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At least 361 records · Page 20

A comparison of the irradiation creep behavior of several graphites - 18583

Graphite creep strain data from the irradiation creep capsule Advanced Graphite Creep-1 (AGC-1) are reported. This capsule was the first (prototype) of a series of five or six capsules planned as part of the AGC experiment, which was designed to fully characterize the effects of neutron irradiation and the radiation creep behavior of current nuclear graphite. The creep strain data and analysis are reported for the six graphite grades incorporated in the capsule. The AGC-1 capsule was irradiated in the Advanced Test Reactor at Idaho National Laboratory (INL) at approximately 700 deg. C and to a peak dose of 7 dpa (displacements per atom). The specimen s final dose, temperature, and stress conditions have been reported by INL and were used during this analysis. The derived creep coefficients (K) were calculated for each grade and were found to compare well to literature data for the creep coefficient, even under the wide range of AGC-1 specimen temperatures. Comparisons were made between AGC-1 data and historical grade data for creep coefficients. (authors)

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Macroscopic Properties of Restacked, Redox-Liquid Exfoliated Graphite and Graphite Mimics Produced in Bulk Quantities

The excellent properties exhibited by monolayer graphene have spurred the development of exfoliation techniques using bulk graphite to produce large quantities of pristine monolayer sheets. Development of simple chemistry to exfoliate and intercalate graphite and graphite mimics in large quantities is required for numerous applications. To determine the macroscopic behavior of restacked, exfoliated bulk materials, a systematic approach is presented using a simple, redox-liquid sonication process along to obtain large quantities of 2D and 3D hexagonally layered graphite, molybdenum disulfi de, and boron nitride, which are subsequently characterized to observe chemical and structural changes. For MoS 2 sonicated with the antioxidant sodium bisulfi te, results from Raman spectroscopy, X-ray diffraction, and electron microscopy indicate the presence of distorted phases from different polymorphs, and apparent nanotube structures in the bulk, restacked powder. Furthermore, using thermograviemtric analysis, the antioxidant enhances the resistance to oxidative degradation of MoS 2 , upon thermal treatment up to 900 C. The addition of the ionic antioxidant decreased dispersion stability in non-polar solvent, suggesting decreased compatibility with non-polar systems. Using simple chemical methods, the ability to generate tailored multidimensional layered materials with unique macroscopic properties is critical for numerous applications, including electrical devices, reinforced polymer composites, lithium ion capacitors, and chemical sensing.

Srivastava, Vikram K↗

Multimodal quantification of degradation pathways during extreme fast charging of lithium-ion batteries

Enabling fast charging of Li-ion batteries will be a key step towards realizing the technology's full potential in electric vehicles. Currently, fast charging is limited by a variety of processes that reduce cell capacity upon extended cycling. Using a multimodal approach combining incremental capacity analysis (dQ/dV), high energy X-ray diffraction (HEXRD), and mass spectrometry titration (MST), we identify specific degradation mechanisms—including Li plating, dead Li x C 6 formation, Li 2 C 2 formation, solid carbonate solid-electrolyte interphase (SEI) deposition, and loss of positive electrode active material (LAM PE )—that occur during extended fast charge cycling. We find that Li plating is the major source of capacity loss in cells cycled at 6C, while non-carbonate SEI species deposition on the graphite anode is the main source of capacity loss when cycled at 4C. We also study local degradative phenomena by examining specific ~1–5 cm 2 regions of the cells using HEXRD and MST. Here, we find that plated Li is often collocated with dead Li x C 6 , Li 2 C 2 , and solid carbonate SEI species, and these additional species cumulatively account for ~20% of the capacity lost during 6C cycling. Finally, in a cell with an anomalously high amount of LAM PE (quantified via dQ/dV), we find that regions of cathode degradation were accompanied by non-carbonate SEI products on the adjacent region of the anode. We postulate that this phenomenon arises due to crosstalk between the electrodes, wherein soluble electrolyte oxidation products formed at the delithiated cathode migrate to the graphite anode and are ultimately deposited on the graphite surface. This work demonstrates the utility of combining multiple characterization techniques to reveal a more holistic understanding of degradative phenomena that occur across multiple length scales during fast charge.

25 ENERGY STORAGE↗

Fully Fluorinated Local High Concentration Electrolytes Enabling High Energy Density Si Anodes

To develop fluorinated localized high concentration electrolytes as a novel approach for constructing a functional SEI on Si based anodes. The technological approach combines the SEI modification strategies of fluorinated carbonate solvents and local high concentration electrolytes. The resulting synergy of anion and fluorinated solvent decomposition will form a mechanically robust, fluorinated SEI that enables extended cycling with high capacity retention. The electrolytes will enable demonstration of silicon-graphite anodes with high Si content, paired with NMC811 cathodes. Characterization will focus on galvanostatic cycling to evaluate electrochemical performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Fracture modes in off-axis fiber composites

Criteria were developed for identifying, characterizing, and quantifying fracture modes in high-modulus graphite-fiber/resin unidirectional composites subjected to off-axis tensile loading. Procedures are described which use sensitivity analyses and off-axis data to determine the uniaxial strength of fiber composites. It was found that off-axis composites fail by three fracture modes which produce unique fracture surface characteristics. The stress that dominates each fracture mode and the load angle range of its dominance can be identified. Linear composite mechanics is adequate to describe quantitatively the mechanical behavior of off-axis composites. The uniaxial strengths predicted from off-axis data are comparable to these measured in uniaxial tests.

Sinclair, J. H.↗

Fracture modes in off-axis fiber composites

Criteria have been developed for identifying, characterizing, and quantifying fracture modes in high-modulus graphite-fiber/resin unidirectional composites subjected to off-axis tensile loading. Procedures are described which use sensitivity analyses and off-axis data to determine the uniaxial strength of fiber composites. It was found that off-axis composites fail by three fracture modes which produce unique fracture surface characteristics. The stress that dominates each fracture mode and the load angle range of its dominance can be identified. Linear composite mechanics is adequate to describe quantitatively the mechanical behavior of off-axis composites. The uniaxial strengths predicted from off-axis data are comparable to those measured in uniaxial tests.

Sinclair, J. H.↗

Compression failure of composite laminates

This presentation attempts to characterize the compressive behavior of Hercules AS-1/3501-6 graphite-epoxy composite. The effect of varying specimen geometry on test results is examined. The transition region is determined between buckling and compressive failure. Failure modes are defined and analytical models to describe these modes are presented.

Pipes, R. B.↗

Space radiation effects on the dimensional stability of a toughened epoxy graphite composite

The effects of a simulated space radiation environment on the dimensional stability of an elastomer-toughened epoxy-graphite composite were determined. The response of the material was characterized following exposure to radiation doses equivalent to geosynchronous orbit lifetimes ranging from 6 months to 30 years. The results show that radiation interacts with the epoxy matrix to embrittle the composite, beginning at relatively low total doses (10 to the 7th power rads). The embrittlement results in thermal expansion changes and significant laminate microcracking during thermal cycling. These property changes could limit the service life of this material in some spacecraft applications.

Sykes, G. F.↗

Characterization of zirconium carbides using electron microscopy, optical anisotropy, Auger depth profiles, X-ray diffraction, and electron density calculated by charge flipping method

Samples with five different zirconium carbide compositions (C/Zr molar ratio=0.84, 0.89, 0.95, 1.05, and 1.17) have been fabricated and studied using a variety of experimental techniques. Each sample was zone refined to ensure that the end product was polycrystalline with a grain size of 10-100 {mu}m. It was found that the lattice parameter was largest for the x=0.89 composition and smallest for the x=1.17 total C/Zr composition, but was not linear; this nonlinearity is possibly explained using electron densities calculated using charge flipping technique. Among the five samples, the unit cell of the ZrC{sub 0.89} sample showed the highest electron density, corresponding to the highest carbon incorporation and the largest lattice parameter. The ZrC{sub 0.84} sample showed the lowest carbon incorporation, resulting in a larger number of carbon vacancies and resultant strain. Samples with larger carbon ratios (x=0.95, 1.05, and 1.17) showed a slight decrease in lattice parameter, due to a decrease in electron density. Optical anisotropy measurements suggest that these three samples contained significant amounts of a graphitic carbon phase, not bonded to the Zr atoms. - Graphical abstract: Characterization of zirconium carbides using electron microscopy, optical anisotropy, Auger depth profiles, X-ray diffraction, and electron density calculated by the charge flipping method. Highlights: Black-Right-Pointing-Pointer The lattice parameter variation: ZrC{sub 0.89}>ZrC{sub 0.84}>ZrC{sub 0.95}>ZrC{sub 1.05}>ZrC{sub 1.17}. Black-Right-Pointing-Pointer Surface oxygen with no correlation to the lattice parameter variation. Black-Right-Pointing-Pointer ZrC{sub 0.89} had highest electron densities correspond to highest carbon incorporation. Black-Right-Pointing-Pointer Second highest lattice parameter in ZrC{sub 0.84} due to strain. Black-Right-Pointing-Pointer Unit cell electron density order: ZrC{sub 0.95}>ZrC{sub 1.05}>ZrC{sub 1.17}.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

AGC-1 Pre-Irradiation Data Report Status

The Next Generation Nuclear Plant (NGNP) Graphite R&D program is currently measuring irradiated material property changes in several grades of nuclear graphite for predicting their behavior and operating performance within the core of new Very High Temperature Reactor (VHTR) designs. The Advanced Graphite Creep (AGC) experiment consisting of six irradiation capsules will generate this irradiated graphite performance data for NGNP reactor operating conditions. All samples in the experiment will be fully characterized before irradiation, irradiated in the Advanced Test Reactor (ATR), and then re-examined to determine the irradiation induced changes to key materials properties in the different graphite grades. The information generated during the AGC experiment will be utilized for NRC licensing of NGNP reactor designs, shared with international collaborators in the Generation IV Information Forum (GIF), and eventually utilized in ASME design code for graphite nuclear applications. This status report will describe the process the NGNP Graphite R&D program has developed to record the AGC1 pre-irradiation examination data.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

PT AND PT/NI "NEEDLE" ELETROCATALYSTS ON CARBON NANOTUBES WITH HIGH ACTIVITY FOR THE ORR

Platinum and platinum/nickel alloy electrocatalysts supported on graphitized (gCNT) or nitrogen doped carbon nanotubes (nCNT) are prepared and characterized. Pt deposition onto carbon nanotubes results in Pt 'needle' formations that are 3.5 nm in diameter and {approx}100 nm in length. Subsequent Ni deposition and heat treatment results in PtNi 'needles' with an increased diameter. All Pt and Pt/Ni materials were tested as electrocatalysts for the oxygen reduction reaction (ORR). The Pt and Pt/Ni catalysts showed excellent performance for the ORR, with the heat treated PtNi/gCNT (1.06 mA/cm{sup 2}) and PtNi/nCNT (0.664 mA/cm{sup 2}) showing the highest activity.

36 MATERIALS SCIENCE↗

Aqueous Li-ion battery enabled by halogen conversion–intercalation chemistry in graphite

The use of 'water-in-salt' electrolytes has considerably expanded the electrochemical window of aqueous lithium-ion batteries to 3 to 4 volts, making it possible to couple high-voltage cathodes with low-potential graphite anodes. However, the limited lithium intercalation capacities (less than 200 milliampere-hours per gram) of typical transition-metal-oxide cathodes preclude higher energy densities. Partial or exclusive anionic redox reactions may achieve higher capacity, but at the expense of reversibility. Here we report a halogen conversion-intercalation chemistry in graphite that produces composite electrodes with a capacity of 243 milliampere-hours per gram (for the total weight of the electrode) at an average potential of 4.2 volts versus Li/Li + . Experimental characterization and modelling attribute this high specific capacity to a densely packed stage-I graphite intercalation compound, C 3.5 [Br 0.5 Cl 0.5 ], which can form reversibly in water-in-bisalt electrolyte. By coupling this cathode with a passivated graphite anode, we create a 4-volt-class aqueous Li-ion full cell with an energy density of 460 watt-hours per kilogram of total composite electrode and about 100 per cent Coulombic efficiency. Here, this anion conversion-intercalation mechanism combines the high energy densities of the conversion reactions, the excellent reversibility of the intercalation mechanism and the improved safety of aqueous batteries.

25 ENERGY STORAGE↗

Hydrothermal Synthesis of Platinum-Group-Metal-Free Catalysts: Structural Elucidation and Oxygen Reduction Catalysis

In this paper, a hydrothermal approach to generate a platinum-group-metal-free (PGM-free) Fe-N-C catalyst for the oxygen reduction reaction (ORR) is introduced. The process involves partial carbonization by hydrothermal means followed by thermal treatment to obtain the final catalysts. Detailed X-ray scattering analysis of the glucose-imidazole catalysts (termed as GLU-IMID-C catalysts), obtained for the first time with the use of CarbonXS GUI program, reveals the presence of face-centered cubic (FCC) iron nanoparticles embedded in partially graphitic carbon in all catalyst variations. We also report the physical characterization of these catalysts by using X-ray photoelectron spectroscopy, Brunauer-Emmett-Teller surface area analysis, and transmission electron microscopy. The electrocatalytic behavior of the catalysts towards oxygen reduction is studied separately in acidic and alkaline electrolytes by rotating ring disk electrode measurements. The catalysts exhibit high ORR activity in acidic (0.5 M H 2 SO 4 ) and alkaline (0.1 M KOH) electrolytes. Lastly, a precursor structure-performance relationship of these catalysts and their performance trends in both electrolytes has been discussed in this work.

36 MATERIALS SCIENCE↗

Ultrasonic characterization of multilayered thick composite plates

Guided wave propagation in a periodically laminated plate is considered when each lamina is transversely isotropic with its symmetry axis lying in the plane of the graphite-epoxy plate. The dispersion behavior of propagation modes influences the dynamic response and can be used to ultrasonically characterize the mechanical properties of the laminated plate. It is assumed that fibers are oriented at 90 deg to one another in adjacent layers and all the laminae are of equal thickness. Results obtained are in good agreement with exact solutions of previous studies.

Karunasena, W.↗

Characterization of Organic Materials in the Xenolithic Clasts in Sharps (H3.4) Meteorite Using Microraman Spectroscopy

Graphitization of carbon is an irreversible process which alters the structure of graphitic materials in response to the increase in metamorphic grade (temperature and/or pressure). Carbonaceous materials offer a reliable geothermometer as their Raman spectra change systematically with increasing metamorphic grade [1-3]. In this study, we identified carbonaceous materials in the xenolithic clasts in Sharps and interpreted their metamorphic history by revealing the structural organization (order) of the polyaromatic organic phases using μ-Raman spectroscopy.

Chan, Q. H. S.↗

Fullerene-like defects in high-temperature neutron-irradiated nuclear graphite

Irradiation-induced defect evolution in graphite is particularly important for its application in graphite-moderated nuclear reactors. The evolution of defects directly influences macroscopically observed property changes in irradiated nuclear graphite which, in turn, can govern the lifetime of graphite components. This article reports novel defect structures and the irradiation response of microstructural features occurring in high-temperature irradiated nuclear graphite IG-110. High resolution transmission electron microscopy (HRTEM) was used to characterize specimens neutron-irradiated at a high temperature (≥ 800°C) at doses of 1.73 and 3.56 atomic displacements per atom (dpa). Concentric shelled and fullerene-like defects were found to result in swelling along the c-axis and contraction along the a/b-axis of crystallites. Furthermore, such defects are shown to occur within, and partially fill, Mrozowski cracks prior to turnaround dose. In addition, in situ TEM under similar irradiation conditions was used to capture the real-time dynamic evolution of defects, providing unambiguous analysis of the evolution of the graphite structures during irradiation. Here, the results suggest the mainstream theory for radiation damage in nuclear graphite (which assumes additional basal plane formation as the sole reason) to be an incorrect interpretation of defect evolution contributing to irradiation-induced property changes at higher temperatures.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗