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DOE OSTI2020

Crack nucleation and growth during dynamic indentation of chemically-strengthened glass

Dynamic point impact loading is a primary cause of fracture of glass screens on mobile devices. An improved understanding of crack initiation and evolution under high-speed indentation could contribute to the development of materials with better performance, but experimental observations are challenging due to the short timescales and limited depth-of-field of optical microscopy. To address this need, we have observed fracture of a chemically-strengthened glass during dynamic indentation using in situ x-ray phase-contrast imaging (XPCI). Median cracks initiate below the surface of the glass, at a depth approximately corresponding to the depth at which the surface residual compressive stress diminishes to zero. These cracks initially propagate at ~10ms –1 , rapidly accelerating to > 100ms –1 . We also observe some evidence for rate-dependent behavior, in that indentation at the lowest rates studied here (below about ~0.15ms –1 ) fails to initiate cracks regardless of the depth of the indentation (up to 18μm), while indentation at higher rates produces median cracks that either arrest or cause complete fracture, depending on the depth of indentation.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Analytic model of dislocation density evolution in fcc polycrystals accounting for dislocation generation, storage, and dynamic recovery mechanisms

Here, an analytic model of the evolution of dislocation density in fcc polycrystals is described. The evolution equations approximately account for most known dislocation storage, dynamic recovery, and dislocation generation mechanisms in fcc polycrystals. Specifically, the model incorporates network (forest) and grain boundary storage, mobile-network and mobile–mobile annihilation, screw–screw annihilation via athermal and thermal single cross-slip, generation by double cross-slip (Koehler mechanism, including dipole formation), Frank-Read sources, grain boundary nucleation, and mobile–immobile dislocation nucleation due to shock loading. Single cross-slip is assumed to proceed through the Friedel–Escaig (FE) mechanism; the corresponding activation energy is calculated using a modified FE model. The activation energy for double cross-slip is calculated for the first time by extending the FE model. The exact evolution equations are integro-differential equations, and as such are difficult to implement in a code; hence, the evolution equations are simplified by making several approximations. Preliminary results on copper are presented, including comparisons to experimental data.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Low-energy helium plasma effects on textured micro-porous tungsten

The effects of low-energy helium plasma on surface evolution and restructuring of micro-porous tungsten and tungsten-rhenium micro-engineered materials was experimentally investigated. Tungsten foam samples of 45 and 80 Pores Per Inch (PPI) of three types of textured surface architecture (nodular W, dense Re-pillars, and W-coated Re-pillars) were exposed to low-energy helium plasma at 80 and 200 eV to fluence levels of 1, 2, and 7 x 10 25 m -2 at 1123 K. The sidewalls of Re pillars exhibited surface holes due to trapped helium while their tips were found to form complex nano-scale web structures, 100's of microns across, rather than nano-tendrils (fuzz) that are often observed in flat W samples. A nano-necklace bead/string structure was observed for the first time on Re pillars, likely driven by a high density of nano-meter size helium bubbles crowded near pillar tips. W-coated Re pillars exhibited typical fuzz nanostructures seen on flat and untextured W-foam, albeit much shorter. While the height of W-fuzz was found to depend on the square root of ion fluence, the nano-web height was found to be linearly dependent on ion fluence. The fuzz was found to grow much slower on nodular foams as compared to planar tungsten, by as much as 25% slower in the W-coated Re pillar samples. Weight loss due to ion sputtering was found to be significantly reduced in nodular foam as compared to planar tungsten, but was found to be more pronounced with Re pillars. Surface coverage by nano-webs may provide insulation against plasma disruptions and act as a passive Thermal Protection System (TPS) that may be ablated during severe plasma disruptions, thus protecting the underlying surface. W-pillars or W-coated Re-pillars are found to allow trapped helium to diffuse out of the surface instead of building up sub-surface stress.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Multiscale modeling of fission gas behavior in U 3 Si 2 under LWR conditions

In this work, we present a model of fission gas behavior in U 3 Si 2 under light water reactor (LWR) conditions for application in engineering fuel performance codes. The model includes components for intra-granular and inter-granular behavior of fission gases. The intra-granular component is based on cluster dynamics and computes the evolution of intra-granular fission gas bubbles and swelling coupled to gas diffusion to grain boundaries. The inter-granular component describes the evolution of grain-boundary fission gas bubbles coupled to fission gas release. Given the lack of experimental data for U 3 Si 2 under LWR conditions, the model is informed with parameters calculated via atomistic simulations. In particular, we derive fission gas diffusivities through density functional theory calculations, and the re-solution rate of fission gas atoms from intra-granular bubbles through binary collision approximation calculations. Further, the developed model is applied to the simulation of an experiment for U 3 Si 2 irradiated under LWR conditions available from the literature. Results point out a credible representation of fission gas swelling and release in U 3 Si 2 . Finally, we perform a sensitivity analysis for the various model parameters. Based on the sensitivity analysis, indications are derived that can help in addressing future research on the characterization of the physical parameters relative to fission gas behavior in U 3 Si 2 . The developed model is intended to provide a suitable infrastructure for the engineering scale calculation of fission gas behavior in U 3 Si 2 that exploits a multiscale approach to fill the experimental data gap and can be progressively improved as new lower-length scale calculations and validation data become available.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2018

Microstructure evolution and mechanical properties of Cu/Sn/Ag TLP-bonded joint during thermal aging

Highlights: • The thermal reliability of the Cu/Sn/Ag TLP-bonded joint was investigated through high-temperature storage. • A diffusion reaction occurred at the interface between Cu{sub 3}Sn and Ag{sub 3}Sn during thermal aging. • The mechanism of the Cu{sub 3}Sn/Ag{sub 3}Sn interfacial reaction was investigated from thermodynamics and kinetics. - Abstract: Low-temperature transient liquid phase (TLP) bonding is a promising joining technology for high-temperature electronic devices packaging. However, the effect of thermal aging on the joint microstructure and performance has been rarely studied so far. In this paper, the relationship between microstructural evolution and mechanical property was developed for the Cu/Sn/Ag TLP-bonded joint during 350 °C aging. Experimental results show that an interfacial reaction occurs between the intermetallic compounds (IMCs) of Cu{sub 3}Sn and Ag{sub 3}Sn, which induces that a great amount of Cu{sub 3}Sn particles or wedges embed into the Ag-Sn phase layer. The reaction process is controlled by a volume diffusion of Cu elements from the Cu substrate, and capable of promoting the transformation from Ag{sub 3}Sn into Ag(Sn) solid solution. Cu{sub 41}Sn{sub 11} phase can be formed at the expense of Cu{sub 3}Sn and Cu, of which transformation process is completely achieved after aging for 480 h, and the Cu(Sn) solid solution intimately contacts with the opposite Ag(Sn) solid solution in many areas after aging for 960 h. The joint mechanical property initially declines due to the formation of Cu{sub 41}Sn{sub 11} phase and Cu-Sn IMCs grain coarsening, and then increases because of the complete depletion of Cu{sub 3}Sn and substantial precipitation of Cu(Sn) solid solution. After aging for nearly 1000 h, the joint still maintains a high shear strength of >40 MPa, indicating an excellent thermal reliability.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Numerical Analysis of Experiments on Thermally Induced Dissociation of Methane Hydrates in Porous Media

Numerical simulation is essential for the prediction and evaluation of hydrocarbon reservoir performance. Numerical simulators developed for the description of the behavior of hydrates under production and the corresponding flow of fluids and heat accounting for all known processes are powerful, but they need validation through comparison to field or experimental data in order to instill confidence in their predictions. In this study, we analyze by means of numerical simulation the results of an experiment of methane hydrate dissociation by thermal stimulation in unconsolidated porous media heated through the vessel walls. The physics captured by the model include multicomponent heat and mass transfer, multiphase flow through porous media, and the phase behavior of the CH 4 + H 2 O system involved in methane hydrate formation and dissociation. The set of governing equations consists of the mass and energy conservation equations coupled with constitutive relationships, i.e., the dissolution of gas in H 2 O, relative permeability and capillary pressure models, composite thermal conductivity models, and methane hydrate phase equilibria. The model geometry describes accurately the hydrate reactor used in a recent experimental study investigating methane hydrate dissociation behavior [Chong et. al. Appl. Energy 2016, 177, 409-421]. The cumulative gas production is estimated and validated against three tests of experimental data involving different boundary temperatures, showing a good agreement between observations and numerical predictions. The predicted evolution of the spatial distributions of different phases over time shows that hydrate dissociation progresses inward from the reactor boundary to the center, methane gas accumulates to the top of the reactor because of buoyancy, and water migrates down to the bottom of the reactor because of gravity. A sharp hydrate dissociation front is predicted, and the estimated location of hydrate dissociation front suggests a linear relationship with the square root of time. A sensitivity analysis on the thermal conductivity of sand under fully saturated conditions is conducted to elucidate its effect on the gas production behavior. In addition, the energy efficiency ratio computed from the simulation of this boundary-wall heating technique varies from 14.0 to 16.2. Deviations between observations and predictions of the evolution of the temperature profile are attributed to initial heterogeneous distribution of the hydrate phase in the hydrate reactor.

42 ENGINEERING↗

DOE OSTI2016

Complexation and phase evolution at dimethylformamide-Ag(111) interfaces

The interaction of solvent molecules with metallic surfaces impacts many interfacial chemical processes. We investigate the chemical and structure evolution that follows adsorption of the polar solvent dimethylformamide (DMF) on Ag(111). An Ag(DMF) 2 coordination complex forms spontaneously by DMF etching of Ag(111), yielding mixed films of the complexes and DMF. Utilizing ultrahigh vacuum scanning tunneling microscopy (UHV-STM), in combination with X-ray photoelectron spectroscopy (XPS) and density functional theory (DFT) computations, we map monolayer phases from the 2-D gas regime, consisting of a binary mixture of DMF and Ag(DMF) 2 , through the saturation monolayer limit, in which these two chemical species phase separate into ordered islands. Structural models for the near-square DMF phase and the chain-like Ag(DMF) 2 phase are presented and supported by DFT computation. Interface evolution is summarized in a surface pressure-composition phase diagram, which allows structure prediction over arbitrary experimental conditions. In conclusion, this work reveals new surface coordination chemistry for an important electrolyte-electrode system, and illustrates how surface pressure can be used to tune monolayer phases.

2-D phases↗

DOE OSTI2022

Step-by-step state-selective tracking of fragmentation dynamics of water dications by momentum imaging

Abstract The double photoionization of a molecule by one photon ejects two electrons and typically creates an unstable dication. Observing the subsequent fragmentation products in coincidence can reveal a surprisingly detailed picture of the dynamics. Determining the time evolution and quantum mechanical states involved leads to deeper understanding of molecular dynamics. Here in a combined experimental and theoretical study, we unambiguously separate the sequential breakup via D + + OD + intermediates, from other processes leading to the same D + + D + + O final products of double ionization of water by a single photon. Moreover, we experimentally identify, separate, and follow step by step, two pathways involving the b 1 Σ + and a 1 Δ electronic states of the intermediate OD + ion. Our classical trajectory calculations on the relevant potential energy surfaces reproduce well the measured data and, combined with the experiment, enable the determination of the internal energy and angular momentum distribution of the OD + intermediate.

74 ATOMIC AND MOLECULAR PHYSICS↗

DOE OSTI2014

Orbit-based analysis of resonant excitations of Alfvén waves in tokamaks

The exponential growth phase of fast-ion-driven Alfvénic instabilities is simulated and the resonant wave-particle interactions are analyzed numerically. The simulations are carried out in realistic magnetic geometry and with a realistic particle distribution for a JT-60U plasma driven by negative-ion-based neutral beams. In order to deal with the large magnetic drifts of the fast ions, two new mapping methods are developed and applied. The first mapping yields the radii and pitch angles at the points, where the unperturbed orbit of a particle intersects the mid-plane. These canonical coordinates allow to express analysis results (e.g., drive profiles and resonance widths) in a form that is easy to understand and directly comparable to the radial mode structure. The second mapping yields the structure of the wave field along the particle trajectory. This allows us to unify resonance conditions for trapped and passing particles, determine which harmonics are driven, and which orders of the resonance are involved. This orbit-based resonance analysis (ORA) method is applied to fast-ion-driven instabilities with toroidal mode numbers n = 1-3. After determining the order and width of each resonance, the kinetic compression of resonant particles and the effect of linear resonance overlap are examined. On the basis of the ORA results, implications for the fully nonlinear regime, for the long-time evolution of the system in the presence of a fast ion source, and for the interpretation of experimental observations are discussed.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2015

Cavitation inception by the backscattering of pressure waves from a bubble interface

The secondary cavitation that occurs by the backscattering of focused ultrasound from a primary cavitation bubble caused by the negative pressure part of the ultrasound (Maxwell, et al., 2011) might be useful for the energy exchange due to bubble oscillations in High Intensity Focused Ultrasound (HIFU). The present study is concerned with the cavitation inception by the backscattering of ultrasound from a bubble. In the present experiment, a laser-induced bubble which is generated by a pulsed focused laser beam with high intensity is utilized as a primary cavitation bubble. After generating the bubble, focused ultrasound is emitted to the bubble. The acoustic field and the bubble motion are observed with a high-speed video camera. It is confirmed that the secondary cavitation bubble clouds are generated by the backscattering from the laser-induced bubble. The growth of cavitation bubble clouds is analyzed with the image processing method. The experimental results show that the height and width of the bubble clouds grow in stepwise during their evolution. The direct numerical simulations are also conducted for the backscattering of incident pressure waves from a bubble in order to evaluate a pressure field near the bubble. It is shown that the ratio of a bubble collapse time t{sub 0} to a characteristic time of wave propagation t{sub S}, η = t{sub 0}/t{sub s}, is an important determinant for generating negative pressure region by backscattering. The minimum pressure location by the backscattering in simulations is in good agreement with the experiment.

42 ENGINEERING↗

DOE OSTI2018

Late-time mixing and turbulent behavior in high-energy-density shear experiments at high Atwood numbers

The LANL Shear Campaign uses millimeter-scale initially solid shock tubes on the National Ignition Facility to conduct high-energy-density hydrodynamic plasma experiments, capable of reaching energy densities exceeding 100 kJ/cm3. These shock-tube experiments have for the first time reproduced spontaneously emergent coherent structures due to shear-based fluid instabilities [i.e., Kelvin-Helmholtz (KH)], demonstrating hydrodynamic scaling over 8 orders of magnitude in time and velocity. The KH vortices, referred to as “rollers,” and the secondary instabilities, referred to as “ribs,” are used to understand the turbulent kinetic energy contained in the system. Their evolution is used to understand the transition to turbulence and that transition's dependence on initial conditions. Experimental results from these studies are well modeled by the RAGE (Radiation Adaptive Grid Eulerian) hydro-code using the Besnard-Harlow-Rauenzahn turbulent mix model. Information inferred from both the experimental data and the mix model allows us to demonstrate that the specific Turbulent Kinetic Energy (sTKE) in the layer, as calculated from the plan-view structure data, is consistent with the mixing width growth and the RAGE simulations of sTKE.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2023

Tuning the band topology of GdSb by epitaxial strain

Rare-earth monopnictide (RE-V) semimetal crystals subjected to hydrostatic pressure have shown interesting trends in magnetoresistance, magnetic ordering, and superconductivity, with theory predicting pressure-induced band inversion. Yet, thus far, there have been no direct experimental reports of interchanged band order in RE-Vs due to strain. This work studies the evolution of band topology in biaxially strained GdSb(001) epitaxial films using angle-resolved photoemission spectroscopy (ARPES) and density functional theory (DFT). As biaxial strain is tuned from tensile to compressive strain, the gap between the hole and the electron bands dispersed along [001] decreases. The conduction and valence band shifts seen in DFT and ARPES measurements are explained by a tight-binding model that accounts for the orbital symmetry of each band. Finally, we discuss the effect of biaxial strain on carrier compensation and magnetic ordering temperature.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Core formation and core composition from coupled geochemical and geophysical constraints

The formation of Earth’s core left behind geophysical and geochemical signatures in both the core and mantle that remain to this day. Seismology requires that the core be lighter than pure iron and therefore must contain light elements, and the geochemistry of mantle-derived rocks reveals extensive siderophile element depletion and fractionation. Both features are inherited from metal–silicate differentiation in primitive Earth and depend upon the nature of physiochemical conditions that prevailed during core formation. To date, core formation models have only attempted to address the evolution of core and mantle compositional signatures separately, rather than seeking a joint solution. Here we combine experimental petrology, geochemistry, mineral physics and seismology to constrain a range of core formation conditions that satisfy both constraints. We find that core formation occurred in a hot (liquidus) yet moderately deep magma ocean not exceeding 1,800 km depth, under redox conditions more oxidized than present-day Earth. This new scenario, at odds with the current belief that core formation occurred under reducing conditions, proposes that Earth’s magma ocean started oxidized and has become reduced through time, by oxygen incorporation into the core. As a result, this core formation model produces a core that contains 2.7–5% oxygen along with 2–3.6% silicon, with densities and velocities in accord with radial seismic models, and leaves behind a silicate mantle that matches the observed mantle abundances of nickel, cobalt, chromium, and vanadium.

58 GEOSCIENCES↗

DOE OSTI2020

An atom probe tomography and inventory calculation examination of second phase precipitates in neutron irradiated single crystal tungsten

Tungsten is the prime candidate material for the plasma facing divertor system and first wall armor of future nuclear fusion reactors. However, the understanding of the microstructural and chemical evolution of pure tungsten under neutron irradiation is relatively unknown, in part due to a lack of experimental data on this topic. Here, single crystal tungsten has been irradiated in the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory at a nominal temperature of 700–800 °C to damage levels of 0.1 and 1.8 displacements per atom (dpa). Inventory calculations of the neutron irradiation experiments have been used to track isotope generation and decay to inform atom probe tomography (APT) results in the determination of the transmutation-induced precipitate compositions. Furthermore, APT crystallography has been used to show the relationship between precipitates and matrix. The composition of the precipitates is shown to progress towards that of the σ-phase at the highest dose studied, with those precipitates lying along crystallographic planes similar to those of displacement-induced dislocations. This work also sets the framework for APT studies of materials that contain isotopic ratios far from those observed in the natural state.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2017

Helium, hydrogen, and fuzz in plasma-facing materials

Tungsten, the primary material under consideration as the divertor material in magnetic-confinement nuclear fusion reactors, has been known for the last decade to form 'fuzz'—a layer of microscopic, high-void-fraction features on the surface—after only a few hours of exposure to helium plasma. Fuzz has also been observed in molybdenum, tantalum, and several other metals. Helium bubbles in tungsten and other metals are also known to change the hardness of the surface, accumulate at grain boundaries and dislocations, and increase hydrogen isotope retention. Further, this article reviews helium- and hydrogen-induced surface evolution, including fuzz formation, in tungsten and other plasma-facing materials, as well as modeling and experimental efforts that have been undertaken to understand the mechanisms of fuzz formation, helium and hydrogen transport in plasma-facing materials, and relevant atomic-scale and electronic effects relevant to plasma-facing materials.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Influence of conical wire array geometry on plasma flow and temperature profiles of radiatively cooled jets

The influence of conical wire array geometry on the formation and dynamics of pulsed-power driven plasma jets is investigated. In the experiments, the jet becomes isolated from the inflows as it passes through an aperture, allowing the study of its intrinsic evolution for different conical angles. Here, our results show that, regardless of the array opening angle, the jets are supersonic, highly collisional, and exhibit an exponential axial density decay with a characteristic scale length of 𝐿 𝑛 ≈ 3 mm, significantly shorter than the overall length of the jet. In contrast, axial velocity systematically increases with larger array opening angles. The near invariance of the density profile is attributed to a compensating mechanism between geometric divergence and axial acceleration, consistent with an asymptotically steady flow regime. Additionally, temperature measurements reveal ion-electron thermal decoupling near the base of the jet, with equilibration downstream. Analysis of radiative cooling and collisional energy exchange timescales indicates that the plasma evolves in a radiatively stable regime and that the two-temperature profile is fully described by the competition between both methods. These findings provide valuable information into the internal structure and evolution of pulsed-power plasma jets in regimes dominated by geometric shaping and radiative cooling, demonstrating experimental control over flow acceleration and collimation relevant to both laboratory and astrophysical contexts.

Physics - Plasma physics↗

DOE OSTI2019

Development of a Host-Based Intrusion Detection and Control Device for Industrial Field Control Devices

Industrial control systems contain a multitude of devices deployed into the field to observe and control a physical process. Currently, most of these devices lack common host-based cybersecurity features, which can lead them to be seen as vulnerable targets. The Cymbiote device was developed to address this problem by examining multiple streams of data to determine what might indicate a potential threat, and to evaluate and execute appropriate response actions. This paper discusses the evolution of the Cymbiote device in response to evaluation and testing done on real-world hardware. Experimental results are discussed, as are the new developments that have been made to the device in response to the findings. In addition, we describe future research directions for this approach along with the experimental setup changes in response to the requirements for statistical rigor.

Rice, Theora R.↗

DOE OSTI2016

Stability and Activity of (Pr 1‐x Nd x ) 2 NiO 4 as Cathodes for Solid Oxide Fuel Cells: I. Quantification of Phase Evolution in Pr 2 NiO 4

Praseodymium nickelate (Pr 2 NiO 4 ) is an active oxygen electrode for solid oxide fuel cells, but undergoes phase transition at elevated temperatures (e.g., 750°C). Quantification of this phase evolution in an operating single cell is challenging because of the overlap of X‐ray diffraction ( XRD ) peaks between the cathode and oxide current collector. In this work, we replace the oxide current collector with a gold metal grid, circumventing these challenges by allowing the exposure of the cathode to the X‐ray beam, while eliminating peak overlap. Quantification of the phase evolution was performed by a least‐squares fitting of the linear combination of XRD standards against the experimental patterns. Energy‐dispersive spectroscopy analysis on long‐term operated cells showed the absence of reactions between the gold grids and the cathodes. Additionally, the grids exhibited excellent mechanical stability under operating conditions and enabled similar cell performance as an oxide current collector.

Dogdibegovic, Emir↗