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At least 595 records · Page 33

Mechanical behavior of bimetallic stainless steel and gray cast iron repairs via directed energy deposition additive manufacturing

The utility of gray cast iron in engine components remains tied to the mechanical performance and cost. Repair and remanufacturing of castings offer economical and sustainable benefits; however, high thermal input from traditional fusion-based welding is unable to restore the original mechanical quality owing to brittle microstructures and porosity formed in situ. Directed energy deposition (DED) is an additive manufacturing method that has received considerable interest for repairs owing to the highly controllable nature of the process. Despite this, few works have connected the effect of DED parameters on actual interfacial strength. Consequently, distinct DED parameter combinations were identified to maximize the strength and fatigue life of the repaired cast iron. Further, high speed melt pool imaging and residual stress measurements are provided to aid in the understanding of the metallurgical quality and strength seen in these structures. In general, higher scanning speeds and lower thermal gradients promoted comparable tensile strength to that of the original gray cast iron. The results presented here provide a foundation to tune in the DED process to generate the required mechanical quality as a starting point for future process advancements.

36 MATERIALS SCIENCE↗

Modulation of thermal conductivity of iron-doped ß-Ga2O3 by helium-ion irradiation

This study examines the impact of helium-ion irradiation on the thermal conductivity of ß-Ga2O3. A laser-based spatial domain thermoreflectance technique is used to investigate thermal conductivity map for both un-irradiated and irradiated ß-Ga2O3, which are then validated against simulation results derived from density functional theory-based phonon transport simulations. Since helium bubble evolution was ob- served at the nanoscale using transmission electron microscopy, the simulation study was carried out on eight distinct helium-induced sites in ß-Ga2O3. Our findings indicate a reduction in thermal conductivity for the irradiated samples. Experimental results show a significant reduction in thermal conductivity in irradiated samples, with de- creases of approximately 25% along the [100] direction and 40% along [001] directions. Phonon transport simulations closely replicate these findings, particularly when helium occupying interstitial sites, predicting reductions of ˜53% along [100] and ˜50% along [001] directions. This work underscores the role of irradiation-induced microstructural changes in the heat transport properties of ß-Ga2O3 which is crucial for its application in sensor devices in extreme environments.

36 - MATERIALS SCIENCE↗

Metal–Ligand Cooperativity via Exchange Coupling Promotes Iron- Catalyzed Electrochemical CO 2 Reduction at Low Overpotentials

Biological and heterogeneous catalysts for the electrochemical CO 2 reduction reaction (CO 2 RR) often exhibit a high degree of electronic delocalization that serves to minimize overpotential and maximize selectivity over the hydrogen evolution reaction (HER). Here, we report a molecular iron(II) system that captures this design concept in a homogeneous setting through the use of a redox non-innocent terpyridine-based pentapyridine ligand (tpyPY2Me). As a result of strong metal-ligand exchange coupling between the Fe(II) center and ligand, [Fe(tpyPY2Me)] 2+ exhibits redox behavior at potentials 640 mV more positive than the isostructural [Zn(tpyPY2Me)] 2+ analog containing the redox-inactive Zn(II) ion. This shift in redox potential is attributed to the requirement for both an open-shell metal ion and a redox non-innocent ligand. The metal-ligand cooperativity in [Fe(tpyPY2Me)] 2+ drives the electrochemical reduction of CO 2 to CO at low overpotentials with high selectivity for CO 2 RR (>90%) and turnover frequencies of 100,000 s -1 with no degradation over 20 h. The decrease in the thermodynamic barrier engendered by this coupling also enables homogeneous CO 2 reduction catalysis in water without compromising selectivity or rates. Synthesis of the two-electron reduction product, [Fe(tpyPY2Me)] o , and characterization by X-ray crystallography, Mössbauer spectroscopy, X-ray absorption spectroscopy (XAS), variable temperature NMR, and density functional theory (DFT) calculations, support assignment of an open-shell singlet electronic structure that maintains a formal Fe(II) oxidation state with a doubly reduced ligand system. Furthermore, this work provides a starting point for the design of systems that exploit metal-ligand cooperativity for electrocatalysis where the electrochemical potential of redox non-innocent ligands can be tuned through secondary metal-dependent interactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Non-Altermagnetic Origin of Exchange Bias Behaviors in Incoherent RuO 2 /Fe Bilayer Heterostructures

Initially identified as a promising altermagnetic (AM) candidate, rutile RuO 2 has since become embroiled in controversy due to contradictory findings of modeling and measurements of the magnetic properties of bulk crystals and thin films. For example, despite observations of a bulk nonmagnetic state using density functional theory, neutron scattering, and muon spin resonance measurements, patterned RuO 2 Hall bars and film heterostructures display magnetotransport signatures of magnetic ordering. Among the characteristics routinely cited as evidence for AM is the observation of exchange bias (EB) in an intimately contacted Fe-based ferromagnetic (FM) layer, which can arise due to interfacial coupling with a compensated antiferromagnet. Here, within this work, the origins of this EB coupling in Ru-capped RuO 2 /Fe bilayers are investigated using polarized neutron diffraction, polarized neutron reflectometry, cross-sectional transmission electron microscopy, and super conducting quantum interference device measurements. These experiments reveal that the EB behavior is driven by the formation of an iron oxide interlayer containing Fe 3 O 4 that undergoes a magnetic transition and pins interfacial moments within Fe at low temperature. These findings are confirmed by comparable measurements of Ni-based heterostructures, which do not display EB coupling, as well as magnetometry of additional Fe/Ru bilayers that display oxide-driven EB coupling despite the absence of the epitaxial RuO 2 layer. While these results do not directly refute the possibility of AM ordering in RuO 2 thin films, they reveal that EB, and related magnetotransport phenomena, cannot alone be considered evidence of this characteristic in the rutile structure due to interfacial chemical disorder.

RuO2↗

Process design and techno-economic analysis for bio-based graphite and liquid hydrocarbons production from lignocellulosic biomass

The worldwide demand for graphite, as the main anode material for Li-ion batteries, is expected to double by 2028 since it supports the use of electricity, including transient renewable sources, for energy storage, sustainable mobility, and automation. However, the dependence on non-renewable and external resources jeopardizes the world supply chain. This study explores the technical and economic performance of transforming lignocellulosic biomass into biographite and fuel-grade hydrocarbons through pyrolysis bio-oil upgrading. According to simulation results, the total power demand for the biorefinery reached 10,784 kWh per tonne of biographite, of which 36 % can be supplied by the heat integration network and power plant. Sensitivity and risk analyses were conducted to evaluate the economics, with process yields identified as the most relevant indicators to the minimum selling price (MSP). The analysis revealed a promising cost-competitive range for biographite MSP against fossil-based graphite (medium quality synthetic graphite Chinese market price ~$\$$4.2/kg). Case D, which includes biofuels as a byproduct, presents the best metrics, reaching a MSP of $\$$3.3/kg of anode-grade biographite with a profit margin of 27 %. While including biofuels in the product slate provides the best economic performance, the uncertainty associated with the big capital investment makes its risk 13 % higher to attain an IRR >20 % than the case in which biographite is produced as a standalone product. Overall, this study demonstrates that integrated biorefineries can produce a cost-competitive bio-based anode material for Li-ion batteries.

09 BIOMASS FUELS↗

Daily operational impacts on battery degradation in heavy-duty electric drayage trucks

Battery aging is a critical factor influencing the performance, longevity, and cost of ownership of battery electric trucks (BETs). This paper presents a comprehensive evaluation of battery aging for two Li-ion battery chemistries, Nickel-Manganese-Cobalt (NMC) and Lithium-Iron-Phosphate (LFP), accounting for both cycling and calendar aging. In contrast to traditional methods that rely on simplified linear degradation models based on manufacturer-provided data, this study employs semi-empirical aging models calibrated to experimentally collected data. The models are integrated into a detailed vehicle simulation environment, enabling a comprehensive assessment of battery degradation under realistic operating conditions. A case study focusing on heavy-duty electric drayage truck operations in the Port of Savannah, GA, is presented to illustrate the impact on battery pack lifespan of: seasonal variations, daily operational activities, charging strategies, and battery storage conditions. The results illuminate the significance of the battery pack’s state of charge during stationary periods, such as overnight storage or weekend parking, on battery degradation and its potential implications for long-term vehicle viability. Additionally, the study explores how different operational and environmental factors affect battery degradation, offering critical insights into best battery charging and storage practices. Our results demonstrate that LFP outperforms NMC in terms of years of useful life; however, by utilizing charging strategies that minimize the amount of time the battery spends resting at high levels of state-of-charge, the lifespan of the battery pack that uses NMC can nonetheless be increased by more than a factor of two.

25 ENERGY STORAGE↗

Impact of Acid–Base Stimulation Sequence on Mineral Stability for Tight/Impermeable Unconventional Carbonate-Rich Rocks: A Delaware Basin Case Study

We report mineral precipitation due to reactions with injected fluids during unconventional fracture stimulation is a well-recognized problem. The goal of this study is to evaluate secondary mineral precipitation and permeability attenuation under chemical injection scenarios specific to the Delaware basin. Whole cylindrical cores (2.54 cm diameter and 2.54 cm height) and ground shale (150–250 μm) from the carbonate-rich Bone Spring Formation, Delaware Basin TX (Leonardian), were reacted at 80 °C and 85 bar using a hydraulic fracturing fluid (HFF) recipe and an injection sequence typical of the Delaware Basin. The reacted shales and solutions were analyzed using a variety of laboratory- and synchrotron-based techniques to characterize both the chemical and spatial distributions of secondary mineral precipitation and identify changes in permeability and mineralogy. This carbonate-rich shale (>84% calcite) rapidly neutralized the acidic HFF. Synchrotron-based X-ray fluorescence mapping coupled with X-ray absorption spectroscopy (both bulk and micro) showed that most of the iron was in an oxidized form prior to exposure to HFF and that almost all iron(II) became fully oxidized after the reaction. Scanning electron microscopy images of the ground shale samples primarily identified iron(oxyhydr)oxide microcrystals on grain surfaces. A few small isolated iron-rich areas also contained sulfur, suggesting that some pyrite was preserved when isolated within a calcite crystal but that most was oxidized. The rapid neutralization of the acid spearhead in these carbonate-rich samples demonstrates that the acid spearhead is useful for initiating fractures in extremely calcite-rich rocks but does little to enhance rock permeability. This suggests that the impact of the acid spearhead is significantly smaller for carbonate-rich shales compared to clay-rich shales, which has broad implications for acidizing in carbonate-rich shale formations and iron transformations within these shales.

58 GEOSCIENCES↗

High-Resolution XFEL Structure of the Soluble Methane Monooxygenase Hydroxylase Complex with its Regulatory Component at Ambient Temperature in Two Oxidation States

Soluble methane monooxygenase (sMMO) is a multicomponent metalloenzyme that catalyzes the conversion of methane to methanol at ambient temperature using a nonheme, oxygen-bridged dinuclear iron cluster in the active site. Structural changes in the hydroxylase component (sMMOH) containing the diiron cluster caused by complex formation with a regulatory component (MMOB) and by iron reduction are important for the regulation of O 2 activation and substrate hydroxylation. Structural studies of metalloenzymes using traditional synchrotron-based X-ray crystallography are often complicated by partial X-ray-induced photoreduction of the metal center, thereby obviating determination of the structure of the enzyme in pure oxidation states. Here, microcrystals of the sMMOH:MMOB complex from Methylosinus trichosporium OB3b were serially exposed to X-ray free electron laser (XFEL) pulses, where the ≤35 fs duration of exposure of an individual crystal yields diffraction data before photoreduction-induced structural changes can manifest. Merging diffraction patterns obtained from thousands of crystals generates radiation damage-free, 1.95 Å resolution crystal structures for the fully oxidized and fully reduced states of the sMMOH:MMOB complex for the first time. The results provide new insight into the manner by which the diiron cluster and the active site environment are reorganized by the regulatory protein component in order to enhance the steps of oxygen activation and methane oxidation. Furthermore, this study also emphasizes the value of XFEL and serial femtosecond crystallography (SFX) methods for investigating the structures of metalloenzymes with radiation sensitive metal active sites.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A hemoprotein with a zinc-mirror heme site ties heme availability to carbon metabolism in cyanobacteria

Abstract Heme has a critical role in the chemical framework of the cell as an essential protein cofactor and signaling molecule that controls diverse processes and molecular interactions. Using a phylogenomics-based approach and complementary structural techniques, we identify a family of dimeric hemoproteins comprising a domain of unknown function DUF2470. The heme iron is axially coordinated by two zinc-bound histidine residues, forming a distinct two-fold symmetric zinc-histidine-iron-histidine-zinc site. Together with structure-guided in vitro and in vivo experiments, we further demonstrate the existence of a functional link between heme binding by Dri1 (Domain related to iron 1, formerly ssr1698) and post-translational regulation of succinate dehydrogenase in the cyanobacterium Synechocystis , suggesting an iron-dependent regulatory link between photosynthesis and respiration. Given the ubiquity of proteins containing homologous domains and connections to heme metabolism across eukaryotes and prokaryotes, we propose that DRI (Domain Related to Iron; formerly DUF2470) functions at the molecular level as a heme-dependent regulatory domain.

59 BASIC BIOLOGICAL SCIENCES↗

Rapid quantitative analysis of trace elements in plutonium alloys using a handheld laser-induced breakdown spectroscopy (LIBS) device coupled with chemometrics and machine learning

Here, we present the first reported quantification of trace elements in plutonium via a portable laser-induced breakdown spectroscopy (LIBS) device and demonstrate the use of chemometric analysis to enhance the handheld device's sensitivity and precision. Quantification of trace elements such as iron and nickel in plutonium metal via LIBS is a challenging problem due to the complex nature of the plutonium optical emission spectra. While rapid analysis of plutonium alloys has been demonstrated using portable LIBS devices, such as the SciAps Z300, their detection limits for trace elements are severely constrained by their achievable pulse power and length, light collection optics, and detectors. In this paper, analytical methods are evaluated as a means to circumvent the detection constraints. Three chemometric methods often used in analytical spectroscopy are evaluated; principal component regression, partial least-squares regression, and artificial neural networks. These models are evaluated based on goodness-of-fit metrics, root mean-squared error, and their achievable limits of detection (LoDs). Partial least squares proved superior for determining content of iron and nickel in plutonium metal, yielding LoDs of 15 and 20 ppm, respectively. These results of identifying the undesirable trace elements in plutonium components are critical for applications such as fabricating radioisotope thermoelectric generators or nuclear fuel.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Linking the Spin Transition of Ferric Iron in δ‐(Al,Fe)OOH to Water Storage in the Lower Mantle

As the most massive geochemical reservoir, the lower mantle affects the Earth's budget of volatile elements, including hydrogen or H 2 O. The properties of minerals in the lower mantle are further affected by changes in the electronic configurations of iron cations, that is, by spin transitions. The feedback between spin transitions and potential storage of H 2 O in solid hydrous phases in the lower mantle, however, remains unexplored. By combining high‐pressure nuclear resonant inelastic X‐ray scattering and high‐pressure high‐temperature X‐ray diffraction experiments, we constrained the thermal equation of state of δ‐(Al,Fe)OOH, a member of the phase H solid solution. Based on the derived thermal equation of state of δ‐(Al,Fe)OOH and the underlying thermodynamic model, we calculate the excess Gibbs free energy that arises from the spin transition of ferric iron in this compound and evaluate the effect on phase equilibria. The results of our analysis show that the spin transition of ferric iron in phase H may significantly reduce the thermodynamic activity and hence the concentration of H 2 O in a coexisting hydrous melt. As a consequence, nominally anhydrous minerals of the lower mantle may become dehydrated in the presence of phase H. Our analysis further suggests that, under certain conditions, the spin transition may expand the thermal stability of Fe 3+ ‐bearing phase H and create a geochemical link between the storage of H 2 O in phase H and ferric iron in the lower mantle.

Buchen, Johannes [Univ. of Bayreuth (Germany); Cal↗

Integration of Omics into a New Comprehensive Rate Law for Competitive Terminal Electron-Accepting Processes in Reactive Transport Models: Application to N, Fe, S, and Contaminant Transformations in Stream and Wetland Sediments

Surface waters represent important sources of alternate energy and drinking water in the United States, and characterizing the biogeochemical processes that affect surface water quality is relevant to the DOE-BER mission. Sediment biogeochemical processes regulate the release of carbon (C), nutrients, and contaminants to surface waters and thus influence water quality. Sediment biogeochemical processes are dynamic and affected by the deposition and remobilization of solid material and changes in environmental conditions driven by water discharge variations. Wetlands are important natural filters of surface waters which may either trap, metabolize, or mobilize nutrients and contaminants. Despite their importance, biogeochemical processes regulating nutrient and contaminant release and C transformation in stream and wetland sediments cannot be predicted accurately by current mathematical models. These reactive transport models largely rely on detectable changes in geochemical conditions to activate metabolic processes, do not accurately account for the competition between microbial processes, and poorly constrain effects of hydrological perturbations on biogeochemical processes. In this BER-SBR exploratory project, metagenomic and geochemical signatures were combined to identify microbially-mediated redox processes in anaerobic stream and wetland sediments from the Savannah River Site (SRS, ANL SFA) and East Fork Poplar Creek (EFPC, ORNL SFA) that play important roles in C, uranium (U), and mercury (Hg) transformations. In addition, sediment incubations were conducted to examine the competition between anaerobic respiration processes Finally, new rate laws were developed for reactive transport models that rely on complementary metagenomic and geochemical signatures to identify the underlying anaerobic microbial processes in stream and wetland sediments, describe the competition between the dominant metabolic processes involved in nutrient release and U and Hg mobilization, and more accurately quantify carbon transformation and the response of microbial processes to changes in redox conditions associated with hydrological forcing. These rate laws were optimized in batch reactors with SRS wetland sediments, where iron and sulfate reduction dominate. Anaerobic carbon remineralization processes followed the expected thermodynamic sequence of microbial respiration with depth in both sediments, except that geochemical signals indicated that sulfate reduction was inactive in EFPC sediments and moderate in SRS wetland sediments. Estimates indicated that microbial iron reduction contributed to at least half of the production of reduced iron in these sediments. Incubations demonstrated that nitrate reduction, denitrification, and dissimilatory nitrate reduction to ammonium were active in the natural EFPC sediment and activated upon nitrate amendment in these nitrate-rich sediments. In turn, these processes were outcompeted by the addition of either iron oxides or sulfate as alternative terminal electron acceptors. Although geochemical products of sulfate reduction were not detected in the incubations, the abundance of sulfate reduction genes increased with depth in the sediment and was equally more pronounced in treatments amended with either iron oxides or sulfate. Simultaneously, anaerobic sulfide oxidizing bacteria coupling sulfide oxidation to DNRA (and not conventional denitrification) were apparently enriched over time, regardless of the treatments. These findings indicate that sulfate reduction is important in freshwater stream sediments and probably catalyzed by a cryptic sulfur cycle involving nitrogen species, in which the sulfur products from sulfate reduction are immediately removed by side reactions and not detectable by geochemical measurements alone. Similar experiments in SRS sediments, however, demonstrated little interaction between nitrogen and sulfur cycling microorganisms. Sulfate reduction was impacted by the addition of more thermodynamically favorable electron acceptors, suggesting either that iron-reducing microorganisms outcompeted sulfate-reducing microorganisms for organic substrate, depleting the stock of electron donor available for sulfate reduction, or that the cryptic sulfur cycle was shunted by the precipitation of FeS generated as a result of the abiotic reduction of iron oxides by dissolved sulfide. A diagnostic modeling exercise was conducted to further investigate the competition between terminal electron accepting processes. As conventional kinetic models typically do not account for cryptic cycles and used inaccurate formulations to describe competition between microbial communities, new metabolic rate laws were developed that explicitly express the electron acceptor-specific enzyme of each energetically favorable metabolic process based on gene abundance detected in the incubations. The model was tested with the sediment slurry incubation data to determine whether substrate competition could explain the decrease in sulfate reduction observed in the presence of iron oxide competitor. The model was able to reproduce geochemical concentrations really well in each treatment once the model was calibrated with the unamended control, suggesting that microbial competition was indeed driven by thermodynamic considerations. Overall, carbon remineralization processes and rates will be reproduced much more realistically with the new metabolic rate laws.

54 ENVIRONMENTAL SCIENCES↗

Machine-Learned Force Field for Molecular Dynamics Simulations of Nonequilibrium Ammonia Synthesis on Iron Catalysts

Ammonia (NH 3 ) is one of the most important industrial chemicals. The conventional NH 3 synthesis method-the Haber–Bosch process-converts atmospheric nitrogen (N 2 ) into NH 3 using H 2 with an iron (Fe) catalyst. However, this process requires high pressures (100–200 atm) and temperatures (700–800 K) near thermal equilibrium. Recently, Fe-based nanocatalysts have been reported to produce promising NH 3 yields under atmospheric pressures and temperature-modulated nonequilibrium conditions. Understanding the mechanism of nonequilibrium catalysis with programmed temperature variation could help to optimize this fully electrified and less energy-intensive process. Although reactive molecular dynamics (RMD) simulations can be a useful tool to model nonequilibrium catalytic processes, they require the development of accurate force fields (i.e., interatomic potentials). Here, we present a machine-learned (ML) force field within the Deep Potential MD (DPMD) framework, trained using periodic density functional theory (DFT) calculations, to model NH 3 synthesis on Fe catalysts with various surface adsorbates such as *N, *H, *N 2 , *H 2 , *NH, *NH 2 , and *NH 3 . Here, we generated the DFT data from static models of elementary reactions on the most stable (110) surface of body-centered cubic Fe, which then were augmented by data from constant number of particles–volume–temperature (NVT) DFT-MD trajectories at various temperatures. Finally, we utilized the fully optimized ML force field to investigate reaction dynamics at an Fe(110) surface at linearly increasing temperatures using NVT-DPMD simulations. Our simulations indicate that pulsed temperature ramping could prove favorable for NH3 synthesis. For example, we conducted ramping under multiple sets of conditions: (i) from 900 to 1200 K over periods of 0.1–0.3 ns for Fe surfaces precovered with N or NH along with H; and (ii) from 300 to 600 K over 0.1–0.3 ns for Fe surfaces precovered with NH 3 . While our simulations so far are limited to short time scales (very rapid heating), these observations shed light on the mechanism of the high NH 3 synthesis rate achieved in a novel temperature-modulated nonequilibrium catalytic reactor using pulsed heating and cooling.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Iron-assisted growth of anisotropic ZnO nanostructures

Anisotropic nanostructures offer a promising pathway to modulate structure-function relationships of materials. However, the correlation between growth direction of high-quality anisotropic nanostructures, the synthesis conditions and mechanisms controlling their growth, and their magnetic and optical properties remain underexplored. In this study, we developed an iron-assisted anisotropic growth method to form zinc oxide nanostructures on the O-polar (0001̄) surface, resulting in two distinct ZnO-based nanostructures: hand-shaped nanostructures and truncated hexagonal nanopyramids. In contrast to most reports of anisotropic nanostructure synthesis, which primarily focus on morphology control through ligand-ligand interactions, the current study probes the effects of doping on anisotropic growth, and how doping, along with ligand-ligand interactions and facet-specific ligand binding, control nanostructure morphology. The reaction mechanisms leading to formation of these novel structures were thoroughly probed by systematically manipulating synthesis parameters. A two-step formation mechanism was identified: first, a hexagonal platform forms through an initial homogeneous nucleation process, followed by secondary heterogeneous nucleation, which results in metastable secondary nanostructures growing on the oxygen-rich template. Optical and magnetic properties of these Fe/ZnO nanostructures were characterized. Our findings provide a new strategy that uses a magnetic element as a dopant to build new nanostructures of ZnO with controllable size and shape growing on an oxygen-rich crystal plane. These materials could have applications in novel technologies where both optoelectronic and magnetic properties are of interest.

Xuan, Zhengxi↗

Geochemical Impact of Acid Spearhead and Slickwater Stimulation on Wolfcamp Shale from the Hydraulic Fracturing Test Site

The Hydraulic Fracturing Test Site 1 (HFTS-1) was a field study performed in the Wolfcamp Formation in the West Texas Permian (Midland) Basin, USA, with a focus on improving the efficiency of hydraulic fracturing. Investigating site-specific rock-fluid geochemical interactions during hydraulic fracturing is an important step to understanding the impact on formation shale porosity, permeability, and long-term shale gas production. During field operations in this region, hydraulic fracturing fluid (HFF) injection usually starts with a concentrated acid spearhead for rapid rock dissolution, followed by the injection of near-neutral pH slickwater containing chemicals and proppants. A multistep sequential injection approach was used to investigate different stages of rock-fluid interactions. The carbonate content in the host rock is important when acid spearhead is considered, as carbonate mineral dissolution is rapid and can result in porosity and permeability changes in the shale matrix. Here, in this study, we designed flow-through experiments using fractured carbonate-rich and clay-rich Wolfcamp shale cores with (1) a short-time acid soaking step and (2) a long-term slickwater flow-through step to simulate the injection method used at HFTS-1. The fluid chemistry was analyzed. A thorough mineralogical progression [e.g., Calcium (Ca) dissolution and iron (Fe) redox progression] in the cores during HFF injection was also characterized and imaged by synchrotron microprobe. Reactive transport modeling was performed based on the experimental setup. The results showed that the acid spearhead is a crucial step in creating a reaction front by mineral dissolution, especially in carbonate-rich shales. A slight layer of ferrihydrite precipitated during the slickwater flow-through period. This study provides insights into potential geochemical impact due to hydraulic fracturing operations in the Permian Basin.

clastic rock↗

Self-Limitations of Heat Release in Coupled Core-Shell Spinel Ferrite Nanoparticles: Frequency, Time, and Temperature Dependencies

We explored a series of highly uniform magnetic nanoparticles (MNPs) with a core-shell nanoarchitecture prepared by an efficient solvothermal approach. In our study, we focused on the water dispersion of MNPs based on two different CoFe 2 O 4 core sizes and the chemical nature of the shell (MnFe 2 O 4 and spinel iron oxide). We performed an uncommon systematic investigation of the time and temperature evolution of the adiabatic heat release at different frequencies of the alternating magnetic field (AMF). Our systematic study elucidates the nontrivial variations in the heating efficiency of core-shell MNPs concerning their structural, magnetic, and morphological properties. In addition, we identified anomalies in the temperature and frequency dependencies of the specific power absorption (SPA). We conclude that after the initial heating phase, the heat release is governed by the competition of the Brown and Néel mechanism. In addition, we demonstrated that a rational parameter sufficiently mirroring the heating ability is the mean magnetic moment per MNP. Our study, thus, paves the road to fine control of the AMF-induced heating by MNPs with fine-tuned structural, chemical, and magnetic parameters. Importantly, we claim that the nontrivial variations of the SPA with the temperature must be considered, e.g., in the emerging concept of MF-assisted catalysis, where the temperature profile influences the undergoing chemical reactions.

36 MATERIALS SCIENCE↗

Strontium Effects on the Formation of Iron-Intermetallic Phases in Secondary Al–9Si–0.6Fe Alloys

The presence and morphology of Fe-containing intermetallic phases affect the mechanical properties of aluminum alloys, especially in secondary Al–Si-based cast alloys. Although strontium (Sr) addition of 50 to 500 ppm is known to refine the needle-type eutectic silicon structure, the influence of Sr on the formation of Fe-intermetallic phases remains unclear. The present work investigates the combined additions of Sr and Mn to Al–9Si–0.6Fe–0.35Mg (All compositions are in wt pct except otherwise stated.) alloys on the formation of Fe-intermetallic phases at different solidification rates from ~ 1.5 to ~ 60 °C/s. Long and branched-type AlFeSi phase with size ranging from 50 to 120 µm are more common when solidified at the rate of 1.5 °C/s regardless of Sr and Mn additions. However, at the fast solidification rate of 60 °C/s, a 60 ppm Sr addition significantly reduced the average length of needle-shaped AlFeSi phase to less than 3 to 5 µm. Thermodynamic simulations have been performed using CALculation of PHAse Diagrams (CALPHAD) models to predict the formation of various phases and their possible interactions during solidification. The results indicated that the combination of a high solidification rate and about 60 ppm of Sr is beneficial to refining the δ-Al 3 FeSi 2 phase in Al–Si–Mg alloys containing 0.6 pctFe. As a result, this unexpected finding of Fe-intermetallic refinement by low Sr addition (~60 ppm) provides an important guide in designing secondary alloys for sustainable casting applications.

36 MATERIALS SCIENCE↗

Bridging Structure, Magnetism, and Disorder in Iron-Intercalated Niobium Diselenide, Fe x NbSe 2 , below x = 0.25

Transition-metal dichalcogenides (TMDs) intercalated with magnetic ions serve as a promising materials platform for developing next-generation, spin-based electronic technologies. In these materials, one can access a rich magnetic phase space depending on the choice of intercalant, host lattice, and relative stoichiometry. The distribution of these intercalant ions across given crystals, however, is less well defined–particularly away from ideal packing stoichiometries–and a convenient probe to assess potential longer-range ordering of intercalants is lacking. Here, we demonstrate that confocal Raman spectroscopy is a powerful tool for mapping the onset of intercalant superlattice formation in Fe-intercalated NbSe 2 (Fe x NbSe 2 ) for 0.14 ≤ x < 0.25. We use single-crystal X-ray diffraction to confirm the presence of longer-range intercalant superstructure and employ polarization-, temperature-, and magnetic field-dependent Raman measurements to examine both the symmetry of emergent phonon modes in the intercalated material and potential magnetoelastic coupling. Magnetometry measurements further indicate a correlation between the onset of magnetic ordering and the relative degree of intercalant superlattice formation. These results show Raman spectroscopy to be an expedient, local probe for mapping intercalant ordering in this class of magnetic materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗