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At least 163 records · Page 9

Development of graphite/copper composites utilizing engineered interfaces

In situ measurements of graphite/copper alloy contact angles were made using the sessile drop method. The interfacial energy values obtained from these measurements were then applied to a model for the fiber matrix interfacial debonding phenomenon found in graphite/copper composites. The formation obtained from the sessile drop tests led to the development of a copper alloy that suitably wets graphite. Characterization of graphite/copper alloy interfaces subjected to elevated temperatures was conducted using Scanning Electron Microscopy, Energy Dispersive Spectroscopy, Auger Electron Spectroscopy, and X Ray Diffraction analyses. These analyses indicated that during sessile drop tests conducted at 1130 C for 1 hour, copper alloys containing greater than 0.98 at pct chromium form continuous reaction layers of approx. 10 microns in thickness. The reaction layers are adherent to the graphite surface. The copper wets the reaction layer to form a contact angle of 60 deg or less. X ray diffraction results indicate that the reaction layer is Cr3C2.

Devincent, Sandra M.↗

Brazing of Carbon Carbon Composites to Cu-clad Molybdenum for Thermal Management Applications

Advanced carbon carbon composites were joined to copper-clad molybdenum (Cu/Mo) using four active metal brazes containing Ti (Cu ABA, Cusin-1 ABA, Ticuni, and Ticusil) for potential use in thermal management applications. The brazed joints were characterized using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and Knoop microhardness measurements across the joint region. Metallurgically sound C-C/Cu/Mo joints, devoid of interfacial cracks formed in all cases. The joint interfaces were preferentially enriched in Ti, with Cu ABA joints exhibiting the largest interfacial Ti concentrations. The microhardness measurements revealed hardness gradients across the joint region, with a peak hardness of 300-350 KHN in Cusin-1 ABA and Ticusil joints and 200-250 KHN in Cu ABA and Ticuni joints, respectively.

Singh, M.↗

On Stability and Electrochemical Performance of 316 Stainless Steel in Wastewater: Implications for Resource Recovery

Electrochemical nutrient recovery systems rely on stable electrode materials capable of operating in chemically complex wastewater environments. We investigated corrosion resistance and interfacial electrochemical behavior of 316 stainless steel (SS316) in a synthetic wastewater matrix representative of centrate streams, a key knowledge gap in electrochemical phosphorus recovery. A comprehensive suite of electrochemical techniques (chronoamperometry, cyclic voltammetry, potentiodynamic polarization, and electrochemical impedance spectroscopy (EIS)) and surface characterization methods (scanning electron microscopy, X-ray diffraction) were employed. Results revealed that wastewater containing typical ionic constituents (such as PO 4 3- , NH 4 + , and divalent cations) exhibited enhanced cathodic activity and the formation of a more stable, protective surface film on SS316 that mitigated chloride-induced corrosion. In contrast, SS316 in the NaCl solution showed significant susceptibility to passive layer breakdown and localized corrosion. Time-resolved EIS further confirmed improved interfacial stability and restricted charge transfer in WW over time, in stark contrast to the progressive passive layer degradation in NaCl. Surface analyses corroborated these findings, showing limited surface attack in WW compared to distinct localized corrosion features in NaCl. These findings indicate that competing ionic species in WW effectively mitigate chloride aggressiveness, enhance SS316 stability, and demonstrate improved electrode longevity and reliability for sustainable wastewater-based electrochemical phosphorus recovery applications.

36 MATERIALS SCIENCE↗

Fatigue characterization of advanced carbon-carbon composites

Response of quasi-isotropic laminates of SiC coated Carbon-Carbon (C/C) composites under flexural fatigue are investigated at room temperature. Virgin as well as mission cycled specimens are tested to study the effects of thermal and pressure cycling on the fatigue performance of C/C. Tests were conducted in three point bending with a stress ratio of 0.2 and frequency of 1 Hz. Fatigue strength of C/C has been found to be considerably high - approximately above 85 percent of the ultimate flexural strength. The fatigue strength appears to be decreasing with the increase in the number of mission cycling of the specimens. This lower strength with the mission cycled specimens is attributed to the loss of interfacial bond strength due to thermal and pressure cycling of the material. C/C is also found to be highly sensitive to the applied stress level during cyclic loading, and this sensitivity is observed to increase with the mission cycling. Weibull characterization on the fatigue data has been performed, and the wide scatter in the Weibull distribution is discussed. Fractured as well as untested specimens were C-scanned, and the progressive damage growth during fatigue is presented.

Mahfuz, Hassan↗

Heterogeneous Multilayer Nanopores via Chemically Tuned Dielectric Breakdown for Single‐Molecule Sensing

Solid-state nanopores are powerful platforms for single-molecule sensing, yet their performance is often constrained by fabrication complexity, noise, and limited control over surface properties. Here we report a direct method to fabricate heterogeneous multilayer nanopores using chemically tuned controlled dielectric breakdown (CT-CDB). We integrate hBN, MoS 2 , or graphene atop a silicon nitride membrane to form five distinct bilayer and tri-layer architectures, with bare SiN x nanopore as a control. CT-CDB achieves pore formation reproducibly through material-stacks with high efficiency, good pore size control, and strong yield, validated by various characterizations. Transferrin protein translocation experiments, supported by simulations, reveal that multilayer configurations modulate protein conformations, ionic current blockade and dwell time distributions, reflecting combined effects of membrane type, interfacial chemistry, and local electric field gradients. A supervised machine learning framework is implemented to assist identifying multilayer structure effects embedded in signal signatures, with over 96% accuracy. This work presents a modular and scalable framework for functional nanopore engineering with complex structural integration, thereby expanding the potential of 2D materials in single-molecule sensing applications.

2D materials↗

A critical study of the role of the surface oxide layer in titanium bonding

Scanning electron microscope/X-ray photoelectron spectroscopy (SEM/XPS) analysis of fractured adhesively bonded Ti 6-4 samples is discussed. The text adhesives incuded NR 056X polyimide, polypheylquinoxaline (PPQ), and LARC-13 polyimide. Differentiation between cohesive and interfacial failure was based on the absence of presence of a Ti 2p XPS photopeak. In addition, the surface oxide layer on Ti-(6A1-4V) adherends is characterized and bond strength and durability are addressed. Bond durability in various environmental conditions is discussed.

Dias, S.↗

Onset of Convection Due to Surface Tension Variations in Multicomponent and Binary Fluid Layers

Under certain conditions, such as in thin liquid films or microgravity, surface tension variations along a free surface can induce convection. Convection onset due to surface tension variation is important to many terrestrial technological processes in addition to microgravity materials processing applications. Examples include coating, drying crystallization, solidification, liquid surface contamination, and containerless processing. In double-diffusive and multicomponent systems, the spatial variations of surface tension are associated with two or more stratifying agencies, respectively. For example, both temperature and species (concentration) gradients are associated with convection in the solidification of binary alloys or salt ponds. The direction of the two (or more) gradients has a profound effect on the nature of the flow at or slightly beyond the onset of convection. Our recent work at the NASA Lewis Research Center focused on characterizing surface-tension-induced onset of convection, often referred to as Marangoni-Benard convection. Exact solutions for the stationary neutral stability of multicomponent fluid layers with interfacial deformation were derived. These solutions also permit the computation of a boundary curve that separates the long and finite wavelength instabilities. Computing points along this boundary using the exact solution (when possible) is more efficient than the typical numerical approaches, such as finite difference or spectral methods. Above the curve, a long wavelength instability was predicted, suggesting that convection would occur principally through one large flow cell in the layer, whereas below the curve, finite wavelength instabilities occur which suggest multiple finite-sized circulation cells. For many common liquids with layer depths greater than 100 mm, finite wave instability is predicted under terrestrial conditions; however, with little exception, long wavelength instability is predicted in microgravity for the identical fluid systems.

Skarda, J. Raymond Lee↗

Determination of plate wave velocities and diffuse field decay rates with braod-band acousto-ultrasonic signals

Lowest symmetric and lowest antisymmetric plate wave modes were excited and identified in broad-band acousto-ultrasonic (AU) signals collected from various high temperature composite materials. Group velocities have been determined for these nearly nondispersive modes. An algorithm has been developed and applied to determine phase velocities and hence dispersion curves for the frequency ranges of the broad-band pulses. It is demonstrated that these data are sensitive to changes in the various stiffness moduli of the materials, in agreement by analogy, with the theoretical and experimental results of Tang and Henneke on fiber reinforced polymers. Diffuse field decay rates have been determined in the same specimen geometries and AU configuration as for the plate wave measurements. These decay rates are of value in assessing degradation such as matrix cracking in ceramic matrix composites. In addition, we verify that diffuse field decay rates respond to fiber/matrix interfacial shear strength and density in ceramic matrix composites. This work shows that velocity/stiffness and decay rate measurements can be obtained in the same set of AU experiments for characterizing materials and in specimens with geometries useful for mechanical measurements.

Kautz, Harold E.↗

The Surface-Topography Challenge: A Multi-Laboratory Benchmark Study to Advance the Characterization of Topography

Surface performance is critically influenced by topography in virtually all real-world applications. The current standard practice is to describe topography using one of a few industry-standard parameters. The most commonly reported number is Ra, the average absolute deviation of the height from the mean line (at some, not necessarily known or specified, lateral length scale). However, other parameters, particularly those that are scale-dependent, influence surface and interfacial properties; for example the local surface slope is critical for visual appearance, friction, and wear. The present Surface-Topography Challenge was launched to raise awareness for the need of a multi-scale description, but also to assess the reliability of different metrology techniques. In the resulting international collaborative effort, 153 scientists and engineers from 64 research groups and companies across 20 countries characterized statistically equivalent samples from two different surfaces: a “rough” and a “smooth” surface. The results of the 2088 measurements constitute the most comprehensive surface description ever compiled. We find wide disagreement across measurements and techniques when the lateral scale of the measurement is ignored. Consensus is established through scale-dependent parameters while removing data that violates an established resolution criterion and deviates from the majority measurements at each length scale. Our findings suggest best practices for characterizing and specifying topography. The public release of the accumulated data and presented analyses enables global reuse for further scientific investigation and benchmarking.

42 ENGINEERING↗

The mechanism of hydroxyapatite coatings degradation at high substrate temperatures

Physical vapor deposition methods used for hydroxyapatite (HA) coatings typically require elevated substrate temperatures and post-deposition annealing to induce crystallization. However, such thermal treatments can degrade both the mechanical integrity and bioactivity of the coating, particularly when substrate temperatures exceed 500 °C. The mechanisms underlying these phenomena remain insufficiently understood. In this study, HA thin films were deposited on silicon and Ti6Al4V substrates using pulsed laser deposition and were systematically characterized to elucidate these mechanisms. XPS and SIMS analyses revealed a temperature-dependent loss of OH − and PO 4 3− groups, an increased Ca/P ratio, and the formation of interfacial oxides, all of which contribute to weakened adhesion. To clarify the temperature-dependent decline in bioactivity, protein adsorption behavior was analyzed using a Kramers-type kinetic framework; the fitted desorption kinetics indicate that coatings deposited near ∼500 °C provide the most stable protein attachment, whereas higher temperatures accelerate desorption due to dehydroxylation and carbonate substitution. Together, these findings provide mechanistic insight into the thermal degradation of HA coatings and offer a framework for optimizing deposition parameters to preserve stoichiometry, adhesion, and bioactivity for long-term biomedical applications.

Kylychbekov, Salizhan [Univ. of Oxford (United Kin↗

Rheo–Electric Foundations and Engineering of Carbon Slurry Flow Electrodes

Flowable carbon slurry electrodes promise continuous, scalable electrochemical desalination and energy storage when their rheology (flow and stability) and electronic connectivity are jointly optimized. This report integrates six complementary thrusts that we executed under the Laboratory Directed Research and Development (LDRD) project: (i) a fast, ex situ, centrifuge-compatible method to quantify pellet (packed slurry) electronic conductivity, with a validated cell constant (“shape factor”) and quantitative structure–property insights for carbon mixtures; (ii) a controlled circulation study showing that peristaltic pumping can irreversibly alter particle size and morphology over laboratory-relevant durations; (iii) development of a miniature jet pump that preserves particle integrity while achieving entrainment ratios of 2–4 at practical flow rates; (iv) a comprehensive mapping of how a representative non-ionic surfactant (Tween 20) collapses the carbon gel network, separating network-percolation losses from intrinsic particle contact resistance; (v) in-situ visualization revealing how gravitational settling and flow-driven mixing compete to control charge transport, with dynamic bed layers preventing saturation while achieving 30-fold local concentration enhancement; and (vi) a simple, widely adoptable fabrication route to structured, gas-nitrided titanium nitride (TiN) titanium current collectors that dramatically lower interfacial losses and enable geometry-driven performance gains. Together, these results provide a coherent toolchain and design rules to accelerate formulation screening, de-risk device prototyping, and standardize characterization for carbon slurry electrodes in flow-electrode capacitive deionization (FCDI), electrochemical flow capacitor (EFC), and related systems.

25 ENERGY STORAGE↗

Damage development in titanium metal matrix composites subjected to cyclic loading

Several layups of SCS-6/Ti-15-3 composites were investigated. Fatigue tests were conducted and analyzed for both notched and unnotched specimens at room temperature and elevated temperatures. Thermo-mechanical fatigue results were analyzed. Test results indicated that the stress in the 0 degree fibers is the controlling factor in fatigue life. The static and fatigue strength of these materials is shown to be strongly dependent on the level of residual stresses and the fiber/matrix interfacial strength. Fatigue tests of notched specimens showed that cracks can initiate and grow many fiber spacings in the matrix materials without breaking fibers. Fiber bridging models were applied to characterize the crack growth behavior. The matrix cracks are shown to significantly reduce the residual strength of notched composites. The notch strength of these composites was accurately predicted using a micromechanics based methodology.

Johnson, W. S.↗

Damage development in titanium metal-matrix composites subjected to cyclic loading

Several layups of SCS-6/Ti-15-3 composites were investigated. Fatigue tests were conducted and analyzed for both notched and unnotched specimens at room temperature and elevated temperatures. Thermo-mechanical fatigue results were analyzed. Test results indicated that the stress in the 0 degree fibers is the controlling factor in fatigue life. The static and fatigue strength of these materials is shown to be strongly dependent on the level of residual stresses and the fiber/matrix interfacial strength. Fatigue tests of notched specimens showed that cracks can initiate and grow many fiber spacings in the matrix materials without breaking fibers. Fiber bridging models were applied to characterize the crack growth behavior. The matrix cracks are shown to significantly reduce the residual strength of notched composites. The notch strength of these composites was accurately predicted using a micromechanics based methodology.

Johnson, W. S.↗

A Eulerian three-fluid flow framework for the study of fuel dispersal behavior under loss-of-coolant accident conditions

As the nuclear industry explores new fuel designs to accommodate increased burnup, studying fuel behavior during loss-of-coolant accidents is essential for ensuring the safe operation of light-water reactors. Here, this study presents a computational model to simulate the intricate three-phase flow dynamics of fuel dispersal following cladding breach, where solid fuel particles and carrier fission gases interact with the surrounding liquid or gas medium. The model utilizes a Eulerian three-fluid framework to depict the phase interaction within interpenetrating continua, treating fragmented fuel as granular material. Closure relationships for bulk-flow properties of the solid phase and detailed interfacial exchange terms in high-temperature, high-speed gas-solid-liquid flow scenarios are proposed. The model was validated using adiabatic experimental results in the literature, focusing on characterizing fuel dispersal behavior during loss-of-coolant accidents conditions. Settlement characteristics of the solids, quantified by the probability distribution of equivalent particles, closely matched probability density functions reported in experimental studies. Key highlights of this study include the theoretical description of a coupled three-phase flow with phase change, interpretation of the high-pressure boundary conditions and insights into the transient behavior of gas-solid-liquid phase dynamics during a simulated high-speed dispersal event.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Water-stable direct air capture of CO 2 with microcapsules of task-specific ionic liquid and their electrothermal regeneration

Microcapsules of the task specific ionic liquid (TSIL) 1-ethyl-3-methylimidazolium 2-cyanopyrrolide [EMIM][2CNpyr] with composite polydimethylsiloxane (PDMS) shells were fabricated for use in CO 2 direct air capture (DAC) conditions. The TSIL was encapsulated using an oil-in-oil emulsion as a templating procedure through two different approaches. In the first approach, a PDMS-polyurea (PU) shell was constructed by interfacial polymerization, while in the second approach, a graphene oxide (GO)-PDMS shell was constructed by cross-linking GO sheets. The composition and structure of both capsule types were fully characterized, and their CO 2 DAC performance was evaluated by gravimetric and breakthrough analysis. Both capsules exhibited competitive capacities, with the PDMS-PU capsules and the GO-PDMS capsules reaching 0.75 mol kg −1 and 0.66 mol kg −1 , respectively. We further demonstrate that both capsule systems can be regenerated with complementary electrothermal methods. Microwave (MW) regeneration was used for the PDMS-PU capsules, effectively releasing absorbed CO 2 in less than an hour. Owing to the electrical conductivity of GO, GO-PDMS capsules were regenerated via radio frequency heating (RF). This work highlights the importance and opportunity of tuning solid–liquid composite performance for advanced applications, including direct air capture of carbon dioxide.

Al-Mahbobi, Luma [Texas A&M University, College St↗

Pd/CeO2/SiC Chemical Sensors

The incorporation of nanostructured interfacial layers of CeO2 has been proposed to enhance the performances of Pd/SiC Schottky diodes used to sense hydrogen and hydrocarbons at high temperatures. If successful, this development could prove beneficial in numerous applications in which there are requirements to sense hydrogen and hydrocarbons at high temperatures: examples include monitoring of exhaust gases from engines and detecting fires. Sensitivity and thermal stability are major considerations affecting the development of high-temperature chemical sensors. In the case of a metal/SiC Schottky diode for a number of metals, the SiC becomes more chemically active in the presence of the thin metal film on the SiC surface at high temperature. This increase in chemical reactivity causes changes in chemical composition and structure of the metal/SiC interface. The practical effect of the changes is to alter the electronic and other properties of the device in such a manner as to degrade its performance as a chemical sensor. To delay or prevent these changes, it is necessary to limit operation to a temperature <450 C for these sensor structures. The present proposal to incorporate interfacial CeO2 films is based partly on the observation that nanostructured materials in general have potentially useful electrical properties, including an ability to enhance the transfer of electrons. In particular, nanostructured CeO2, that is CeO2 with nanosized grains, has shown promise for incorporation into hightemperature electronic devices. Nanostructured CeO2 films can be formed on SiC and have been shown to exhibit high thermal stability on SiC, characterized by the ability to withstand temperatures somewhat greater than 700 C for limited times. The exchanges of oxygen between CeO2 and SiC prevent the formation of carbon and other chemical species that are unfavorable for operation of a SiC-based Schottky diode as a chemical sensor. Consequently, it is anticipated that in a Pd/CeO2/SiC Schottky diode, the nanostructured interfacial CeO2 layer would contribute to thermal stability and, by contributing to transfer of electrons, would also contribute to sensitivity.

Lu, Weijie↗

Studies of the nature of interfacial barriers in high efficiency crystalline silicon solar cells

The effects of interfacial barriers in crystalline silicon solar cells were studied. The effort was directed toward the investigation and use of such techniques as Angular Resolved Parameter Spectroscopy (ARAPS) and Impedance Spectroscopy in initially characterizing n-type Si doped to levels commonly used for n+p solar cells, and eventually Si solar cells. The objectives of the research are given. Those accomplished are detailed, as are recommendations for future work.

Bates, Clayton W., Jr.↗

Multi-stage load partitioning in additively manufactured Al6061+TiC nanocomposite characterized by in-situ neutron diffraction

Metal matrix composites (MMCs), combining metal matrix and ceramic particles, exhibit high mechanical strength and stiffness compared to conventional metallic materials. During fusion-based additive manufacturing (AM), MMCs undergo a rapid heating and cooling thermal history, which affects the interfacial bonding, thermal misfit stress and mechanical load transfer behavior between the metal matrix and particles, thus impacting the bulk mechanical performance. Here, we investigate the deformation dynamics and phase-specific load transfer in fusion-based AMed Al6061 +TiC MMCs through in-situ neutron diffraction. By calculating the phase-specific lattice strains, a multi-stage load transfer and deformation behavior during uniaxial compression is revealed: (1) elastic deformation in Stage I for both phases; (2) sudden stress rebalance between two phases in Stage II, evidenced by a sudden decrease in Al lattice strain and increase in TiC; (3) active load carrying by both phases in Stage III, with both phases experiencing an increase in lattice strains. Further, the deformation mechanism of each stage is deducted by correlating the evolutions of the interphase stresses and peaks’ broadening and intensity of the Al matrix. The local plastic deformation of the Al matrix near the phase interface is triggered and leads to stress rebalancing in Stage II. The global plastic deformation subsequently propagates throughout the Al matrix in Stage III, and the composite is further hardened through both dislocation multiplication and load transfer. The findings offer valuable insights into deformation and load-sharing behavior in AMed MMCs.

36 MATERIALS SCIENCE↗