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At least 397 records · Page 22

Optimized manufacturing process for multilayer two-dimensional focusing mirrors in laboratory X-ray applications

Recent advances in laboratory X-ray applications require high-performance optical components that achieve exceptional imaging resolution and beam uniformity within compact experimental setups. Montel mirrors have become a preferred solution due to their unique dual-reflection focusing mechanism and a space-efficient design. Here, in this study, we present an effective manufacturing process for producing Montel mirrors tailored to focus laboratory X-ray beams. The mirrors were fabricated from single-crystal silicon substrates, chosen for their high mechanical stability and compatibility with precision polishing techniques. Our approach begins with the integration of a deterministic chemo-mechanical polishing (CMP)-based pre-shaping step followed by ion beam figuring (IBF), significantly improving manufacturing efficiency. Subsequently, our custom-developed advanced metrology and IBF techniques were employed for fabricating an off-axis, elliptical cylinder Montel mirror system with a 6-mrad total slope, with stringent optical specifications. While post-IBF processes, including multilayer coating, dicing, and gluing, introduced minor surface errors, yet their impact on performance remained negligible. The Montel mirrors manufactured with the optimized process exhibited significantly improved beam uniformity and a reduced focal spot size. These findings validate our approach as a viable solution for high-precision Montel mirror fabrication and facilitate further advancements in laboratory X-ray applications.

36 MATERIALS SCIENCE↗

A snapshot of high-entropy alloy processing techniques and their effects on resulting mechanical properties

High-entropy alloys (HEAs) exhibit exceptional strength, corrosion resistance, and thermal stability, making them promising candidates for nuclear, aerospace, and other extreme applications. While most prior work has focused on compositional design, manufacturing techniques themselves can alter microstructure and mechanical properties as dramatically as alloy chemistry. This review compiles and compares the effects of processing routes—including arc melting, induction melting, mechanical alloying with spark plasma sintering, and additive manufacturing—on the structure and properties of HEAs. Quantitative comparisons highlight, for example, that SPS-processed alloys can achieve ∼20–45 % higher yield and tensile strength than arc-melted counterparts, while Bridgman solidification produces nearly single-crystal structures with elongation to failure exceeding 80 %. Additive manufacturing routes such as selective laser melting offer fine microstructures but also introduce anisotropy and porosity, leading to yield strengths spanning 100–600 MPa for the same composition. By synthesizing such results, this review provides actionable insight into how processing routes interact with HEA core effects (high entropy, lattice distortion, sluggish diffusion, and cocktail effect) to determine performance, thereby offering a practical guide for optimizing manufacturing strategies.

36 MATERIALS SCIENCE↗

Identifying electrochemical processes by distribution of relaxation times in proton exchange membrane electrolyzers

Distribution of relaxation time (DRT) is used to interpret electrochemical impedance spectroscopy (EIS) for proton exchange membrane (PEM) water electrolyzers, with an attempt to separate overlapped relaxation processes in Nyquist plots. By varying operating conditions and catalyst loadings, four main relaxation peaks arising from EIS can be identified and successfully separated from low to high frequencies as (P1) mass transport, (P2) oxygen evolution reaction kinetics, (P3) reaction kinetics (with faster time constant than P2), and (P4) ionic transport. Here, the shape, height, and frequency of the DRT peaks change with different membrane electrode assembly (MEA) configurations. Electron microscopy reveals distinct features from the cross-sectioned MEAs which verify critical DRT results in that increasing the iridium (Ir)-anode loading from 0.2 mgIr/cm 2 to 1.5 mgIr/cm 2 reduces kinetic losses due to higher site-access; a thick and compacted anode, however, also triggers higher ohmic resistances from membrane/catalyst layer hydration and increases transport losses due to longer ionomer pathways. DRT provides higher resolution to EIS for deconvoluting processes with different relaxation times and the quantification of DRT peaks improves the accounting of total losses from each process.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A review of thermo-hydro-mechanical modeling of coupled processes in fractured rock: From continuum to discontinuum perspective

Coupled thermo-hydro-mechanical (THM) processes in fractured rock are playing a crucial role in geoscience and geoengineering applications. Diverse and conceptually distinct approaches have emerged over the past decades in both continuum and discontinuum perspectives leading to significant progress in their comprehending and modeling. This review paper offers an integrated perspective on existing modeling methodologies providing guidance for model selection based on the initial and boundary conditions. By comparing various models, one can better assess the uncertainties in predictions, particularly those related to the conceptual models. The review explores how these methodologies have significantly enhanced the fundamental understanding of how fractures respond to fluid injection and production, and improved predictive capabilities pertaining to coupled processes within fractured systems. It emphasizes the importance of utilizing advanced computational technologies and thoroughly considering fundamental theories and principles established through past experimental evidence and practical experience. The selection and calibration of model parameters should be based on typical ranges and applied to the specific conditions of applications. The challenges arising from inherent heterogeneity and uncertainties, nonlinear THM coupled processes, scale dependence, and computational limitations in representing field scale fractures are discussed. Realizing potential advances on computational capacity calls for methodical conceptualization, mathematical modeling, selection of numerical solution strategies, implementation, and calibration to foster simulation outcomes that intricately reflect the nuanced complexities of geological phenomena. Future research efforts should focus on innovative approaches to tackle the hurdles and advance the state-of-the-art in this critical field of study.

Coupling scheme↗

Influence of porous aluminosilicate grain size materials in experimental and modelling Cs + adsorption kinetics and wastewater column process

This paper focuses on the influence of the grain size of a geopolymer based adsorbent on its Cs + adsorption performances both in batch and fixed-bed process. The geopolymer phase was used as a binder to support NaY zeolite particle in a 20 wt% charged porous composite with 160 m 2 .g –1 of porous surface area. These samples were shaped with three grain sizes (50 /100/500 µm) to remove 80–90 mg/g of Cs + in batch and column operations. After their microstructural and porous characterizations, their efficiency and adsorption characteristics were investigated through adsorption isotherms and kinetic in the two processes. While the grain size has no influence on the maximal extraction capacity of the adsorbent, it strongly affects the sorption kinetic. By coupling experimental data and a modelling approach, the complex sorption mechanism was highlighted, suggesting a new insight of the contaminant sorption kinetic. Then, comparison of batch and column adsorption experiments illustrates the detailed explanation of various process parameters for column study. The results show challenges for fixed-bed column utilization by the choice of the appropriate grain size as a compromise between the material sorption kinetic and hydrodynamic considerations. Furthermore, this is of high importance to more accurately optimize the design of column adsorption to assess the transport of Cs+ in multi-porous tailored grain size materials.

36 MATERIALS SCIENCE↗

Effect of LPBF Processing Parameters on Inconel 718 Lattice Structures: Geometrical Characteristics, Surface Morphology, and Mechanical Properties

Laser Powder Bed Fusion (LPBF) enables the additive manufacturing of complex lattice structures. However, the fabrication of lattice structures via LPBF poses challenges in achieving the intended geometrical accuracy due to their inherent complexity. This study investigates the effects of LPBF processing parameters, specifically laser power and scanning speed, on the geometrical characteristics, surface quality, and mechanical behavior of Inconel 718 lattices structures. The results reveal that processing parameters required for the fabrication of near-full dense structures do not translate effectively to lattice configurations, as variations in energy input influence lattice geometry and surface quality. In this work, strut thickness, open-pore size, open-cell porosity, and surface roughness were measured, and the mechanical properties of the lattices were evaluated under shear loading. The findings indicate that lower energy inputs, achieved by reducing laser power and increasing scanning speed, yield porous structures but lead to mechanical degradation. In contrast, high energy inputs lead to lattices with enhanced strength but result in undesirable open-pore blockage and dimensional inaccuracies. These findings provide insights into tailoring LPBF parameters for dimensional accuracy in lattices and correlating the processing parameters to mechanical performance and surface roughness.

36 MATERIALS SCIENCE↗

Higher levels of mixed-linkage (1,3;1,4)-β-glucan in transgenic grasses may impact soil C processing

Carbohydrates, including mixed-linkage glucan (MLG), in grass cell walls make them a valuable potential feedstock for biofuel production. Hence, the development of transgenic grasses with elevated levels of MLG is being actively pursued worldwide. Changes in chemical and physical root characteristics of MLG-overproducing transgenic plants can affect processing of the root-derived carbon (C) by soil microorganisms, impacting soil C cycling. Here, this study is the first attempt to elucidate the impact of MLG-related genetic modifications on root traits, root decomposition, and soil C processing. We explored four genotypes of Brachypodium ( Brachypodium distachyon ): a wildtype, a loss-of-function mutant with low MLG, an MLG overexpressing line, and a line lacking MLG hydrolase (with high MLG), incubating their roots in soils of two contrasting vegetation histories: monoculture switchgrass and polyculture restored prairie. The four genotypes exhibited contrasting root MLG and soluble sugar concentrations, and different growth phenotypes. Roots with the highest MLG content resulted in a ∼55 % increase in microbial biomass C compared to wildtype in both soils. However, the genotype effects on C mineralization rates were influenced by the vegetation history, with significant effects observed only in the soil from switchgrass but not prairie origin. While further work is required to understand the full impact of MLG-overproducing plants on soil C accrual, our findings suggest that their influence on soil C processes cannot be discounted.

Brachypodium distachyon↗

Investigation of the temperature-dependent failure processes in PVD Cr-coated ZIRLO nuclear fuel cladding using in situ X-ray micro-tomography imaging

In this work, an accident tolerant fuel cladding system with Cr coating deposited using physical vapour deposition (PVD) method onto commercial Optimized ZIRLO™ was studied. The cladding tubes were machined into C-rings and loaded to failure under compression with real-time synchrotron micro-X-ray computed tomography (XCT) imaging at room temperature (RT), 345 °C, 650 °C and 950 °C in argon (Ar) atmosphere. The mechanical behaviour and failure processes were found strongly temperature-dependent where the Cr coating showed brittle fracture at RT and 345 °C, ductile fracture at 650 °C and a reversion to brittle fracture at 950 °C. Nanoindentation measurements and scanning electron microscopy (SEM) imaging were conducted on the materials after high temperature testing. It was found that recrystallisation of the Cr coating occurred at elevated temperatures, which significantly affected its local properties hence the failure behaviour at different temperatures. This work represents the first in situ 3D XCT observation of progressive failure processes in PVD Cr-coated ZIRLO claddings up to 950 °C providing critical insights into its brittle-to-ductile transition (BDTT) behaviour and subsequent ductile-to-brittle reversion with the increase in temperature. Moreover, results are compared with other PVD Cr-coated Zircaloy materials from open literature; the influences of the coating microstructure and local properties on the failure stress/strain and fracture processes are discussed.

Yuan, Guanjie↗

First-Principles Simulation of Beam-Induced Processes Underlying Atomic Manipulation in Electron Microscopes

The development of experimental methods and apparatuses capable of promoting atomically precise material manipulations holds great promise for realizing the ultimate limit of feature miniaturization in materials and devices. The ability to modify materials atom by atom is anticipated to usher in new technologies in areas as diverse as separation science, medicine, and quantum information science. Historically, scanning probe-based techniques have been the most prominent approaches in this space. However, these methods are best suited for the manipulation of surface-exposed regions of materials, as the strong perturbations required for bond scission are delivered most effectively to atoms in the near-proximity to the scanning probe. In contrast, convergent electron beams with energies tuned slightly below the threshold for inducing irreversible knock-on damage have recently been employed (within scanning transmission electron microscopy) to promote atomic-scale bond rearrangements in various beam-stable solids. Currently, however, the efficiency and selectivity of beam-induced atomic manipulation processes with focused electron beams are such that long irradiation times are required to induce a desired atomic rearrangement. With a better understanding of the underlying physics dictating the outcome of a given irradiation event, methods can be devised to improve the efficiency of these techniques so that their promise can be fully realized through widespread adoption.To this end, this Account details our recent efforts to develop and apply tractable first-principles simulation approaches for studying the response of materials to electric beam-like external electric potentials applied in real space. We briefly review the concepts and capabilities in the area of atomically precise materials manipulation and review the early demonstrations of accomplishments in this area, focusing on studies using scanned convergent electron beam probes in particular. We expound upon the depth of the challenge and identify critical shortcomings of theoretical methods that have previously been employed in the simulation of beam-induced processes. We then describe the computational methods that we have generalized from the concepts and tools most commonly applied to the study of molecular photochemistry and how our adaptations of these methods can be employed to capture the relevant dynamical phenomena for beam-induced processes ranging from the initial electron scattering to the ensuing multistate reactions. Here, we contextualize these methods within the current state of the art in this area, which has historically focused primarily on the simulation of inelastic image formation in the electron microscope for the purpose of interpreting the results of quantitative electron microscopy experiments. We demonstrate that the spatial distribution of state-specific excitation rates due to the presence of an external (probe) electric charge is inhomogeneous, such that irradiation at particular locations in materials can favor specific electronic transitions (and disallow others). In addition to the potential for excited-state reaction pathways to be accessed through the initial inelastic scattering of the tightly focused electron beam from the targeted atoms, we also identify favorable conditions for the electronically nonadiabatic evolution of the highly vibrationally excited system to open complex multistate reaction pathways. Implications of the early results for understanding the mechanisms and potential routes to improved efficiency and selectivity in beam-induced reactions are discussed. We conclude with a summary of the current state of theory and modeling capabilities in this area and provide our perspective on future directions for theoretical and experimental developments that we view as crucial to advancing the use of convergent electron beams in mode-specific, atomically precise platforms for direct-write materials modifications.

36 MATERIALS SCIENCE↗

Process Feasibility Analysis of Waste Biomass Valorization to Biochar and Bio-Oil via Slow and Fast Pyrolysis

The United States has abundant biomass and waste feedstock to support the nation's energy addition and affordability targets. Pyrolysis, a thermochemical conversion process, decomposes lignocellulosic feedstocks into liquid, solid, and gaseous fuels that can contribute to the domestic production of biofuels, biopower, and bioproducts. Growing private sector interest in this technology is a key motivation for this comprehensive techno-economic process modeling analysis of a respective biorefinery that includes feedstock preprocessing, slow and fast pyrolysis, and product separation to bio-oil, biochar, and syngas hydrocarbons. Results show that biochar from slow pyrolysis could achieve minimum selling prices (MSPs) of $\$$188-$\$$260/t, competitive with reported market values, while bio-oil from fast pyrolysis is estimated to yield MSPs of $\$$6.49-$\$$9.68/GGE, approximately twice conventional fuel benchmarks. Sensitivity analysis identifies feedstock cost, product yield, and scale as primary cost drivers, while scenarios involving biochar carbon credits and high value applications may substantially improve economics. Overall, these results suggest that continued innovation in feedstock logistics, process integration, and market development will be critical to achieving economically viable and scalable bioproducts.

09 BIOMASS FUELS↗

Postfire Biogeochemical Processes: Implications to Source Water Quality in Fire-Influenced Watersheds

Forested watersheds are instrumental in providing purified and reliable water to millions of people worldwide. The changing climate has increased the frequency and severity of global fire events. Forested watersheds and their ecosystem functions are greatly disrupted during fire activity. Postfire concerns in forested watersheds include unpredictable and potentially simultaneous alterations in source water quality and hydro-biogeochemical processes. Here, the degree of fire severity can complexly modify water quality through the production of fire-transformed constituents on the burned forest floor (i.e., nutrients, metal(loid)s, dissolved organic matter, and the formation of disinfection byproducts). Correspondingly, fire severity and postfire rainfall patterns can refine hydro-biogeochemical processes that influence the transport of the fire-transformed constituents (i.e., vegetation function, soil structure, hydrological pathways, and microbial communities). Postfire alterations to water quality and hydro-biogeochemical processes introduce further complexity with varying temporal influence, which ranges from months to decades. As postfire water quality and watershed response research progresses, it is essential to homogenize interdisciplinary expertise to bridge knowledge gaps between fields ranging from forest ecology, hydrology, microbiology, and geochemistry. A multidisciplinary approach in wildfire research will facilitate a comprehensive perception of the diverse water quality risks associated with fire activity and mitigate fire concerns on a global level.

Disinfection Byproducts↗

Designing a Robust MEA-Based Post-Combustion Carbon Capture Process with Capture Rate Guarantees

This work presents an application of the nonlinear two-stage robust optimization solver PyROS to the model-based design and operation of a monoethanolamine scrubbing process for CO<sub>2</sub> capture under epistemic uncertainty. Through this application, risk-averse process designs are successfully obtained for CO<sub>2</sub> capture targets ranging from 90% to over 99%. In particular, the risk-averse solutions for CO<sub>2</sub> capture targets of up to 98% are shown to be only marginally more expensive than their nominally optimal counterparts. Thus, the results demonstrate the utility of recently developed nonlinear robust optimization approaches for the solution of large-scale chemical process models under uncertainty.

20 FOSSIL-FUELED POWER PLANTS↗

Physics-Informed Gaussian Process Inference of Liquid Structure from Scattering Data

We present a nonparametric Bayesian framework to infer radial distribution functions from experimental scattering measurements with uncertainty quantification using nonstationary Gaussian processes. The Gaussian process prior mean and kernel functions are designed to mitigate well-known numerical challenges with the Fourier transform, including discrete measurement binning and detector windowing, while encoding fundamental yet minimal physical knowledge of the liquid structure. We demonstrate uncertainty propagation of the Gaussian process posterior to unmeasured quantities of interest. Experimental radial distribution functions of liquid argon and water with uncertainty quantification are provided as both a proof of principle for the method and a benchmark for molecular models.

Chemical structure↗

Operando XPS for Plasma Process Monitoring: A Case Study on the Hydrogenation of Copper Oxide Confined under h-BN

Here, we demonstrate that ambient pressure x-ray photoelectron spectroscopy (APXPS) can be used for in situ studies of dynamic changes in surface chemistry in a plasma environment. This opens a new and vast application space for XPS and greatly complements modern spectroscopy techniques to probe plasma-solid/liquid interactions relevant to process monitoring in the semiconductor industry, bio-medical plasma applications and plasma remediation technologies. Hexagonal boron nitride (h-BN) grown on Cu was used in this study as a well-defined model system for plasma process monitoring and because of its unique chemical, optical and electrical properties that make it a prospective material for advanced electronics. To better understand the stability and surface chemistry of h-BN during plasma assisted processing, we track in real time the plasma-induced chemical state changes of B, N and the underlying Cu substrate using APXPS equipped with an AC discharge plasma source operating at 13 Pa. Residual gas analysis (RGA) mass-spectra were concurrently collected during plasma-XPS to track reaction products formed during plasma exposure. A clear reduction of Cu x O is seen, while an h-BN layer remains intact, suggesting hydrogen radical (H • ) species can attack the exposed and h-BN covered Cu oxide patches and partially reduce the underlying substrate without significantly damaging the overlaying h-BN, which is of practical importance for development of h-BN encapsulated devices and interfaces. In addition to demonstration of plasma-XPS capabilities we discuss the observed challenges (e.g., parasitic plasma-chamber walls reactions and charging effects) and propose potential solutions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A Reduced-Temperature Process for Preparing Atomically Clean Si(100) and SiGe(100) Surfaces with Vapor HF

Silicon processing techniques such as atomic precision advanced manufacturing (APAM) and epitaxial growth require surface preparations that activate oxide desorption (typically >1000 °C) and promote surface reconstruction toward atomically clean, flat, and ordered Si(100)-2 × 1. Here, in this study, we compare the aqueous and vapor phase cleaning of Si and Si/SiGe surfaces to prepare APAM-ready and epitaxy-ready surfaces at lower temperatures. Angle resolved X-ray photoelectron spectroscopy (ARXPS) and Fourier transform infrared (FTIR) spectroscopy indicate that vapor hydrogen fluoride (VHF) cleans dramatically reduce carbon surface contamination and allow the chemically prepared surface to reconstruct at lower temperatures, 600 °C for Si and 580 °C for a Si/Si 0.7 Ge 0.3 heterostructure, into an ordered atomic terrace structure indicated by scanning tunneling microscopy (STM). After thermal treatment and vacuum hydrogen termination, we demonstrate STM hydrogen desorption lithography (HDL) on VHF-treated Si samples, creating reactive zones that enable area-selective chemistry by using a thermal budget similar to CMOS process flows. We anticipate that these results will establish new pathways to integrate APAM with Si foundry processing.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Self-Trapped-Exciton Radiative Recombination in β–Ga 2 O 3 : Impact of Two Concurrent Nonradiative Auger Processes

The peculiarities of radiative and nonradiative processes associated with self-trapped intrinsic eXcitons in the excited β-Ga 2 O 3 crystals are studied via time-resolved techniques of induced absorption, transient grating, and photoluminescence (PL) at room temperature. The excitation above the bandgap is produced by laser pulses with linear light polarization parallel and orthogonal in the (–201) and (001) planes. We elucidate that the nonradiative recombination rate occurring in the eXciton prevails over its radiative emission rate in a wide range of free carrier concentration composed of excited and equilibrium electrons. Hence, the nonradiative recombination has no effect on the strong anisotropy and the shape of the eXciton emission band. However, we find out that the conventional ABC model of electron effective lifetime is insufficient for explanation of the excitation dependences. Inclusion of two nonradiative Auger mechanisms in a modified ABC formula provides excellent agreement of these dependences. We conclude that the trap-assisted Auger process is in proportion to the free electron density with coefficient B = 1.1 × 10 –11 cm 3 /s and appears at low/intermediate excitation, while the triple-particle Auger process is in proportion to Δn 2 with coefficient C = 8 × 10 –30 cm 6 /s and appears at high excitation conditions. The transition between two Auger mechanisms is accompanied by a rise of the eXciton diffusivity in preferred crystallographic directions where the radiative PL intensity is maximal. The diffusion length LD in these directions can reach values ~300 nm, but, at high excitations, LD becomes limited by Auger lifetimes. These findings pave the way for the implementation of self-trapped eXcitons into specific optoelectronic devices.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

CO 2 Conversion to Butene via a Tandem Photovoltaic–Electrochemical/Photothermocatalytic Process: A Co-design Approach to Coupled Microenvironments

Here, we developed a tandem, unassisted, solar-driven electrochemical and photothermocatalytic process for the single-pass conversion of CO 2 to butene using only simulated solar irradiation as the energetic input. The two-step process involves electrochemical CO 2 reduction (CO 2 R) to ethylene followed by ethylene dimerization to butene. We assessed two unassisted electrochemical setups to concentrate ethylene in the CO 2 R reactor, achieving concentrations up to 5.4 vol.% with 1.8% average solar-to-ethylene conversion and 5.6% average CO 2 -to-ethylene single-pass conversion under 1-sun illumination. When passed through the photothermocatalytic ethylene oligomerization reactor, we generated 600 ppm of butene under 3-sun illumination. Through analysis of this process, we identified that the presence of H 2 , CO, and H 2 O leads to rapid deactivation of the Ni-based ethylene oligomerization catalyst.

14 SOLAR ENERGY↗

DeSelenator: A Se-Removal Process for Environmental Decontamination of Wastewaters from Coal-Burning Power Plants

Selenium may become a toxic contaminant of freshwater systems when released into the environment through industrial wastewaters from mining, coal-burning power plants, or oil refining. Efficient and cost-effective Se-removal technologies are therefore necessary to reduce Se concentrations in these wastewaters to below the regulatory discharge limits. In this study, we have demonstrated an effective process that removes Se, mostly as selenate anions, from wastewaters generated by coal-burning power plants. This process, dubbed DeSelenator, leverages the high concentration of sulfate relative to selenate in the wastewater and the propensity of these oxyanions to cocrystallize with benzene-bis-iminoguanidinium (BBIG) cations into extremely insoluble salts (on par with BaSO 4 ). The SO 4 2− /SeO 4 2− cocrystallization with BBIG removes over 90% of S and Se from the wastewater. Following removal of the precipitate by filtration, the filtrate is passed over an anion-exchange resin that further reduces selenium concentration to 5 ppb, the EPA’s regulatory limit for freshwater systems. Finally, the effluent is passed over an activated carbon column, which removes 99.8% of the residual BBIG ligand remaining after crystallization, allowing for the safe discharge of the treated water into the environment. The Se-removal process was first optimized in the lab at the bench scale and then tested in the field at the Tennessee Valley Authority’s Bull Run coal-burning power plant. A technoeconomic assessment found the cost of water treatment with DeSelenator is on par with that of the active biological method, which is currently considered a state-of-the-art Se-removal technology.

anions↗