC at 850 °C was investigated by conducting fatigue tests employing constant strain amplitudes for strain ratio (R) values of 0, −1 and carrying out extensive SEM and TEM examinations. Cyclic life of the alloy reduces for all fatigue tests conducted employing R = 0 in comparison with R = −1 owing to sustained mean stress developed during fatigue at R = 0. TEM examinations confirmed that sustained mean stress developed during low strain amplitude fatigue test (Δε/2 = 0.5%) using R = 0 condition prevented slip transfer from γ-channels to γ′-precipitates and resulted in the formation of dislocation substructures such as networks, nodes etc. and also promoted dislocation looping around γ′-precipitates. Lower fatigue life at R = 0 is mainly attributed to the development of these types of substructures, which promotes strain localization in both intra as well intergranular regions. Whereas, in specimen fatigue tested (Δε/2 = 0.5%) using R = −1 condition, shearing of γ′-precipitates by APB coupled dislocation and formation of stacking faults were observed. The formation and nature of stacking faults were analysed using weak beam imaging technique. Stacking fault formed during fatigue tests using R = −1 condition matured to micro-twins when Δε/2 value was increased to 0.8%. The mechanism of formation of these microtwins is discussed in detail. SEM based microstructural and fractographic examinations revealed that mean stress induced creep effect resulted in intergranular crack initiation and grain boundary cavitation during fatigue tests under R = 0 condition and therefore verified the facts revealed in TEM studies.

36 MATERIALS SCIENCE↗

High aspect ratio anisotropic silicon etching for x-ray phase contrast imaging grating fabrication

Lab based x-ray phase contrast imaging (XPCI) systems have historically focused on medical applications, but there is growing interest in material science applications for non-destructive analysis of low density materials. Extending this imaging technique to higher density materials or larger samples requires higher aspect ratio gratings, to allow the use of a higher energy x-ray source. Here, we demonstrate the use of anisotropic silicon (Si) etching in potassium hydroxide (KOH), to achieve extremely high aspect ratio gratings. This method has been shown to be effective in fabricating deep, uniform gratings by taking advantage of the etch selectivity of differing crystalline planes of silicon. Our work has introduced a method for determining Si crystalline plane directions, specific to (110) Si wafers, enabling high alignment accuracy of the etch mask to these crystalline planes.

36 MATERIALS SCIENCE↗

Transverse beam profile measurement system for the Duke storage ring

The transverse beam emittance is a crucial parameter determining the brightness of an electron storage ring based synchrotron radiation source. The beam emittance is typically determined using the transverse electron beam size and the beta function at a particular location. For a low energy storage ring, the direct imaging method using visible/UV light has many advantages, including being simple, straightforward, and cost-effective. The resolution of such a system can be quite adequate for measuring electron beams with a reasonably large transverse beam size. In this work, we present the development of a new transverse beam profile measurement system for the Duke storage ring. This new system has been characterized to allow absolute measurements of the electron beam size while achieving better system resolution than previously thought possible for the direct imaging technique. The preliminary measurement results show that this system is capable of measuring the horizontal beam size over a wide range of the electron beam energies and currents. The system has also been demonstrated as a useful tool to study the intra-beam scattering related emittance increase in the storage ring.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Charge collection efficiency of diamond and silicon sensors irradiated with alpha particles

To evaluate the viability of using semiconductors as sensor materials in a detector for the Associated Particle Imaging technique, the radiation hardness of silicon and diamond diodes to alpha particles has been assessed. Here, the detector lifetimes for both silicon and diamond sensors were measured under the prolonged exposure to alpha particles emitted by an 241 Am source. The silicon detector was exposed to alpha radiation for approximately two months, reaching an accumulated fluence of ~ 1.5 x 10 12 α cm –2 . Additionally, by using a high purity single-crystal diamond with coplanar electrodes operating with full charge collection, the diamond detector response was measured over approximately ten months reaching an accumulated fluence of over 6 x 10 12 α cm –2 cm.

47 OTHER INSTRUMENTATION↗

Shielding development for the spallation neutron source VENUS instrument

VENUS is a neutron imaging instrument that will use a broad range of neutron wavelengths, from epithermal to cold energies, and will include enhanced contrast mechanisms. It will offer novel energy-selective imaging techniques directly connecting complex engineering materials and systems’ structures, properties, and functions to reveal practical and fundamental answers about their real-world performance. Here, the instrument will be built at SNS beamline 10, facing the decoupled poisoned hydrogen moderator. The driving cost for the instrument is the beamline and instrument cave shielding. Final analyses were performed to evaluate the thickness and composition of shielding materials for the instrument cave and beamline to meet radiation safety criteria for the instrument to start up in 2024 after completing the SNS proton power upgrade.

43 PARTICLE ACCELERATORS↗

YOLO2U-Net: Detection-guided 3D instance segmentation for microscopy

Microscopy imaging techniques are instrumental for characterization and analysis of biological structures. As these techniques typically render 3D visualization of cells by stacking 2D projections, issues such as out-of-plane excitation and low resolution in the z-axis may pose challenges (even for human experts) to detect individual cells in 3D volumes as these non-overlapping cells may appear as overlapping. In this paper a comprehensive method for accurate 3D instance segmentation of cells in the brain tissue is introduced. The proposed method combines the 2D YOLO detection method with a multi-view fusion algorithm to construct a 3D localization of the cells. Next, the 3D bounding boxes along with the data volume are input to a 3D U-Net network that is designed to segment the primary cell in each 3D bounding box, and in turn, to carry out instance segmentation of cells in the entire volume. The promising performance of the proposed method is shown in comparison with current deep learning-based 3D instance segmentation methods.

3D instance segmentation↗

Estimating diffusion coefficients of shale oil, gas, and condensate with nano-confinement effect

Molecular diffusion plays an important role in oil and gas migration in tight shale formations. However, there are insufficient reference data in the literature to specify the diffusion coefficients within porous media. This study aims at calculating diffusion coefficients of shale gas, shale condensate, and shale oil at reservoir conditions with CO 2 injection for EOR/EGR. The large nano-confinement effects including large gas-oil capillary pressure and critical property shifts could alter the phase behaviors. This paper estimates the diffusivities of shale fluids in nanometer-scale shale rock from two perspectives: 1) examining the shift of diffusivity caused by nanopore confinement effects from phase change (phase composition and fluid property) perspective, and 2) calculating the effective diffusion coefficient in porous media by incorporating rock intrinsic properties (porosity and tortuosity factor). The tortuosity is obtained by using tortuosity-porosity relations as well as the measured tortuosity of shale from 3D imaging techniques. The results indicated that nano-confinement effects could affect the diffusion coefficient through altering the phase properties, such as phase compositions and densities. Compared to bulk phase diffusivity, the effective diffusion coefficient in porous shale rock is reduced by 10 2 to 10 4 times as porosity decreases from 0.1 to 0.03.

04 OIL SHALES AND TAR SANDS↗

In-situ 4D visualization and analysis of temperature-driven creep in an oil shale propped fracture

Here, the proppant embedment due to creep in shales is a known issue affecting the useable lifetime of wells in unconventional oil and gas recovery. One of the factors influencing creep is the presence of organics, whose properties can be very sensitive to temperature. In this work we investigated for the first time the role of temperature-induced creep increase in proppant embedment in an organics-rich Green River oil shale sample via in-situ synchrotron X-ray micro-computed tomography. We observed that temperatures as low as 75 °C already induce fast creep, with a fracture aperture closing rate of 13 μm/h and a loss of fracture conductivity rate of 8.7%/h, due only to proppant embedment, in the measured interval at the first heating stage. Local displacement data analysis provided evidence for markedly plastic deformation around the proppant-shale contacts, in contrast with the brittle proppant embedment observed on more cemented and less organics-rich shales at room temperature. The results highlight how the problem of temperature-dependent mechanical behavior might be more important than previously thought, in shales with a high content in organics, and that in-situ micro-imaging techniques can play a key role in understanding the underlying mechanisms, contributing to solve creep-related problems associated with hydraulic fracturing in complex scenarios.

02 PETROLEUM↗

Coupled aging effects in nanofiber-reinforced siloxane foams

Here, this study investigates the combined effects of ionizing radiation and thermal treatments on the aging of siloxane foams containing small amounts of carbon nanofibers. Our siloxane foams were exposed to accelerated aging conditions for more than two years, resulting in very low dose rates. In addition, foams were aged under compressive load to evaluate the strength of the porous microstructure. Samples were characterized by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance spectroscopy (NMR), Mössbauer, mass spectroscopy, electron paramagnetic resonance spectroscopy (EPR), solvent swelling, imaging techniques, uniaxial compressive load testing and tear testing. No significant changes in thermal stability or chemistry of the accelerated aged foam were observed, although gas evolution was detected. Changes in crystallization levels at low temperatures, microstructure, and mechanical properties were observed for foams with and without carbon nanofibers. In particular, foams aged under compressive load showed irreversible deformation of the porous microstructure. This study demonstrates that aging effects were enhanced when thermal and radiolysis were coupled together and that the addition of carbon nanofibers did not improve aging effects.

36 MATERIALS SCIENCE↗

Impact of krypton irradiation on a single crystal tungsten: Multi-modal X-ray imaging study

Understanding microstructural and strain evolutions induced by noble gas production in the nuclear fuel matrix or plasma-facing materials is crucial for designing next generation nuclear reactors, as they are responsible for volumetric swelling and catastrophic failure. In this paper we describe a multimodal approach combining synchrotron-based nanoscale X-ray imaging techniques with atomic-scale electron microscopy techniques for mapping chemical composition, morphology and lattice distortion in a single crystal W induced by Kr irradiation. We report that Kr-irradiated single crystal W undergoes surface deformation, forming Kr containing cavities. Furthermore, positive strain fields are observed in Kr-irradiated regions, which lead to compression of underlying W matrix.

36 MATERIALS SCIENCE↗

Non-destructive spatial analysis of phosphatase activity and total protein distribution in the rhizosphere using a root blotting method

Phosphorus (P) is an essential macronutrient for plant growth, but bioavailable P in soils is often limited due to immobilization resulting from pH and geochemical interactions. Understanding the dynamics of P in soils and elucidating the mechanisms by which plants access P from their environment are critical to evaluating productivity, particularly in nutrient poor environments. Phosphorus from organic matter can act as a major source of P for organisms in soil systems. Phosphatases, enzymes that liberate inorganic P from organic sources, are produced by both plants and microbes and are considered one of the most active classes of enzymes in soil. In this work we developed a root blotting method to spatially image phosphatase activity in the rhizosphere. Proteins from the rhizosphere are transferred to a nitrocellulose membrane while retaining their enzymatic activity and two-dimensional spatial distribution. Subsequent application of a fluorogenic phosphatase indicator, DDAO phosphate, enables visualization of the distribution of phosphatase activity in the sample. The proteins can then be fixed to the membrane and treated with a SYPRO® Ruby gel stain, a fluorescent total protein stain, allowing for visualization of total protein distribution. Taken together, the images of phosphatase activity and total protein localization can be mapped back to the root architecture and provide insight into factors affecting the spatial distribution of enzymatic activity and protein accumulation in the rhizosphere. Notably, this method can be applied to plants growing in rhizoboxes containing soil or soilless growth mixtures (e.g., sand or various potting mixes) and, because of the non-destructive nature of this approach, be performed over time to track changes. We anticipate that this fluorescent indicator imaging technique on root blots can be used in diverse plant-microbe-soil systems to better understand the role of phosphatases in P acquisition and soil P cycling.

59 BASIC BIOLOGICAL SCIENCES↗

Effect of simvastatin on vascular tone in porcine coronary artery: Potential role of the mitochondria

Statins induce acute vasorelaxation which may contribute to the overall benefits of statins in the treatment of cardiovascular disease. The mechanism underlying this relaxation is unknown. As statins have been shown to alter mitochondrial function, in this study we investigated the role of mitochondria in the relaxation to simvastatin. Relaxation of porcine coronary artery segments by statins was measured using isolated tissue baths. Mitochondrial activity was determined by measuring changes in rhodamine 123 fluorescence. Changes in intracellular calcium levels were determined in freshly isolated smooth muscle cells with Fluo-4 using standard epifluorescent imaging techniques. Simvastatin, but not pravastatin, produced a slow relaxation of the coronary artery, which was independent of the endothelium. The relaxation was attenuated by the mitochondrial complex I inhibitor rotenone (10 μM) and the complex III inhibitor myxothiazol (10 μM), or a combination of the two. The complex III inhibitor antimycin A (10 μM) produced a similar time-dependent relaxation of the porcine coronary artery, which was attenuated by rotenone. Changes in rhodamine 123 fluorescence showed that simvastatin (10 μM) depolarized the membrane potential of mitochondria in both isolated mitochondria and intact blood vessels. Simvastatin and antimycin A both inhibited calcium-induced contractions in isolated blood vessels and calcium influx in smooth muscle cells and this inhibition was prevented by rotenone. In conclusion, simvastatin produces an endothelium-independent relaxation of the porcine coronary artery which is dependent, in part, upon effects on the mitochondria. The effects on the mitochondria may lead to a reduction in calcium influx and hence relaxation of the blood vessel. - Highlights: • Simvastatin produces a relaxation of the porcine coronary artery. • This relaxation is inhibited by mitochondrial complex inhibitors. • Simvastatin alters mitochondrial membrane potential in intact blood vessels. • Simvastatin inhibits calcium influx in smooth muscle cells, prevented by a mitochondrial inhibitor. • Simvastatin-induced relaxations are dependent upon mitochondrial activity.

60 APPLIED LIFE SCIENCES↗

Exploring chemistry with single-molecule and -particle fluorescence microscopy

The evolution of single-molecule and -particle fluorescence microscopy imaging techniques for the investigation of chemical reactions yielded achievements at all fronts, from synthetic organic chemistry to materials science. The removal of ensemble averaging effects uncovers unique, otherwise hidden reaction intermediates, reactivity, and kinetics. Thus, new insights can be obtained even for well-explored chemical reactions and processes. The aim of this article is to serve as a guide and a source of inspiration for scientists who wish to develop single-molecule and -particle fluorescence microscopy to answer questions in chemistry. Here, we describe the current status of technical accomplishments in the field and point out technical and conceptual obstacles for overcoming in the near future, with focus on improvement of bench-scale synthetic reactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗