An image-based equation for estimating the prospective CO2 storage resource of organic-rich shale formations
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Azenkeng, Alexander↗
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Statistical fracture behavior of doped UO 2 using a ball-on-ring equibiaxial flexure test method
Metal oxide dopants, such as titanium and chromium oxides, have garnered considerable attention for their potential to increase grain size (≥ 30 µm) in UO 2 fuel, purportedly enhancing fission gas retention during reactor operation. Fuel performance is significantly impacted by fuel fracture behavior, so it is important to understand the effects of enhanced grain size and dopant content on UO 2 fuel fracture. UO 2 pellets were doped with 0.1 wt% TiO 2 and 0.3 wt% Cr 2 O 3 to alter density and grain size. Inductively coupled plasma mass spectroscopy measured dopant levels pre- and post-sintering. X-ray diffraction revealed lattice changes and microstrain via Rietveld refinement. Field emission scanning electron microscopy determined grain sizes of approximately 30 µm for TiO 2 doping and 7 µm for Cr 2 O 3 doping. Transverse rupture strength tests were performed on over 30 samples per dataset to obtain characteristic strength and Weibull modulus. Results indicate no statistical difference in fracture strength between 0.1 wt% TiO 2 doped UO 2 and undoped UO 2 , while 0.3 wt% Cr 2 O 3 doped UO 2 exhibited a 20% decrease in fracture strength. Doped UO 2 samples also showed reduced Weibull modulus compared to undoped UO 2 , suggesting increased scatter in fracture strength. This study's findings suggest that titanium and chromium oxide doping in UO 2 , regardless of grain size, induce residual stresses, decreasing fracture strength and increasing variability in fracture behavior.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Degradation of a Cr-Mo steel by carbide precipitation over long-term service
Microstructure of the 40-year service-exposed 1Cr-0.5Mo steel extracted from pressure vessels through the boat sampling technique was characterized using x-ray diffraction, field-emission scanning electron microscopy, energy dispersive spectrometry, electron backscatter diffraction, focused ion beam, and transmission electron microscopy. The microstructure degradation during long-term service was identified. Statistical crystal plastic ity models were developed to correlate the microstructure and mechanical properties quantitatively. The steel is found significantly strengthened but slightly embrittled. Nanoscale Mo 2 C carbides have nucleated within the ferrite matrix over the long-term service, resulting in significant strengthening of the matrix. The coarser grain boundary Cr 23 C 6 carbides, on the other hand, act as the damage accumulation sites and lead to the degradation.
36 MATERIALS SCIENCE↗
Development of an in situ ion irradiation scanning electron microscope
An in situ ion irradiation scanning electron microscope (I 3 SEM) has been developed, installed, and integrated into the Ion Beam Laboratory at Sandia National Laboratories. The I 3 SEM facility combines a field emission, variable pressure, scanning electron microscope, a 6 MV tandem accelerator, high flux low energy ion source, an 808 nm-wavelength laser, and multiple stages to control the thermal and mechanical state of the sample observed. The facility advances real-time understanding of materials evolution under combined environments at the mesoscale. As highlighted in multiple examples, this unique combination of tools is optimized for studying mesoscale material response in overlapping extreme environments, allowing for simultaneous ion irradiation, implantation, laser bombardment, conductive heating, cooling, and mechanical deformation.
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
Characterizing mineralization on low carbon steel exposed to aerated and degassed synthetic hydraulic fracture fluids
This study investigates the mineralization occurring at the interface between injected hydraulic fracturing fluids and steel production casing during the shut-in period of unconventional shale wells. Mild steel coupons were reacted with synthetic hydraulic fracturing fluids with varying base fluid and dissolved gas concentrations. Experiments were carried out in an autoclave system set at 50 °C and 2000 PSI for 2 and 14 days. Physical and mineralogical changes to the steel coupons’ surface were characterized using an FEI Quanta 600 field emission gun (FEG) scanning electron microscope (SEM) and a PANalytical XPert Pro diffractometer. Barite precipitation occurred ubiquitously during the first 48 hours in all experimental scenarios. Sulfate radicals created from degradation and reduction of ammonium persulfate breakers facilitate barite formation. Concomitant barite and corrosion related precipitates on the sample surfaces suggest iron hydroxy salts act as nucleation sites for mineral scale growth. These results suggest hydraulic fracturing fluids may have deleterious effects on the wellbore before production of the well begins.
36 MATERIALS SCIENCE↗
Geochemical and Microstructural Characterization of Shale Rock: A Workflow for Site Evaluation for Energy–Fluids Storage
Shales are a central component of petroleum systems, as source, seal, and unconventional reservoir rocks. Unlike traditional unconventional shale, a newly emerging Caney Shale play is regarded as an unconventional of unconventional shales (UUS), due to its high content of fine-grained materials, lower reservoir porosity, dominance of nanopores, and a scarcity of visible natural fractures. Other developed unconventional shales such as the Woodford and Barnett have larger average pore size, higher porosity, and extensive natural fractures at core scale that contribute to reservoir quality. In this work, the Caney Shale was cored in entirety to characterize its interbedded ductile and reservoir intervals and establish criteria for their recognition. Representative ductile and reservoir intervals known as D2 and R3, respectively, were selected for detailed analysis including variations in elemental composition, mineralogy, facies, and the presence of natural fractures at well and core scales using X-ray fluorescence, X-ray diffraction, and thin section and core description. Characteristics of microstructure and microgeochemistry at nano- and microscales are compared using field emission scanning electron microscopy with energy dispersive spectroscopy and lowpressure nitrogen adsorption isotherms with fractal dimension analysis. The ductile (detrital clay-rich) member D2 is characterized by higher concentrations of Ti and Al and lower Si, while the reservoir R3 (possibly biogenic silica-accumulated) is characterized by lower Ti and Al and higher Si. Eight mixed carbonate–siliciclastic facies are recognized, and R3 shows a higher heterogeneity of facies stacking and average fracture abundance than D2. Further, R3 shows a more microscopically heterogeneous fabric/texture of matrix and a higher microporosity than D2 that has a higher pore surface heterogeneity. A fundamental understanding of the compositional and microstructural characteristics of UUS and further ductile/reservoir intervals will allow for a better assessment of reservoir quality, more effective production of hydrocarbons, and optimized selection of safe caprocks in carbon sequestration and subsurface hydrogen storage.
58 GEOSCIENCES↗
Directional Gateway to Metal Oxidation: 3D Chemical Mapping Unfolds Oxygen Diffusional Pathways in Rhodium Nanoparticles
The interaction of oxygen with a reactive metal is ubiquitous, yet the precise atomic-level mechanisms and pathways leading to the formation of a surface oxide are not well-understood. We report oxygen atom distributions inside Rh single nanoparticles using atom probe microscopy (APM) and demonstrate that mainly facets of the ?022¯? crystallographic directions act as oxygen-permeable gateways. The highly anisotropic spatial distribution of incorporated oxygen atoms is in agreement with video-field emission analyses according to which {113} facets of the ?022¯? zones act as portals for subsurface diffusion. In addition to providing a more fundamental understanding of the precursor states to metal corrosion, in particular for the case of nanosized metal particles, our studies are also relevant for heterogeneous catalysis where catalytic activity and selectivity conform to reaction-induced structural changes of metal nanoparticles.
Lambeets, Sten V M.↗
Iridium-Doped Nanosized Zn–Al Layered Double Hydroxides as Efficient Water Oxidation Catalysts
Layered double hydroxides (LDHs) are an ideal platform to host catalytic metal centers for water oxidation (WO) owing to the high accessibility of water to the interlayer region, which makes all centers potentially reachable and activated. In this paper, we report the syntheses of three iridium-doped zinc–aluminum LDHs (Ir-LDHs) nanomaterials (1–3, with about 80 nm of planar size and a thickness of 8 nm as derived by field emission scanning electron microscopy and powder X-ray diffraction studies, respectively), carried out in the confined aqueous environment of reverse micelles, through a very simple and versatile procedure. These materials exhibit excellent catalytic performances in WO driven by NaIO 4 at neutral pH and 25 °C, with an iridium content as low as 0.5 mol % (~0.8 wt %), leading to quantitative oxygen yields (based on utilized NaIO 4 , turnover number up to ~10,000). Nanomaterials 1–3 display the highest ever reported turnover frequency values (up to 402 min –1 ) for any heterogeneous and heterogenized catalyst, comparable only to those of the most efficient molecular iridium catalysts, tested under similar reaction conditions. The boost in activity can be traced to the increased surface area and pore volume (>5 times and 1 order of magnitude, respectively, higher than those of micrometric materials of size 0.3–1 μm) estimated for the nanosized particles, which guarantee higher noble metal accessibility. X-ray absorption spectroscopy (XAS) studies suggest that 1–3 nanomaterials, as-prepared and after catalysis, contain a mixture of isolated, single octahedral Ir(III) sites, with no evidence of Ir–Ir scattering from second-nearest neighbors, excluding the presence of IrO 2 nanoparticles. The combination of the results obtained from XAS, elemental analysis, and ionic chromatography strongly suggests that iridium is embedded in the brucite-like structure of LDHs, having four hydroxyls and two chlorides as first neighbors. These results demonstrate that nanometric LDHs can be successfully exploited to engineer efficient WOCs, minimizing the amount of iridium used, consistent with the principle of the noble-metal atom economy.
36 MATERIALS SCIENCE↗
3D Printing of Polyelectrolyte Complex-Integrated Photocurable Hydrogel Resins
In this study, we developed a photocurable hydrogel resin incorporating a polyelectrolyte complex (PEC) for 3D printing. Acrylamide-based monomers were formulated with varying PEC contents (0–15 wt %) in an aqueous KBr medium to fabricate patterned porous hydrogel structures. The morphology of printed hydrogels was characterized by field-emission scanning electron microscopy and energy-dispersive X-ray spectroscopy. Notably, the PEC5 and PEC10 formulations exhibited optimal thermal stability and compressive properties, attributed to the homogeneous distribution of PEC domains within the hydrogel matrix. Furthermore, dye adsorption experiments demonstrated excellent removal efficiency, highlighting the potential of PEC-containing hydrogels for environmental remediation applications, particularly in the treatment of dye-contaminated wastewater.
Yang, Jinchul [University of Tennesse Knoxville]↗
Visible Light Harvesting Cr(III) Photocatalysts
Pseudo-octahedral Cr(III) photosensitizers offer a promising alternative to Ru(II)/Ir(III) MLCT chromophores due to their long-lived, strongly photo-oxidizing excited states, yet suffer from poor visible-light absorption. Here, to address this challenge, we prepared a series of homoleptic Cr(III) trissd phenanthroline) complexes bearing arylacetylene units on the 4- and 7-positions at each phenanthroline core. This modification produced a >1 eV bathochromic shift in intraligand (IL) π–π* transitions and enhanced absorption across the UVA and blue-to-green regions (ε ∼25,000–100,000 M –1 cm –1 ) compared to [Cr(phen) 3 ] 3+ , eclipsing traditional MLCT photosensitizers while leaving 2 E ligand-field-emission energies largely unaffected. Nanosecond transient absorption and photoluminescence measurements confirmed long excited-state lifetimes (τ = 33–119 μs in CH 3 ) while featuring strongly oxidizing excited-state potentials: E°'([Cr] 3+ */ 2+ ) = 0.97–1.09 V vs. Fc +/0 . High quantum yields for 1 O 2 production (Φ Δ ≤ 0.85) resulted in efficient photosensitized oxidation of 1,5-dihydroxynaphthalene to juglone under blue or green light irradiation within 30 min (0.1–0.2 mol % catalyst loading). Photocatalytic [4 + 2] cycloadditions under blue or green light (yields up to 100%) were also demonstrated at low catalyst loadings (0.1–0.3 mol %). The combined results demonstrate that large visible absorption cross sections are readily achievable in Cr(III) diimines by leveraging IL transitions, without compromising excited-state energetics or lifetimes.
Wheeler, Jonathan P. [North Carolina State Univers↗
Long-Term Trends for Marine Sulfur Aerosol in the Alaskan Arctic and Relationships With Temperature
Marine aerosol plays a vital role in cloud-aerosol interactions during summer in the Arctic. The recent rise in temperature and decrease in sea ice extent have the potential to impact marine biogenic sources. Compounds like methanesulfonic acid (MSA) and non-sea-salt sulfate (nss-SO 4 2- ), oxidation products of dimethyl sulfide (DMS) emitted by marine primary producers, are likely to increase in concentration. Long-term studies are vital to understand these changes in marine sulfur aerosol and potential interactions with Arctic climate. Samples were collected over three summers at two coastal sites on the North Slope of Alaska (Utqiagvik and Oliktok Point). MSA concentrations followed previously reported seasonal trends, with evidence of high marine primary productivity influencing both sites. When added to an additional data set collected at Utqiagvik, an increase in MSA concentration of + 2.5% per year and an increase in nss-SO 4 2- of + 2.1% per year are observed for the summer season over the 20-year record (1998–2017). This study identifies ambient air temperature as a strong factor for MSA, likely related to a combination of interrelated factors including warmer sea surface temperature, reduced sea ice, and temperature-dependent chemical reactions. Analysis of individual particles at Oliktok Point, within the North Slope of Alaska oil fields, showed evidence of condensation of MSA onto anthropogenic particles, highlighting the connection between marine and oil field emissions and secondary organic aerosol. Finally, this study shows the continued importance of understanding MSA in the Arctic while highlighting the need for further research into its seasonal relationship with organic carbon.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Study of dielectric breakdown in liquid xenon with XeBrA: The xenon breakdown apparatus
Maintaining the electric fields necessary for the current generation of noble liquid time projection chambers (TPCs), with drift lengths exceeding 1 m, requires a large negative voltage applied to their cathode. Delivering such high voltage is associated with an elevated risk of electrostatic discharge and electroluminescence, which would be detrimental to the performance of the experiment. The Xenon Breakdown Apparatus (XeBrA) is a 5-l, high voltage test chamber built to investigate the contributing factors to electrical breakdown in noble liquids. Here, in this work, we present the main findings after conducting scans over stressed electrode areas, surface finish, pressure, and high voltage ramp speed in the medium of liquid xenon. Area scaling and surface finish were observed to be the dominant factors affecting breakdown, whereas no significant changes were observed with varying pressure or ramp speed. A general rise in both the anode current and photon rate was observed in the last 30 s, leading up to a breakdown, with a marked increase in the last couple of seconds. In addition, the position of breakdowns was reconstructed with a system of high-speed cameras and a moderate correlation with the Fowler–Nordheim field emission model was found. Tentative evidence for bubble nucleation being the originating mechanism of breakdown in the liquid was also observed. We deem the results presented in this work to be of particular interest for the design of future, large TPCs, and practical recommendations are provided.
73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
Effects of electron beam irradiation on CrMnV and CrMnTiV high entropy alloys: Nano-mechanical, structural, and thermodynamic perspectives
Beam exit windows are crucial components of any particle accelerator as they provide an interface between the beamline vacuum and target material at atmospheric media. For high beam power machines, special materials and designs are required to withstand high radiation and mechanical loads, while minimizing energy loss during transition and maximizing window lifetime. This research investigates the impact of electron beam exposure to bulk CrMnV and CrMnTiV high entropy alloys (HEAs) with the primary goal of identifying suitable candidate materials for the design of robust and durable exit window settings. The selection criteria include intrinsic characteristics, power dissipation, and mechanical responses. According to the thermodynamic calculations, both equiatomic CrMnV and the addition of 7% of Ti with equiatomic CrMnV yield solid-solutions phases. The structural and mechanical properties of CrMnV and CrMnTiV samples were tested using field emission scanning electron microscopy, atomic force microscopy, scanning electron microcopy with energy dispersive x-ray spectroscopy, x-ray diffraction, and nanoindentation before and after exposure to a dose of ~66 kGy from a 10 MeV e-beam accelerator. Despite exhibiting beam transmission characteristics comparable to Cr and V, the indentation hardness of HEAs exceeded that of the Cr and V samples by five to six times. The examination of the CrMnTiV irradiated samples revealed organized deformation patterns depicting new features, which we suspect twinning and twin boundaries due to the addition of Ti to CrMnV. Ti, a hexagonal-close-packed crystal structure, is commonly known for deformation twinning behavior.
36 MATERIALS SCIENCE↗
An SF 6 gas-insulated −500 kV DC conical insulator vacuum feedthrough
A test electrode was biased to −500 kV direct current (DC) by means of a novel SF 6 gas-insulated conical alumina insulator feedthrough. The design enables the extreme high vacuum conditions required by spin-polarized electron sources by reducing the photogun vacuum chamber volume compared to coaxial cylindrical insulators. In contrast to conventional inverted-insulator photogun designs that rely on solid dielectric interfaces for high-voltage terminations, the present design employs a pressurized SF 6 intervening volume between a conical alumina insulator and a modified commercial epoxy high-voltage cable receptacle. Here, this approach enables the use of commercially available cable hardware while extending the demonstrated operating voltage of solid feedthroughs. A maximum voltage of −500 kV was applied to a test electrode attached to the narrow end of the feedthrough inside a chamber filled with SF 6 at 170.3 kPa (10 psig) and later under vacuum to −259 kV, limited by field emission. The results demonstrate that a commercial high-voltage cable combined with a custom-designed SF 6 gas-insulated vacuum feedthrough can be used to bias photogun electrodes to −500 kV DC.
Palacios-Serrano, Gabriel [Thomas Jefferson Nation↗
Twists and turns: stacking and structure-dependent optical response in MoS 2 nanoscrolls
Transition metal dichalcogenide (TMD) nanoscrolls (NSs), specifically MoS 2 NSs, present unique structural and optical properties, exhibiting prominent photoluminescence (PL) signals despite their multilayer nature. Here, this study investigates the structural and spectroscopic characteristics of MoS 2 NSs, correlating them to show the effects of reduced interlayer interactions on excitons of MoS 2 NSs. The reduction in interlayer interaction arises from two main factors: (1) symmetry-broken mixed stacking due to misalignment between layers and (2) a highly inhomogeneous strain profile generated by the Archimedean spiral geometry with positive eccentricity. Transmission electron microscopy, field emission scanning electron microscopy, atomic force microscopy, Raman spectroscopy, and second harmonic generation measurements confirm these findings. Low-temperature PL spectroscopy explores the impact of reduced interlayer interactions on exciton properties such as exciton–phonon coupling and oscillator strength. This study provides crucial insights into the structure, stacking and unique optical properties of TMD NSs, advancing the understanding of interlayer interactions and their impacts in complex quasi-one-dimensional nanostructures.
25 ENERGY STORAGE↗
Ultracold Electrons via Near-Threshold Photoemission from Single-Crystal Cu(100)
Achieving a low mean transverse energy or temperature of electrons emitted from the photocathode-based electron sources is critical to the development of next-generation and compact x-ray free electron lasers and ultrafast electron diffraction, spectroscopy, and microscopy experiments. In this Letter, we demonstrate a record low mean transverse energy of 5 meV from the cryo-cooled (100) surface of copper using near-threshold photoemission. Further, we also show that the electron energy spread obtained from such a surface is less than 11.5 meV, making it the smallest energy spread electron source known to date: more than an order of magnitude smaller than any existing photoemission, field emission, or thermionic emission based electron source. Overall, our measurements also shed light on the physics of electron emission and show how the energy spread at few meV scale energies is limited by both the temperature and the vacuum density of states.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
Analytical and numerical studies of dark current in radiofrequency structures for short-pulse high-gradient acceleration
High-gradient acceleration is a key research area that could enable compact linear accelerators for future colliders, light sources, and other applications. In the pursuit of high-gradient operation, rf breakdown limits the attainable accelerating gradient in normal-conducting rf structures. Recent experiments at the Argonne Wakefield Accelerator suggest a promising approach: using short rf pulses with durations of a few nanoseconds. Experimental studies show that these 𝒪(1 ns) rf pulses can mitigate breakdown limitations, resulting in higher gradients. For example, an electric field of nearly 400 MV/m was achieved in an 𝑋-band photoemission gun driven by 6-ns-long rf pulses, with rapid rf conditioning and low dark current observed. Despite these promising results, the short-pulse regime remains an underexplored parameter space, and rf breakdown physics under nanosecond-long pulses requires further investigation. In this paper, we present analytical and numerical simulations of dark current dynamics in accelerating cavities operating in the short-pulse regime. We study breakdown-associated processes spanning different time scales, including field emission, multipacting, and plasma formation, using simulations of the 𝑋-band photogun cavities. The results reveal the advantages of using short rf pulses to reduce dark current and mitigate rf breakdown, offering a path toward a new class of compact accelerators with enhanced performance and reduced susceptibility to breakdown.
Linear accelerators↗
Electromagnetic Shielding Design for 200 kW Stationary Wireless Charging of Light-Duty EV
Wireless power transfer (WPT) is a developing technology with the advantage of convenience and flexible charging. SAE recommended practice J2954 defines typical size and geometry with aluminum or ferrite plate shielding to limit leakage electromagnetic (EM) fields for WPT with power levels lower than 22 kVA from the input side. However, as the WPT power goes up to 100- or 200-kW level, EM safety surrounding the WPT becomes a critical concern. To address this oncoming safety challenge, a novel ferrite shielding design is proposed in this paper. Different misalignment scenarios in accordance with definitions in SAE J2954 are also taken into consideration to ensure EM safety under various operation scenarios. Simulation results, which are preliminarily verified by magnetic field measurements at 1.1 m from the center of the vehicle side coil under 100 kW operation, indicate that the magnetic field leakage can be maintained below the limits defined in SAE J2954 for 200 kW operation. A 3.3 kW scale-down test was also carried out and compared to parallel scale-down simulations. 26.8% field emission reduction is observed from the scale-down test, which supports the effectiveness of the proposed shielding design.
Zhang, Bo↗