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At least 145 records · Page 8

Raman scattering of rhenium for secondary pressure calibration

With the increasing number of 100 s GPa experiments in the diamond anvil cell (DAC), improved accuracy in secondary pressure calibrations to extreme pressures is essential. The rhenium equation of state has been proposed as a pressure calibrant via x-ray diffraction with potentially broad applications as it is commonly used as a gasket material in DAC experiments. In this work, we conducted Raman spectroscopy experiments on rhenium in the DAC and report the pressure shift of the E2g mode, a refined high-pressure C44 and mode-Grüneisen parameter above 200 GPa. We used flat, beveled, and toroidal diamond anvils under quasi-hydrostatic and non-hydrostatic conditions. By measuring the E2g mode from the culet edge to the center, we analyzed pressure distribution based on culet type and distance from the anvil center. The shift in the E2g mode can be expressed as a function of pressure, and diamond edge measurements appear reliable across all anvil types. Comparing the center and edge pressures reveals anvil cupping, offering insights into predicting or preventing anvil failure during materials properties measurements at extreme conditions.

Diamond anvil cells↗

Experimental and computational studies on high-entropy carbide MoNbTaVWC 5 under high pressures

High-entropy carbide, MoNbTaVWC 5 , was synthesized from oxide precursors of the constituent metals, mixed with graphite powder in a microwave-generated hydrogen plasma at 26.66 kPa and 2100 °C. Ambient x-ray diffraction analysis confirms the full conversion of oxide precursors into a single-phase, face-centered cubic structure with a lattice parameter a = 4.3309 Å. Nanoindentation measured a hardness of 24.5 ± 1.3 GPa and an elastic modulus of 386 ± 22 GPa. The synthesized sample, mixed with a copper pressure marker, was studied by the radial x-ray diffraction technique with beryllium gasketing in a diamond anvil cell up to 70 GPa. The experimentally measured pressure–volume curve and shear strength were compared with theoretical predictions using the special quasi-random structure technique and density functional theory. MoNbTaVWC 5 achieved a 12% volume compression at 70 GPa and exhibited a high shear strength of 6.6 GPa. The present study demonstrates that the high-entropy carbide MoNbTaVWC 5 exhibits exceptional incompressibility and high strength under extreme conditions.

36 MATERIALS SCIENCE↗

Effect of pressure cycling and compression rate on the bcc-hcp transition in an FeNi alloy

Here, we investigate the body-centered cubic (bcc) to hexagonal close-packed (hcp) phase transition in Fe-10wt. %Ni alloy, combining pressure cycling and fast compression with time-resolved synchrotron x-ray diffraction in a dynamic diamond anvil cell. Three pressure cycles were conducted with compression rates ranging from 0.1 to nearly 10 3 GPa/s. During the first cycle with the slowest compression, the observed orientations in the bcc and hcp phases are consistent with the Burgers mechanism, followed by c-axis rotation of the hcp phase consistent with {$10$ $\bar{1}2$} twinning. During the following cycles with fast compression at 10 2 –10 3 GPa/s, the hcp phase exhibits negligible c-axis rotation with a nearly constant c/a ratio of ∼1.61 up to ∼30 GPa, indicating suppression of plastic deformation (especially, twinning) due to sample confinement from the gasket. Notably, the onset pressure of the transition decreases with additional pressure cycling and faster compression, which normally leads to over-pressurization. This suggests that defects or shear induced from the pressure cycling reduces the transition kinetics even during fast compression. These insights into the deformation and transition behavior in an FeNi alloy under multiple dynamic loading cycles can offer guidance for future design of advanced structural alloys and improve our understanding of planetary core processes.

FeNi alloy↗

Diamond anvil cell behavior up to 4 Mbar

The diamond anvil cell (DAC) is considered one of the dominant devices to generate ultrahigh static pressure. The development of the DAC technique has enabled researchers to explore rich high-pressure science in the multimegabar pressure range. Here, we investigated the behavior of the DAC up to 400 GPa, which is the accepted pressure limit of a conventional DAC. By using a submicrometer synchrotron X-ray beam, double cuppings of the beveled diamond anvils were observed experimentally. Furthermore, details of pressure loading, distribution, gasket-thickness variation, and diamond anvil deformation were studied to understand the generation of ultrahigh pressures, which may improve the conventional DAC techniques.

47 OTHER INSTRUMENTATION↗

High pressure studies using two-stage diamond micro-anvils grown by chemical vapor deposition

Ultra-high static pressures have been achieved in the laboratory using a two-stage micro-ball nanodiamond anvils as well as a two-stage micro-paired diamond anvils machined using a focused ion-beam system. The two-stage diamond anvils’ designs implemented thus far suffer from a limitation of one diamond anvil sliding past another anvil at extreme conditions. We describe a new method of fabricating two-stage diamond micro-anvils using a tungsten mask on a standard diamond anvil followed by microwave plasma chemical vapor deposition (CVD) homoepitaxial diamond growth. A prototype two stage diamond anvil with 300 μm culet and with a CVD diamond second stage of 50 μm in diameter was fabricated. We have carried out preliminary high pressure X-ray diffraction studies on a sample of rare-earth metal lutetium sample with a copper pressure standard to 86 GPa. Furthermore, the micro-anvil grown by CVD remained intact during indentation of gasket as well as on decompression from the highest pressure of 86 GPa.

36 MATERIALS SCIENCE↗

Tritium Effects on Aromatic Carbon–Loaded Polymers

By incorporating carbon nanotubes (CNTs) and graphene nanomaterials with aromatic sp2 carbon structures, we have specifically tuned filled ethylene propylene diene monomer elastomer (EPDM) seal and gasket composite materials for radiation resistance. Our results show that CNTs and graphene have an increased ability to stabilize the EPDM matrix compared to standard carbon black (CB) as a radiation-resistant filler. Here, graphene outperforms both CNT and CB fillers when considering surface damage under conditions where beta exposure is an issue. Both graphene and CNT fillers offer significantly reduced changes in glass transition temperature under prolonged exposure to tritium compared to CB-filled standards, with a 2.5-fold and almost 5-fold reduction, respectively. Thus, CNT- and graphene-filled O-ring materials could be designed that would maintain acceptable seals significantly longer than currently used composites.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Gamma ray measurements at OMEGA with the newest gas Cherenkov Detector “GCD-3”

Initial results from the newest Gas Cherenkov Detector (GCD-3) are reported demonstrating improved performance over previous GCD iterations. Increased shielding and lengthening of the Cherenkov photon optical path have resulted in a diminished precursor signal with increased temporal separation between the precursor and the primary DT Cherenkov signal. Design changes resulted in a measured GCD-3 sensitivity comparable to GCD-1 at identical 100 psia CO 2 operation. All metal gasket seals and pressure vessel certification to 400 psia operation allow for a GCD-3 lower Cherenkov threshold of 1.8 MeV using the fluorinated gas C 2 F 6 as compared to the 6.3 MeV lower limit of GCD-1 and GCD-2. Calibration data will be used to benchmark GEANT4 and ACCEPT detector models. Lastly, the GCD-3 acts as a prototype for the Super GCD being fielded at the National Ignition Facility (NIF) as part of the National Diagnostics Plan and will be installed at NIF in early 2016.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Finite-Element Simulations of Elastoplastic Flow during Compression of a Sample in a Diamond Anvil Cell under Extremely High Pressure: Effects of Geometry and Material Properties

Finite-element simulations are conducted to investigate large elastoplastic deformations of rhenium under multimegabar pressures in a diamond anvil cell (DAC), with an emphasis on the effects of geometric and material properties. The following published experimental phenomena are reproduced: (1) the pressure distribution at the sample or diamond contact surface and the final sample thickness at pressure up to 300 GPa; (2) the cupping (i.e., appearance of a cuplike concave shape of the contact diamond-sample surface) and double cupping phenomena at megabar pressures; (3) three stages at the curve of the maximum pressure versus compressive force; (4) stages of material flow with increasing load; (5) pressure drop at the periphery after cupping in that region; and (6) change in direction of material flow to the center without change in the sign of the pressure gradient. The effects of the culet geometry, bevel angle, sample thickness, and sample or gasket system are analyzed in detail. The obtained results improve the understanding of the material mechanical response under extreme pressures and large elastoplastic deformations and are beneficial for the optimum design of a DAC with the goal of reaching the high and record high pressures once or multiple times.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Topological states on fractal lattices

Here, we investigate the fate of topological states on fractal lattices. Focusing on a spinless chiral p-wave paired superconductor, we find that this model supports two qualitatively distinct phases when defined on a Sierpinski gasket.While the trivial phase is characterized by a self-similar spectrum with infinitely many gaps and extended eigenstates, the “topological” phase has a gapless spectrum and hosts chiral states propagating along edges of the graph. Besides employing theoretical probes such as the real-space Chern number, inverse participation ratio, and energy-level statistics in the presence of disorder, we develop a simple physical picture capturing the essential features of the model on the gasket. Extending this picture to other fractal lattices and topological states, we show that the p + ip state admits a gapped topological phase on the Sierpinski carpet and that a higher-order topological insulator placed on this lattice hosts gapless modes localized on corners.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Elastic properties of the W 0.75 R e 0.25 alloy at high pressure up to 183 GPa

The high pressure equation of state for the W 0.75 R e 0.25 alloy is experimentally determined up to 183 GPa with synchrotron angle-dispersive powder x-ray diffraction in the diamond-anvil cell and to ∼925 GPa with density-functional theory. W-Re alloys are used in many industrial high-temperature applications and as a confining gasket material in high-pressure diamond-anvil cell research. The inclusion of 25 wt. % Re achieves the highest performance in terms of strength and ductility while also maintaining the body-centered-cubic (bcc) crystal structure, yet to date there has been no investigation into its elastic behavior at high pressure. We present the experimentally and theoretically determined volumetric and elastic pressure response and systematically compare these results to other W-Re alloys, finding that the bulk modulus of W-Re alloys varies nonlinearly with Re content and W 0.75 Re 0.25 becomes less incompressible than W at 85 GPa. Published by the American Physical Society 2025

Alloys↗

Montel mirror based collimating analyzer system for high-pressure resonant inelastic X-ray scattering experiments

Resonant inelastic X-ray scattering (RIXS) is increasingly playing a significant role in studying highly correlated systems, especially since it was proven capable of measuring low-energy magnetic excitations. However, despite high expectations for experimental evidence of novel magnetic phases at high pressure, unequivocal low-energy spectral signatures remain obscured by extrinsic scattering from material surrounding the sample in a diamond anvil cell (DAC): pressure media, Be gasket and the diamond anvils themselves. A scattered X-ray collimation based medium-energy resolution (~100 meV) analyzer system for a RIXS spectrometer at the Ir L 3 -absorption edge has been designed and built to remediate these difficulties. Due to the confocal nature of the analyzer system, the majority of extrinsic scattering is rejected, yielding a clean low-energy excitation spectrum of an iridate Sr 2 IrO 4 sample in a DAC cell. Finally, the energy resolution of different configurations of the collimating and analyzing optics are discussed.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

STUDIES ON PIPELINE POLYETHYLENES IN HYDROGEN GAS ENVIRONMENTS USING IN-SITU AND EX-SITU CHARACTERIZATION METHODS

Polymeric materials are commonplace in the natural gas infrastructure as distribution pipes, coatings, seals, and gaskets. Under the auspices of the U.S. Department of Energy HyBlend program, one of the means to reduce greenhouse gas emissions is with replacing natural gas, either partially or completely, with hydrogen. This approach makes it imperative that we conduct near-term and long-term materials compatibility research in these relevant environments. Insights into the effects of hydrogen and hydrogen gas blends on polymer integrity can be gained through both ex-situ and in-situ analytical methods. Our work represented here highlights a study of the behavior of pipeline polyethylene (PE) materials, including HDPE (Dow 2490 and GDB50) and MDPE (Ineos and legacy Dupont Aldyl A), when exposed to hydrogen by means of in-situ X-ray scattering and ex-situ Raman spectroscopy techniques. Samples were tested in ex-situ hydrogen and argon gas environments and in-situ hydrogen environments to identify differences due to permeation and solubility of these gases. These methods complemented each other because Raman spectroscopy could capture permanent effects after materials were removed from gaseous environments, and in-situ X-ray scattering analysis collected real-time data to elucidate the impact of the gas environment on polymer microstructure. Data collected revealed that the aforementioned polymers did not show significant changes in crystallinity and microstructure under the exposure conditions tested. Our findings from these studies will help establish real-time effects caused by hydrogen gas transport through pipeline polyethylenes by way of its influence on polymer structure and chemistry, which is directly related to pipeline mechanical strength and longevity of service.

Hydrogen materials compatibility, Natural gas pipe↗

Effective Electrode Edge Protection for Proton Exchange Membrane Fuel Cell Drive Cycle Operation

Drive cycle (DC) tests employ rapid load cycling which will result in rapidly changing local operating conditions and consequently high non-uniform mechanical stress at the electrode perimeter. In order to better investigate the impact of electrode irregularities on the long-term behavior of the cell, it is necessary to exclude the edge effects of the membrane electrode assemblies (MEAs) as a failure mode. Therefore, an effective electrode edge protection technique using thin protective gaskets and a hot-pressing procedure was developed which dramatically prolonged lifetime. Open circuit voltage (OCV), air polarization curve, and hydrogen crossover limiting current density were monitored during the DC tests. For post-DC ex-situ analysis, an in-house developed pinhole detection apparatus was employed to analyze quantity, size, and location of the failure points of MEAs with and without edge protection. Non-protected MEAs typically developed tears at the electrode perimeter, while the longer-lasting protected MEAs exhibited seemingly random pinhole development.

30 DIRECT ENERGY CONVERSION↗

Ice-slurry production for solar-ice systems using supercooling with an in-stream crystallizer

Using ice slurry produced from supercooled water with an in-stream crystallizer opens a new path for solarice systems, increasing efficiency and reducing investment cost compared to ice-on-coil systems. Power needs are decoupled from the stored energy since the heat exchangers are not evenly distributed in the ice storage vessel but directly placed as the heat pump evaporator, which depends on the heat pump capacity and not on the ice storage volume. The novel ice storage design can serve as a heat source for a heat pump, where its evaporator is used to supercool water below 0 °C, or for refrigeration. The supercooled water at a temperature around −2 °C, maintained in a meta-stable liquid state, is triggered to nucleate in an in-stream crystallizer. The current design of the ice crystallizer allows for continuous operation of the system and scalability. Experimental results obtained with a gasketed plate heat exchanger used to supercool water and an in-stream crystallizer operated at a power of up to 6.5 kW are presented.

Thamm, Ann-Katrin↗

Water Ingress Testing of the Turbula Jar and U-233 Lead Pig Containers

Understanding the water ingress behavior of containers used at the TA-55 Plutonium Facility has significant implications for criticality safety. The purpose of this report is to document the water ingress behavior of the Turbula Jar with Bakelite lid and Viton gaskets (Turbula Jar) used in oxide blending operations and the U-233 lead pig container used to store and transport U-233 material. The technical basis for water resistant containers at TA-55 is described in LA-UR-15-22781, “Water Resistant Container Technical Basis Document for the TA-55 Criticality Safety Program.” Testing of the water ingress behavior of various containers is described in LA-CP-13-00695, “Water Penetration Tests on the Filters of Hagan and SAVY Containers,” LA-UR-15-23121, “Water Ingress into Crimped Convenience Containers under Flooding Conditions,” and in LA-UR- 16-2411, “Water Ingress Testing for TA-55 Containers.” Water ingress criteria are defined in TA55-AP-522 “TA-55 Criticality Safety Program”, and in PA-RD-01009 “TA55 Criticality Safety Requirements.” The water ingress criteria for submersion is no more than 50 ml of water ingress at a 6” water column height for a period of 2 hours.

42 ENGINEERING↗

Final Technical Report: Affordable, High-Performance, Intermediate Temperature Solid Oxide Fuel Cells

In this project, we improved the power output and voltage efficiency of our intermediate temperature solid oxide fuel cells (IT-SOFCs) with a focus on ~600 °C operation. At these temperatures and with the increased power density (i.e., fewer cells for same power output), the stack cost should be greatly reduced while extending durability. Most SOFC stacks operate at temperatures greater than 800 °C. This can greatly increase the cost of the system (stacks and BOP) as well as maintenance costs since the most common degradation mechanisms are thermally driven. Our approach uses no platinum group metal (PGM) materials and the lower operating temperature allows use of simple stainless steel interconnects and commercial off-the-shelf gaskets in the stack. Furthermore, for combined heating and power (CHP) applications the stack exhaust still provides “high quality” waste heat that can be recovered and used in a chiller or boiler. The anticipated performance, durability, and resulting cost improvements (< $700/kWe) will also move us closer to reaching the full potential of this technology for distributed generation (DG) and residential/commercial CHP. This includes eventual extension to cleaner, more efficient portable generators, auxiliary power units (APUs), and range extenders for transportation. The research added to the understanding of the area investigated by exploring various methods for increasing power density (Watts/square centimeter of active area in each cell) and increasing cell efficiency (increasing the open circuit voltage, or cell voltage with zero external electrical current). The results from this work demonstrated an optimized cell that had greater than 1 W/cm2 at 600 °C and greater than 1.6 W/cm2 at 650 °C. This was demonstrated in large format sizes using both 5 cm by 5 cm and 10 cm by 10 cm cells. Furthermore, this work demonstrated that high stability (no degradation over > 500 hours) can be achieved together with high performance in large format cells as large as 10 cm by 10 cm when operated at ~600 °C. The project culminated in the demonstration of a 12-cell stack using the porous anode-based SOFC technology.

03 NATURAL GAS↗

Recommendations for DOT 7A Type A Drum Closure and Drop Testing with Additional 49 CFR 173.465(c)(2) Testing and Analysis

The Savannah River National Laboratory (SRNL) is in the process of developing recommendation for the U S. Department of Energy contractors and vendors who want to qualify drums as U S. Department of Transportation (DOT) 7A Type A to meet 49 CFR 173.465 drop testing requirements for fissile and non-ftssile material to maintain containment. Based on the finite element analysis (FEA) models, the safety features suffering the maximum damage that result in loss of containment are identified as the closure ring mechanism (in entirety), the top (mouth area) of the drum, and the lid (including the gasket). The maximum damage is measured in terms of the collective ability of these combined three safety features to maintain containment. As such, both drop testing and FEA were performed to determine the sensitivities of these safety features to drop variations. As part of this effort, a series of physical drop tests and FEAs were conducted at SRNL. These tests used Skolnik drums, CQ5508L (see Attachment 1), which are open DOT 7A Type A open- head carbon steel 208-liter (55-gallon) drums with 12-gauge bolted closure rings. Variables studied were (1) stress relief methods during closure ring installation, (2) content configurations, and (3) drum orientations during a 4-foot free fall. It should be noted that the Skolnik CQ5508L drums have a closure ring with a "V shaped" cross section. (1) The closure testing with analysis confirmed that closure stress relief by rapping is necessary to distribute the closure ring tension around the perimeter and to maintain sufficient closure pre-load for lid retention during 4-foot drops of the heavier packages (500 to 1,000 lbs). It was concluded that no specific style of stress relief is preferred (e g., multi-step rapping/torqueing process, heavy hits vs. light hits, hitting near closure vs. away), as long as no additional change in bolt torque occurs with additional rapping. (2) (3) Modeling indicated that maximum damage is a result of both: (2) content configuration and (3) drop orientation. The worst-case content configuration is one with an eccentrically loaded concentrated content mass. FEA modeling showed that the center- of-gravity over top (CGoT) with the eccentric content on the high side was the orientation of maximum damage relative to drum lid retention. In this content configuration (i.e., CGoT), FEA modeling showed payloads over 500 lbs were required to contain a load distribution plate between content and lid. Both analysis and testing showed the drum with distribution plate can pass the 4-foot CGoT drop.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗