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At least 289 records · Page 16

Evaluation of microstructural changes in fresh cement paste using AC impedance spectroscopy vs. oscillation rheology and 1H NMR relaxometry

AC impedance spectroscopy (ACIS) is a promising technique for monitoring the microstructure evolution of fresh cement paste in real-time. This paper compared the change of bulk electric resistivity (ρ{sub bulk}) obtained from ACIS with the developments of storage modulus (G′) and the mean transverse relaxation times (T{sub 2}) of fresh Portland cement pastes within 5 h. It was found that the three different phases (Phase I, II, and III) on the microstructural build-up process of fresh paste can be accurately distinguished by analyzing ρ{sub bulk}, as well as G′ and T{sub 2}. The use of ρ{sub bulk} fails to characterize the microstructural changes in Phase I due to the great sensitivity on the electrical conductivity of the interstitial solution. However, it can successfully reflect the developing features of microstructure in Phases II and III, and reliably evaluate the impacts of water to cement ratio, superplasticizer, and supplementary cementitious materials on the microstructural development.

36 MATERIALS SCIENCE↗

Ultrathin Ruthenium Films on Graphene Buffered SiO 2 via Quasi Van der Waals Epitaxy

In this study, we demonstrate a quasi van der Waals epitaxy approach to prepare single crystalline Ru ultrathin film on large scale, monolayer graphene. Physical and epitaxial properties of bulk, near surface and surface of ultrathin Ru films were comprehensively studied using various structural, morphological, compositional, and electrical characterization techniques. Here, we confirm that Ru can epitaxially grow on single, monolayer graphene using magnetron sputtering at elevated temperature of 600 °C. The epitaxial Ru films with film thickness ranging from 94.2 nm down to 3.9 nm show the (0001) out-of-plane orientation. The epitaxial relationships between Ru and graphene are out-of-plane Ru(0001) || graphene(0001) and in-plane Ru[$11\bar20$] || graphene[$11\bar20$]. All the Ru films show smooth surfaces with root-mean-square roughness less than 0.8 nm and have negligible oxide layer on the surfaces. The Ru films on graphene demonstrate significantly reduced electrical resistivity comparing to their counterpart grown on bare SiO 2 , which show polycrystalline nature. For 7.1 to 3.9 nm film thicknesses, the resistivity of Ru on graphene shows 38 to 45% resistivity decrease from that of Ru film on bare SiO 2 without graphene. Our observations suggest the existence of the above-classical van der Waals interaction between Ru and graphene. On the other hand, graphene is capable of effectively blocking the inter-diffusion/interaction between Ru and SiO 2 during a 1000 °C annealing process.

36 MATERIALS SCIENCE↗

Epitaxial Stabilization and Oxygen Evolution Reaction Activity of Metastable Columbite Iridium Oxide

Non-rutile polymorphs of binary iridium oxide such as columbite IrO 2 (α-IrO 2 ) are promising candidates for highly active acid-stable oxygen evolution reaction (OER) catalysts, yet their synthesis has been challenging due to the dominant thermodynamic stability of rutile IrO 2 (R-IrO 2 ). Here, we report the growth of α-IrO 2 via epitaxial thin films using pulsed laser deposition. We observe that, in competition with R-IrO 2 (100), the films can be optimized to be predominantly (100)-oriented α-IrO 2 . Surprisingly, the activity of α-IrO 2 shows a large discrepancy of ~0.2 V in the overpotential compared to its predicted activity, which is resolved via theoretical calculations to be a crystal orientation effect. This demonstrates that the electrocatalytic activity can be significantly varied upon crystal orientation, a parameter that is difficult to control in conventional polycrystalline systems but accessible in epitaxial thin films. In total, this study demonstrates epitaxial thin film growth as a powerful technique, which can overcome large energetic instabilities on the order of ~300 meV to stabilize metastable material structures inaccessible by bulk synthesis. As a result, this provides unique opportunities to effectively identify the atomic structure of active catalysts by combining investigations of metastable materials with theoretical predictions.

36 MATERIALS SCIENCE↗

Additive Manufacturing of Coreless Flyback Transformers Using Aerosol Jet Printing and Electrochemical Deposition

An additive manufacturing approach combining aerosol jet printing (AJP) and electrodeposition opens a new pathway to the production of lightweight coreless flyback transformer devices for power electronics. AJP of seed layers with resolution on the order of 30 μm is combined with electrodeposition of Cu and Ni for decreased resistance. This combined approach addresses known shortcomings of AJP and electrodeposition. Nanoparticle inks used in AJP of metals have low conductivity versus bulk materials due to their high grain boundary resistance. There is a lack of readily available high-resolution patterning techniques for electrodeposition outside of expensive clean-room-based lithography techniques. Combining these two techniques enables the patterning of high-resolution, high-conductivity components. Here in this manuscript, we report on the construction of coreless flyback transformers consisting of two-layer primary and two-layer secondary spiral inductors separated by layers of a printed UV-curable dielectric. An input voltage of 17 V at 400 kHz was amplified to an output of 1250 V corresponding to a gain of 73.5. COMSOL modeling at the individual inductor level and at the transformer level was used to compare expected inductance, equivalent series resistance (ESR), and coupling with experimentally measured values.

36 MATERIALS SCIENCE↗

Magnesium isotopes of the bulk solar wind from Genesis diamond-like carbon films

–NASA’s Genesis Mission returned solar wind (SW) to the Earth for analysis to derive the composition of the solar photosphere from solar material. SW analyses control the precision of the derived solar compositions, but their ultimate accuracy is limited by the theoretical or empirical models of fractionation due to SW formation. Mg isotopes are “ground truth” for these models since, except for CAIs, planetary materials have a uniform Mg isotopic composition (within ≤1&) so any significant isotopic fractionation of SW Mg is primarily that of SW formation and subsequent acceleration through the corona. This study analyzed Mg isotopes in a bulk SW diamond-like carbon (DLC) film on silicon collector returned by the Genesis Mission. A novel data reduction technique was required to account for variable ion yield and instrumental mass fractionation (IMF) in the DLC. The resulting SW Mg fractionation relative to the DSM-3 laboratory standard was ( 14.4&, 30.2&) (4.1&, 5.5&), where the uncertainty is 2σ SE of the data combined with a 2.5& (total) error in the IMF determination. Two of the SW fractionation models considered generally agreed with our data. Their possible ramifications are discussed for O isotopes based on the CAI nebular composition of McKeegan et al. (2011).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Repair strategy for fused silica wedged focus lens with high-density filamentary damage

The National Ignition Facility (NIF) is intentionally operated with the final fused silica glass (SiO2) optics exposed to fluences and intensities with the potential to induce damage that will grow with additional laser exposure. Therefore, the NIF operates a recycle loop to refurbish final optics by mitigating any initiated surface damage to arrest its growth. However, the morphology of filamentary damage, caused by local self-focusing in the bulk of a silica optic, adds complexity to optics mitigation and provides a limitation to optic reusability. Here, we evaluate techniques for mitigating isolated and clustered filamentary damage. Optical microscopy before and after installation on NIF was used to determine the efficacy of filamentary mitigation after a series of high fluence and intensity laser exposures. The challenges and success rate of the methods are compared for various filamentary damage mitigation strategies.

National Ignition Facility↗

Galvanostatic Intermittent Titration Technique Reinvented: Part II. Experiments

Following a critical review of the galvanostatic intermittent titration technique in Part I, here we experimentally demonstrate how to extract chemical diffusivity with a modified method. We prepare dense bulk samples that ensure diffusion-limitation. We utilize the scaling with $\sqrt{{t}_{\mathrm{relax}}+\tau }-\sqrt{{t}_{\mathrm{relax}}}$ (trelax: relaxation time; τ: pulse duration), avoiding problems with composition-dependent overpotentials. The equilibrium Nernst voltage is measured separately using small porous particles. This separation between the diffusion measurement and the titration procedure is critical for performing each measurement in a reliable setting. We report the chemical diffusion coefficients of LixNi1/3Mn1/3Co1/3O2 and their activation energy. We extract ionic conductivity and compare it with total conductivity to confirm ion-limitation in chemical diffusion. The measurements suggest that the time scale for diffusion in typical Li-ion battery particles could be much shorter than that of the intercalation/deintercalation processes at the particle surface (Biot number less than 0.1).

25 ENERGY STORAGE↗

Assessment of Benefits of Solid-State Advanced Manufacturing Processes for Nuclear Energy Products

The Advanced Materials and Manufacturing Technology (AMMT) program develops cross cutting technologies in support of a broad range of nuclear reactor technologies and maintains U.S. leadership in materials and manufacturing technologies for nuclear energy applications. This overall project provides the U.S. Department of Energy a critical feasibility study comparison of three solid-state processes to other AM processes, thereby providing the feasibility of the solid-state processes examined to manufacture 316H SS and ODS steel components: • Fused-filament fabrication (FFF): This work provides an initial evaluation of the impact of powder morphology and sizes on the FFF process, and the feasibility and adaptability for different material systems, to use FFF for ODS steels and 316 SS. • Shear-assisted processing and extrusion (ShAPE): Specifically for this portion of the project on ShAPE tube forming, the objectives will be to determine the feasibility to direct tube forming of high tensile strength steel tubing, specifically for ODS steel to determine the effect of the patented extrusion process on the dispersoids of the ODS material. Additionally, as often ODS powders are mechanically alloyed and therefore more platelike or angular, this feasibility was to explore the impact on the optimization process and initial feasibility of direct tube forming. • Cold spray and friction stir additive manufacturing as a stretch goal: Bulk and near net shape manufacturing processes for high-temperature, high-strength alloys are needed. Additionally, cold spray techniques can be applied in-situ at the operational level for repair and can provide multiple benefits to the nuclear industry. These tasks aim to provide information to show benefits of cold spray during the full life cycle, namely research and development, product manufacturing, and repair to mention a few key points.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Verification of Special Nuclear Material (SNM) using Active Well Coincidence Counter (AWCC) and a High Purity Germanium (HPGe) Detector

SNM verification can be accomplished via two methods i.e. destructive analysis (DA) or nondestructive analysis (NDA). The DA modes are much more accurate compared to NDA modes; nevertheless, the sample's physical integrity is destroyed in the process. Techniques such as ICP-MS, ID-ICP-MS, TI-MS are few examples of DA, where a bulk material is ground and mixed with a solution (some form of acid) to acquire a homogenous sample. In contrast, NDA modes utilize signals emitted by the sample such as gamma, neutrons, light, or heat to analyze samples under investigation. HPGe detectors are some of the most frequently used gamma detectors to assay SNM. However, in a high activity scenario it provides a large uncertainty and sometimes becomes unfeasible to measure low energy gamma rays. Meanwhile, neutron detectors are not affected by the gamma background, therefore they can be used in addition to the gamma detectors to verify total fissile mass ({sup 235}U + {sup 239}Pu) of SNM. The AWCC is one of the thermal neutron NDA systems developed at the Los Alamos National Laboratory (LANL). It consists of 42 {sup 3}He detectors to measure gross neutrons (singles), coincidence neutrons (doubles), higher order multiplicity counting (triples, quadruples, etc.). It can effectively operate in both active and passive neutron interrogation modes. It can utilize AmLi, AmBe, or {sup 252}Cf active interrogation neutron sources. It is used to verify declared fissile mass ({sup 235}U or {sup 239}Pu) present in SNM. Objectives: Calibrate HPGe and AWCC for lightly irradiated (with enough {sup 137}Cs gamma background) ∼93% enriched HEU fuels; Verify fissile mass ({sup 235}U +{sup 239}Pu) content using AWCC and HPGe; Model and benchmark AWCC in MCNP6. Neutron coincidence and multiplicity counting: Two or more neutrons are coincident if they are detected by the system within the specified gate window; In AWCC: Gate window is 128 μsec; Induced fission in fissile material such as {sup 235}U and {sup 239}Pu - emission of time correlated neutrons - Singles, Doubles, Triples, or Quadruples; No induced fission in non-fissile materials- no correlated neutrons - only singles. SNM can be verified with high accuracy and precision using gamma and neutron NDA instruments such as HPGe and AWCC. Interaction with thermal neutrons. Non-fissile atoms - do not emit correlated neutrons. Fissile atoms - emit correlated neutrons during induced fission events. The time correlated neutrons can be detected by using coincidence or multiplicity counters such as AWCC. Likewise, {sup 235}U produces 186 keV gamma peak that can be measured by a HPGe gamma detector. Counts under 186 keV gamma peak provide information about {sup 235}U content. Combining AWCC and HPGe results can provide better understanding of special nuclear material under investigation.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Strategies for Post-Synthetic Functionalization of Mesoporous Carbon Nanomaterial Surfaces

Most widely used carbon-based materials feature a bulk framework tolerant of extreme pH and temperature conditions while maintaining physical robustness, electrical conductivity, and biological relevance due to its inherent nontoxicity. At the nanoscale, the study of porous carbons has been of interest because of the enhanced accessible surface area relative to nonporous analogues. The evolution of synthetic techniques has developed structural allotropes with tunable internal pore diameter averages spanning from sub-nanometer to micron-plus sizes. Within the mesopore range, surface chemical phenomena abide by a kinetic-limited ruleset (ignoring the effects of bulk diffusion, as they do not pertain to this size regime). Further, mesopores provide sufficient volume and surface area for hosting guest species, including metal nanoparticles (MNP), polymers, small organics, and enzymes. These two unique features of mesoporous carbon (MC) drive interest in surface modifications to create new physicochemical functionality to these systems and their hosted species. As a result, the evolution of surface modification techniques has been scattered to disparate niches across the literature. This review compiles the array of elegant methods by which these carbon systems are topically engineered.

functionalization↗

Roadmap on advanced and / real-time characterisation of solid state materials and devices for energy applications

A strong societal and political drive is motivating the development and optimization of novel energy conversion and storage systems for decarbonization. The successful implementation of solid state devices such as fuel cells and secondary batteries depends, however, on achieving ambitious targets in terms of performance, reliability and cost competitiveness. Research and technology are addressing these needs through a holistic approach including exploration of new materials and nanoarchitectures, as well as system engineering. These significant efforts require the support of appropriate characterization tools capable of assessing nanometer-scale phenomena such as concentration profiles of ionic and electronic charges, local chemical compositions and their evolution over time across interfaces. This roadmap provides an overview of selected advanced characterization techniques for energy materials and devices. Specific focus is put on in situ/operando methods for probing electrochemical phenomena in real-time under realistic working conditions. Experts in the field provide an extensive review of the current state of the art in 2025 and the current and future challenges for the characterization of local chemistry and kinetics in the bulk of the material, in nanoarchitectures (e.g. thin films) and at the interfaces (e.g. grain boundaries, phase contacts, solid/liquid and solid/gas interfaces) . The aim is to provide a detailed guide to the techniques, describing opportunities and bottlenecks for their practical deployment and examples of successful applications.

25 ENERGY STORAGE↗

Characterizing mechanical and microstructural properties of novel montmorillonite-rich polyethylene composites

Montmorillonite (MMT) clays are important industrial materials used as catalysts, chemical sorbents and fillers in polymer–clay nanocomposites. The layered structure of these clays has motivated research into further applications of these low-cost materials, including use as ion exchange media and solid-state ionic conductors. In these applications, the mechanical properties of MMT are key when considering long-term, reliable performance. Previous studies have focused on the mechanical properties of nanocomposites with MMT as the minority component or pure MMT thin films. In this work, the microstructure and mechanical properties of pure MMT and majority MMT/polyethylene composites pressed into dense pellets are examined. Characterization methods such as X-ray diffraction, atomic force microscopy and scanning electron microscopy together with nanoindentation reveal important structure–property relationships in the clay-based materials. Here, utilizing these techniques, we have discovered that MMT processing impacts the layered microstructure, chemical stability and, critically, the elastic modulus and hardness of bulk MMT samples. Particularly, the density of the pellets and the ordering of the clay platelets within them strongly influence the elastic modulus and hardness of the pellets. By increasing pressing force or by incorporating secondary components, the density, and therefore mechanical properties, can be increased. If the layered structure of the clay is destroyed by exfoliation, the mechanical properties will be compromised. Understanding these relationships will help guide new studies to engineer mechanically stable MMT-based materials for industrial applications.

36 MATERIALS SCIENCE↗

Direct ink writing of shear exfoliated two-dimensional nanomaterial- elastomeric multifunctional nanocomposite

Direct ink writing (DIW) of polymer nanocomposites with high loadings of two-dimensional (2D) nanofillers (graphene and hexagonal boron nitride (hBN)) is challenging because of potential clogging, use of hazardous solvents, and agglomeration. Here, in this work, a shear exfoliation and sieving method to prepare DIW ink with high loading of nanofillers produced from low-cost bulk layered materials such as graphite and bulk hBN powder for successful DIW printing without the use of any solvents, binders, or plasticizers. The single-step exfoliation technique resulted in a composite with substantial layer reduction along the c-axis, as confirmed by SEM, TEM, XRD, and Raman analysis. Incorporating exfoliated graphene (40 wt%) increased viscosity by ∼6 orders of magnitude due to enhanced particle–matrix interactions, leading to pronounced yield stress behavior and a yield stress of approximately 1598 Pa, which enabled excellent shape retention during extrusion. Using the DIW technique, porous structures such as desalination membranes, self-sensing bone scaffolds, thermal management coating, and serpentine strain sensors were fabricated. When tested in a direct contact membrane distillation setup, the fabricated membrane demonstrated a promising permeate flux of 21.85 Lm −2 h −1 and a salt rejection of 74.3 %. The fabricated serpentine sensor exhibited stable signal variations under cyclic tensile loading, with a working range of 0–200 % strain and a maximum gauge factor of 43,735. A cell culture test using the printed bone scaffold demonstrated promising cell attachment and proliferation. The DIW printed hBN nanocomposite exhibited reversible shape change under heat, demonstrating potential 4D printing capability and efficient thermal management when exposed to high heat or flame.

Desalination↗

Advanced Analysis of X-ray Fluorescence Measurements of the Interfacial Density of Eu Ions at Liquid–Liquid Interfaces for Solvent Back-Extraction

X-ray fluorescence near total reflection (XFNTR) is the primary technique used to measure the element-specific interfacial density of ions at liquid−liquid interfaces. Fluorescence from ions in the bulk liquids can complicate the determination of the interfacial density; consequently, measurements have been previously limited to samples without ions in the upper phase and with concentrations on the order of 10 μM or less in the lower phase. We modify the analysis of XFNTR data to account for ions in both bulk phases, then demonstrate its use in the context of rare-earth separations processes. In a model of ion stripping (i.e., back-extraction), dodecane solutions of di(2-ethylhexyl)- phosphoric acid (HDEHP) loaded with Eu(III) at the 1 mM level are placed in contact with either pure water or aqueous solutions of nitric or citric acid at pH 3. XFNTR measurements of equilibrated, quiescent samples reveal that citric acid solutions produce a disproportionately large depletion of ions from the interface compared to that from the bulk organic solution, whereas stripping by pure water or nitric acid solutions is negligible. As a result, this advance in the methodology of XFNTR may have broad applicability to the investigation of metal ions in chemical and biological processes at liquid−liquid interfaces.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Photocarrier Dynamics in TlGaS 2 Nanoflakes and van der Waals Heterostructures with Hexagonal Boron Nitride and WS 2 Nanoflakes: Implications for Optoelectronic Applications

We present an experimental investigation on photocarrier dynamics in a TlGaS 2 bulk crystal and its heterostructures with hexagonal BN and WS 2 . The samples were obtained by mechanical exfoliation and dry transfer techniques. The photocarrier dynamics was monitored by a transient absorption technique. We observed a direct optical transition of about 555 nm in the TlGaS 2 crystal. By utilizing transient absorption of that transition, we obtained a hot-carrier energy relaxation time of less than 1 ps and a carrier lifetime of about 300 ps in TlGaS 2 at room temperature. In the hexagonal-BN-TlGaS 2 heterostructure, the photocarrier dynamics was similar to that in TlGaS 2 , indicating the type-I band alignment of this structure with both band extremes located in TlGaS 2 . In the monolayer WS 2 -TlGaS 2 heterostructure, we observed charge transfer from TlGaS 2 to WS 2 and an extended lifetime of the transferred carriers in WS 2 . Here, these results introduce TlGaS 2 as a promising layered material for developing two-dimensional van der Waals materials that can be combined with other two-dimensional materials for various optoelectronic devices.

36 MATERIALS SCIENCE↗

Progress in relativistic laser–plasma interaction with kilotesla-level applied magnetic fields

We report on progress in the understanding of the effects of kilotesla-level applied magnetic fields on relativistic laser–plasma interactions. Ongoing advances in magnetic-field–generation techniques enable new and highly desirable phenomena, including magnetic-field–amplification platforms with reversible sign, focusing ion acceleration, and bulk-relativistic plasma heating. Building on recent advancements in laser–plasma interactions with applied magnetic fields, we introduce simple models for evaluating the effects of applied magnetic fields in magnetic-field amplification, sheath-based ion acceleration, and direct laser acceleration. These models indicate the feasibility of observing beneficial magnetic-field effects under experimentally relevant conditions and offer a starting point for future experimental design.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Robust quantification of the diamond nitrogen-vacancy center charge state via photoluminescence spectroscopy

Nitrogen vacancy (NV) centers in diamond are at the heart of many emerging quantum technologies, all of which require control over the NV charge state. Hence, methods for quantification of the relative photoluminescence intensities of the NV 0 and NV − charge states, i.e., a charge state ratio, are vital. Several approaches to quantify NV charge state ratios have been reported but are either limited to bulk-like NV diamond samples or yield qualitative results. We propose an NV charge state quantification protocol based on the determination of sample- and experimental setup-specific NV 0 and NV − reference spectra. The approach employs blue (400–470 nm) and green (480–570 nm) excitation to infer pure NV 0 and NV − spectra, which are then used to quantify NV charge state ratios in subsequent experiments via least squares fitting. We test our dual excitation protocol (DEP) for a bulk diamond NV sample and 20 and 100 nm nanodiamond particles and compare results with those obtained via other commonly used techniques such as zero-phonon line fitting and non-negative matrix factorization. We find that DEP can be employed across different samples and experimental setups and yields consistent and quantitative results for NV charge state ratios that are in agreement with our understanding of NV photophysics. By providing robust NV charge state quantification across sample types and measurement platforms, DEP will support the development of NV-based quantum technologies.

Color center laser spectroscopy↗

Thermal Conductivity Measurement of Extrusion-Printed Silver Using Modulated Photothermal Radiometry

Flexible printed electronics is a rapidly growing field with applications in conformal and flexible devices. However, the physical properties of the films created by many state-of-the-art printing methods become highly dependent on printing parameters, resulting in varying thermal properties often differing significantly from their bulk ink components. To understand the influence of the printing process, we build upon our previous work, where a noncontact optical technique, known as modulated photothermal radiometry (MPTR), was used to measure the thermal conductivity of aerosol-jet-printed thin films. In this work, we use the method to study the thermal properties of extrusion-printed silver on glass and alumina substrates. A noise-resistant data analysis fitting technique is applied using a 2-D heat transfer model. Here, the thermal conductivity measurement is validated using the Weidemann-Franz (WF) relationship from measured electrical conductivity values.

42 ENGINEERING↗