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At least 127 records · Page 7

Advanced Characterization of Fuel-cladding Chemical Interaction between U-10Zr Fuel and HT9 Cladding Tested in Fast Flux Test Facility

Fuel cladding chemical interaction (FCCI) can greatly accelerate the cladding failure. However, due to the limited space in a fuel cladding assembly, it is historically challenging to gain an mechanistical understanding of the formation mechanism of FCCI and its influence on fuel and cladding performance. With the imminent need to qualify U-10Zr based metallic fuel cladded by HT-9 for advanced reactors demonstration project, it is of vital importance to use advanced characterization method to study FCCI in a unprecedent detailed manner and gain better mechanism understanding of FCCI. Mechanistic Fuel Failure (MFF) series of prototypic fuel elements irradiated in FFTF [1, 2] provides the best samples to study FCCI since the MFF-series assemblies had an axial fuel height the same as proposed length by industry partners. Jason et al. [3] has performed preliminary post-irradiation examination on a MFF fuel pin sample, which was extracted from the HT9 cladded U-10at.%Zr MFF-3 pin MFF-3 pin (#193045) at an axial location of X/L = 0.98. This sample has a peak burnup of 5.7 at.% and peak inner cladding temperature (PICT) of around 615 °C during in-core testing. Scanning electron microscope examination has identified visible FCCI region on more than half of the HT9 circumference [3]. The most striking feature are grain boundary attacking by apparently lanthanides (Lns) rich phase. However, SEM cannot provide accurate assessment of phase and concentration of grain boundary phases and prevented a better understanding of the formation mechanism of such attach. This study, by pairing transmission electron microscope (TEM) characterization and atom probe tomography (APT) techniques with in-situ micro-tensile testing in scanning electron microscope (SEM), aims at gaining in-depth understanding on the formed FCCI region. The identified FCCI region roughly consists of multilayers as illustrated in Figure 1 (c). The main findings are: (1) layer-B shows observable lanthanides (Lns) infiltration along grain boundaries and mechanical softening due to FCCI- and irradiation-induced microstructural and microchemistry changes, particularly the recovery of martensitic lath structure and dissolution of pre-existing M23C6 together with the formation of coarsened Laves phases, (Fe, Cr)2(Mo, W); (2) layer-C is Fe depleted but Lns significantly enriched, becoming very brittle; (3) layer-D is mainly composed of UFe2 and Lns; (4) three FCCI-induced intermetallic U-Fe-Zr phases, ? (Fe0.5Zr0.32U0.18), e (Fe0.3Zr0.4U0.3), ? (Fe0.06Zr0.23U0.71), were identified near layer-E; (5) the ? (Fe0.5Zr0.32U0.18) phase was characterized to be a face centered cubic (FCC) crystal structure. These results will help to better understanding the governing mechanism of FCCI and facilitating the development of theoretical model for assessing the performance of metallic fuel and cladding integrity.

36 MATERIALS SCIENCE↗

New electron microscope employs new video display technique

Video display system for a scanning electron microscope provides slow scanning rates, a self-generated color gradient technique, and allows leisurely viewing of several hours. It also enables the viewing of areas where selected energy regions contribute relatively few electrons, and the changing of specimen position and magnification without adjustments.

Brookshier, W. K.↗

Isothermal oxidation of zirconium using steam

Oxidation of zirconium and its alloys under any atmosphere is generally characterised by a protective and non-protective stage. During the protective stage, the kinetics of oxidation are quasi-parabolic, while the oxide scale formed on the surface of the metal is black, compact, and protective in nature. For the non-protective stage, the oxidation rate becomes linear, while the protective oxide film turns into a deteriorated white scale. Breakaway is known as the transition point from protective to non-protective stage. The actual mechanism leading to breakaway of zirconium is still a matter of controversy, however some of the most common factors affecting breakaway are the following: - Impurities on the metal (Carbon, Oxygen, Nitrogen); - Oxidizing atmosphere (Presence of H{sub 2}O (g) or N{sub 2} (g)); - Sample preparation (Chemically etched or polished); - Temperature (LWR, LOCA). This research investigates the effect of temperature on 'breakaway' when zirconium is oxidized isothermally in steam for 60 min at 800 and 900 deg. C using thermogravimetric and optical microscopic imaging techniques. 1. Steam isothermal oxidations were performed on zirconium at 800 and 900 deg. C using a Thermogravimetric Analyzer (TGA). 2. Log-log plots of mass gain vs time were obtained from thermogravimetric results to calculate the reaction orders (n) and reaction rate constants (K) during oxidation. 3. Results of the kinetics of reaction were correlated with optical microscopic images form Light Microscope (LM) and Scanning Electron Microscope (SEM). Breakaway depends very strongly on temperature. At 800 deg. C, the weight gain followed a cubic-parabolic behaviour with evidence of a protective oxide film. On the other hand, oxidation at 900 deg. C showed signs of breakaway since the oxide film was cracked and oxidation rate was almost linear throughout the reaction.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

An Automated Scanning Transmission Electron Microscope Guided by Sparse Data Analytics

Abstract Artificial intelligence (AI) promises to reshape scientific inquiry and enable breakthrough discoveries in areas such as energy storage, quantum computing, and biomedicine. Scanning transmission electron microscopy (STEM), a cornerstone of the study of chemical and materials systems, stands to benefit greatly from AI-driven automation. However, present barriers to low-level instrument control, as well as generalizable and interpretable feature detection, make truly automated microscopy impractical. Here, we discuss the design of a closed-loop instrument control platform guided by emerging sparse data analytics. We hypothesize that a centralized controller, informed by machine learning combining limited a priori knowledge and task-based discrimination, could drive on-the-fly experimental decision-making. This platform may unlock practical, automated analysis of a variety of material features, enabling new high-throughput and statistical studies.

47 OTHER INSTRUMENTATION↗

Metallurgical characterization of the fracture of several high strength aluminum alloys

The fracture behavior for structural aluminum alloys (2024, 6061, 7075, and 7178) was examined in selected heat treatments. The investigation included tensile, shear, and precracked notch-bend specimens fractured at ambient temperature under monotonic loading. Specimens were obtained from thin sheets and thick plates and were tested in longitudinal and transverse orientations at different strain rates. Microstructures of alloys were examined using the optical microscope and the scanning electron microscope with associated energy dispersive X ray chemical analysis. Several different types of second phase particles, some not reported by other investigators, were identified in the alloys. Fracture morphology was related to microstructural variables, test variables, and type of commercial product. Specimen orientation examined in the present investigation had little effect on fracture morphology. Test strain rate changes resulted in some change in shear fracture morphology, but not in fracture morphology of tensile specimens.

Bhandarkar, M. D.↗

Densities of 5-15 micron interplanetary dust particles

We have measured the densities of about 100 5-15 micron stratospheric IDPs. Great care was taken to minimize selection bias in the sample population. Masses were determined using an absolute x-ray analysis technique with a transmission electron microscope, and volumes were found using scanning electron microscope imagery. Unmelted chondritic particles have densities between 0.5 and 6.0 g/cc. Roughly half of the particles have densities below 2 g/cc, indicating appreciable porosity, but porosities greater than about 70 percent are rare. IDPs with densities above 3.5 g/cc usually contain large sulfide grains. We find no evidence of bimodality in the unmelted particle density distribution. Chondritic spherules (melted particles) have densities near 3.5 g/cc, consistent with previous results for deep sea spherules.

Love, S. G.↗

Densities of stratospheric micrometeorites

We have measured the densities of roughly 150 5- to 15-microns interplanetary dust particles (IDPs) harvested in the stratosphere. Care was taken to minimize selection bias in the sample population. Masses were determined using an absolute X-ray analysis technique with a transmission electron microscope, and volumes were found using scanning electron microscope imagery. Unmelted chondritic particles have densities ranging between 0.3 and 6.2 g/cu cm, averaging 2.0 g/cu cm. The low medium densities indicates appreciable porosity, suggesting primitive, uncompacted parent bodies for these particles. Porosities greater than 70% are rare. IDPs with densities above 3.5 g/cu cm usually contain large sulfide grains. We find no evidence of bimodality in the unmelted particle density distribution. Chondritic spherules (melted particles) have densities near 3.4 g/cu cm, consistent with previous results for stony spheurles culled from deep-sea sediments.

Love, Stanley G.↗

Microbiological Characterization of the International Space Station Water Processor Assembly External Filter Assembly S/N 01

The External Filter Assembly (EFA) S/N 01 is a mesh screen filter with a pore size of approximately 300 micron that was installed in the International Space Station (ISS) Water Processor Assembly (WPA) between the Waste Tank and the Mostly Liquid Separator (MLS) on February 11, 2010 to protect clearances in the MLS solenoid valve SV_1121_3. A removal & replacement of the EFA Filter was performed on March 22, 2011 in response to increasing pressure across the Waste Tank solenoid valve SV_1121_1 and the EFA Filter. The EFA Filter was returned on ULF6 and received in the Boeing Huntsville Laboratory on June 13, 2011. The filter was aseptically removed from the housing, and the residual water was collected for enumeration and identification of bacteria and fungi. Swab samples of the filter surface were also collected for microbiological enumeration and identification. Sample analyses were performed by Boeing Huntsville Laboratory and NASA Johnson Space Center Microbiology for comparison. Photographic documentation of the EFA filter was performed using a stereo microscope and environmental scanning electron microscope. This paper characterizes the amount and types of microorganisms on the filter surface and in the residual water from the filter housing following 1 year of utilization in the ISS WPA.

Weir, Natalee↗

Origin of organic matter and organic pores in the overmature Ordovician-Silurian Wufeng-Longmaxi Shale of the Sichuan Basin, China

Organic matter (OM)-hosted pores play important roles in controlling the porosity and gas content of gas shales. However, the control of organic pore development and preservation remains poorly understood, partly because of the inability to distinguish OM types under the scanning electron microscope (SEM). In this study, seven over-mature Wufeng-Longmaxi Shale samples (equivalent vitrinite reflectance 1.93%–3.07%) were investigated with organic petrography and scanning electron microscope to study the origin of OM and development of organic pores in this black shale succession. Correlative light and electron microscopy was employed to examine pore development in individual macerals. Organic petrographic observations show that OM in these over-mature black shales is dominated by pyrobitumen and graptolites (> 90 vol.% of total OM based on point counting). Pyrobitumen mainly occurs as matrix bitumen in the fine-grained matrix, and also as a mixture with clay minerals and fossil cavity infillings. Vitrinite-like particles are minor constituents of OM in the Wufeng-Longmaxi Shale, and their average reflectance, reflectance distribution, and morphology suggest that they may be derived from graptolite fragments lacking diagnostic features and acritarchs. OM type critically controls the development of organic pores. Here, organic pores primarily occur in pyrobitumen, whereas other macerals are mostly non-porous when examined under the SEM. Results of this study provided important insights into OM thermal evolution and organic pore development in source-rock reservoirs, calling for a critical appraisal of OM in black shales with organic petrography in addition to SEM.

03 NATURAL GAS↗

Nanoscale Mineralogy and Composition of Experimental Regolith Agglutinates Produced under Asteroidal Impact Conditions

On the Moon, the energetics of smaller impactors and the physical/chemical characteristics of the granular regolith target combine to form a key product of lunar space weathering: chemically reduced shock melts containing optically-active nanophase Fe metal grains (npFe0) [1]. In addition to forming the optically dark glassy matrix phase in lunar agglutinitic soil particles [1], these shock melts are becoming increasingly recognized for their contribution to optically active patina coatings on a wide range of exposed rock and grain surfaces in the lunar regolith [2]. In applying the lessons of lunar space weathering to asteroids, the potential similarities and differences in regolith-hosted shock melts on the Moon compared to those on asteroids has become a topic of increasing interest [3,4]. In a series of impact experiments performed at velocities applicable to the asteroid belt [5], Horz et al. [6] and See and Horz [7] have previously shown that repeated impacts into a gabbroic regolith analog target can produce melt-welded grain aggregates morphologically very similar to lunar agglutinates [6,7]. Although these agglutinate-like particles were extensively analyzed by electron microprobe and scanning electron microscopy (SEM) as part of the original study [7], a microstructural and compositional comparison of these aggregates to lunar soil agglutinates at sub-micron scales has yet to be made. To close this gap, we characterized a representative set of these aggregates using a JEOL 7600 field-emission scanning electron microscope (FE-SEM), and JEOL 2500SE field-emission scanning transmission electron microscope (FE-STEM) both optimized for energy dispersive X-ray spectroscopy (EDX) compositional spectrum imaging at respective analytical spatial resolutions of 0.5 to 1 micron, and 2 to 4 nm.

Christoffersen, Roy↗

Particulate impacts on the UHCRE cosmic ray experiment teflon covers: The ESA programme

The optical scanning equipment at the University of Kent Unit for Space Science consists of a 102.5 by 42.5 cm computer controlled motorized stage which has a reproduction accuracy of 30 microns over the entire area. This is used with an optical microscope connected to two charge coupled device video cameras which can be used to obtain stereo color images of any features found. A coordinate system can be defined on each cover by means of two or more reference marks which allow a feature to be located using different equipment such as a scanning electron microscope, providing two known marks can be found. By using back illumination, penetrating features can be found automatically, and their sizes, circularity, and positions logged for later revisiting either on the optical system or using a scanning electron microscope.

Mcdonnell, J. A. M.↗

An efficient instance segmentation approach for studying fission gas bubbles in irradiated metallic nuclear fuel

Abstract Gaseous fission products from nuclear fission reactions tend to form fission gas bubbles of various shapes and sizes inside nuclear fuel. The behavior of fission gas bubbles dictates nuclear fuel performances, such as fission gas release, grain growth, swelling, and fuel cladding mechanical interaction. Although mechanical understanding of the overall evolution behavior of fission gas bubbles is well known, lacking the quantitative data and high-level correlation between burnup/temperature and microstructure evolution blocks the development of predictive models and reduces the possibility of accelerating the qualification for new fuel forms. Historical characterization of fission gas bubbles in irradiated nuclear fuel relied on a simple threshold method working on low-resolution optical microscopy images. Advanced characterization of fission gas bubbles using scanning electron microscopic images reveals unprecedented details and extensive morphological data, which strains the effectiveness of conventional methods. This paper proposes a hybrid framework, based on digital image processing and deep learning models, to efficiently detect and classify fission gas bubbles from scanning electron microscopic images. The developed bubble annotation tool used a multitask deep learning network that integrates U-Net and ResNet to accomplish instance-level bubble segmentation. With limited annotated data, the model achieves a recall ratio of more than 90%, a leap forward compared to the threshold method. The model has the capability to identify fission gas bubbles with and without lanthanides to better understand the movement of lanthanide fission products and fuel cladding chemical interaction. Lastly, the deep learning model is versatile and applicable to the micro-structure segmentation of similar materials.

36 MATERIALS SCIENCE↗

Synchronized voltage contrast display analysis system

An apparatus and method for comparing internal voltage potentials of first and second operating electronic components such as large scale integrated circuits (LSI's) in which voltage differentials are visually identified via an appropriate display means are described. More particularly, in a first embodiment of the invention a first and second scanning electron microscope (SEM) are configured to scan a first and second operating electronic component respectively. The scan pattern of the second SEM is synchronized to that of the first SEM so that both simultaneously scan corresponding portions of the two operating electronic components. Video signals from each SEM corresponding to secondary electron signals generated as a result of a primary electron beam intersecting each operating electronic component in accordance with a predetermined scan pattern are provided to a video mixer and color encoder.

Johnston, M. F.↗

Enabling the Acquisition of Electron Beam-Induced Current (EBIC) Images in Conventional SEM and STEM Instruments

Electron beam-induced current (EBIC) imaging is a well-established scanning electron microscope (SEM) technique used to analyze the behavior of microelectronic devices including solar cells. Recently, the application of EBIC imaging in an aberration-corrected scanning transmission electron microscope (STEM) has been demonstrated and offers great potential for the in situ study of electronic materials, correlating charge transport properties to atomic structural and elemental information. Here, this work presents two ways to implement EBIC imaging in conventional SEM and STEM systems: one relying on the instrument's inherent scanning and imaging electronics and the other involving third-party systems usually available in electron microscopes. The implementation of lock-in EBIC in systems equipped with a fast beam blanker is also described. In addition, this work shows and discusses the different mechanisms at play in EBIC imaging and their dependence on beam energy, sample impedance, and electrical measurement configuration, providing researchers with the basic information needed to apply the technique to their research.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Transport Simulations on Scanning Transmission Electron Microscope Images of Nanoporous Shale

Digital rock physics is an often-mentioned approach to better understand and model transport processes occurring in tight nanoporous media including the organic and inorganic matrix of shale. Workflows integrating nanometer-scale image data and pore-scale simulations are relatively undeveloped, however. In this paper, a workflow is demonstrated progressing from sample acquisition and preparation, to image acquisition by Scanning Transmission Electron Microscopy (STEM) tomography, to volumetric reconstruction to pore-space discretization to numerical simulation of pore-scale transport. Key aspects of the workflow include (i) STEM tomography in high angle annular dark field (HAADF) mode to image three-dimensional pore networks in µm-sized samples with nanometer resolution and (ii) lattice Boltzmann method (LBM) simulations to describe gas flow in slip, transitional, and Knudsen diffusion regimes. It is shown that STEM tomography with nanoscale resolution yields excellent representation of the size and connectivity of organic nanopore networks. In turn, pore-scale simulation on such networks contributes to understanding of transport and storage properties of nanoporous shale. Interestingly, flow occurs primarily along pore networks with pore dimensions on the order of tens of nanometers. Smaller pores do not form percolating pathways in the sample volume imaged. Apparent gas permeability in the range of 10−19 to 10−16 m2 is computed.

42 ENGINEERING↗

Investigation of the relations between neat resin and advanced composite mechanical properties. Volume 1: Results

A detailed evaluation of one untoughened epoxy baseline resin and three toughened epoxy resin systems was performed. The Hercules 3502, 2220-1, and 2220-3, and Ciba-Geigy Fibredux 914 resin systems were supplied in the uncured state by NASA-Langley and cast into thin flat specimens and round dogbone specimens. Tensile and torsional shear measurements were performed at three temperatures and two moisture conditions. Coefficients of thermal expansion and moisture expansion were also measured. Extensive scanning electron microscopic examination of fracture surfaces was performed, to permit the correlation of observed failure modes with the environmental conditions under which the various specimens were tested. A micromechanics analysis was used to predict the unidirectional composite response under the various test conditions, using the neat resin experimental results as the required input data. Mechanical and physical test results, the scanning electron microscope observations, and the analytical predictions were then correlated.

Zimmerman, R. S.↗

Investigation of the relations between resin and advanced composite mechanical properties. Volume 2: Appendices

One untoughened epoxy baseline resin and three toughened epoxy resin systems were evaluated. The Hercules 3502, 2220-1, and 2220-3, and Ciba-Geigy Fibredux 914 resin systems were supplied in the uncured state by NASA-Langley and cast into thin flat specimens and round dogbone specimens. Tensile and torsional shear measurements were performed at three temperatures and two moisture conditions. Coefficients of thermal expansion and moisture expansion were also measured. Extensive scanning electron microscopic examination of fracture surfaces was performed to permit the correlation of observed failure modes with the environmental conditions under which the various specimens were tested. A micromechanics analysis was used to predict the unidirectional composite response under the various test conditions, incorporating the neat resin experimental results as the required input data. The mechanical and physical test results, the scanning electron microscope observations, and the analytical predictions were then correlated.

Zimmerman, R. S.↗