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DOE OSTI2021

In Situ Formation of Polycyclic Aromatic Hydrocarbons as an Artificial Hybrid Layer for Lithium Metal Anodes

Nonuniform Li deposition causes dendrites and low Coulombic efficiency (CE), seriously hindering the practical applications of Li metal. Herein, we developed an artificial solid-state interphase (SEI) with planar polycyclic aromatic hydrocarbons (PAHs) on the surface of Li metal anodes by a facile in situ formation technology. The resultant dihydroxyviolanthron (DHV) layers serve as the protective layer to stabilize the SEI. In addition, the oxygen-containing functional groups in the soft and conformal SEI film can regulate the diffusion and transport of Li ions to homogenize the deposition of Li metal. The artificial SEI significantly improves the CEs and shows superior cyclability of over 1000 h at 4 mAh cm –2 . The LiFePO 4 /Li cell (2.8 mAh cm –2 ) enables a long cyclability for 300 cycles and high CEs of 99.8%. Furthermore, this work offers a new strategy to inhibit Li dendrite growth and enlightens the design on stable SEI for metal anodes.

25 ENERGY STORAGE↗

DOE OSTI2020

Boundary-directed epitaxy of block copolymers

Directed self-assembly of block copolymers (BCPs) enables nanofabrication at sub-10 nm dimensions, beyond the resolution of conventional lithography. However, directing the position, orientation, and long-range lateral order of BCP domains to produce technologicallyuseful patterns is a challenge. Here, we present a promising approach to direct assembly using spatial boundaries between planar, low-resolution regions on a surface with different composition. Pairs of boundaries are formed at the edges of isolated stripes on a background substrate. Vertical lamellae nucleate at and are pinned by chemical contrast at each stripe/ substrate boundary, align parallel to boundaries, selectively propagate from boundaries into stripe interiors (whereas horizontal lamellae form on the background), and register to wide stripes to multiply the feature density. Ordered BCP line arrays with half-pitch of 6.4 nm are demonstrated on stripes >80 nm wide. Boundary-directed epitaxy provides an attractive path towards assembling, creating, and lithographically defining materials on sub-10 nm scales.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Dielectric metasurfaces made from vertically oriented nanoresonators

Dielectric metasurfaces control optical wavefronts via nanoscale resonators laid out across a surface. However, most metasurfaces are, by design, planar. In this work, we demonstrate the ability to fabricate dielectric metasurfaces with vertically oriented dielectric resonators using membrane projection lithography. We first numerically characterize the resonant modes of an array of vertically oriented germanium ellipses with no substrate and identify a narrowband region where the resonators satisfy the first Kerker condition. We then fabricate seven metasurfaces by depositing germanium ellipses onto walls of a 3D micrometer-sized silicon nitride photonic scaffold and characterize their transmission. We find that signatures of the multipolar modes seen in the unsupported array persist in the supported array, but the overall behavior is more complicated due to the scaffold. Further, we show that for a conceptual metasurface containing two coupled, vertically oriented ellipses, the ellipses can generate a sharp resonance with a quality factor of 240.

Gennaro, Sylvain D. (ORCID:0000000222090831)↗

DOE OSTI2022

Micropillar Compression of Additively Manufactured 316L Stainless Steels after 2 MeV Proton Irradiation: A Comparison Study between Planar and Cross-Sectional Micropillars

A micropillar compression study with two different techniques was performed on proton-irradiated additively manufactured (AM) 316L stainless steels. The sample was irradiated at 360 °C using 2 MeV protons to 1.8 average displacement per atom (dpa) in the near-surface region. A comparison study with mechanical test and microstructure characterization was made between planar and cross-sectional pillars prepared from the irradiated surface. While a 2 MeV proton irradiation creates a relatively flat damage zone up to 12 µm, the dpa gradient by a factor of 2 leads to significant dpa uncertainty along the pillar height direction for the conventional planar technique. Cross-sectional pillars can significantly reduce such dpa uncertainty. From one single sample, three cross-sectional pillars were able to show dpa-dependent hardening. Furthermore, post-compression transmission electron microscopy allows the determination of the deformation mechanism of individual micropillars. Cross-sectional micropillar compression can be used to study radiation-induced mechanical property changes with better resolution and less data fluctuation.

transmission electron microscopy↗

DOE OSTI2022

Lithium extraction composite for recovery of lithium from brines, and process of using said composition

A lithium extraction composite comprising: (i) a porous support and (ii) particles of a lithium-selective sorbent material coated on at least one surface of the support, wherein the support has a planar membrane, fiber (or rod), or tubular shape. A method for extracting and recovering a lithium salt from an aqueous solution by use of the above-described composition is also described, the method comprising (a) flowing the aqueous source solution through a first zone or over a first surface of the lithium extraction composite to result in selective lithium intercalation in the lithium-selective sorbent material in the first zone or first surface; and (b) simultaneously recovering lithium salt extracted in step (a) from said lithium-selective sorbent material by flowing an aqueous stripping solution through a second zone or over a second surface of the lithium extraction composite in which lithium ions from the first zone or first surface diffuse.

Bhave, Ramesh R.↗

DOE OSTI2025

Toward Verification of RANS Simulations of the T-Tube Modular Divertor Using Large Eddy Simulations of Impinging Turbulent Plane Jets

Turbulent impinging jets have been proposed to cool high heat flux plasma-facing components such as the solid tungsten target plates of the divertor in long-pulse magnetic fusion energy reactors. In particular, the T-tube modular divertor, originally developed by the ARIES Team, consists of two concentric cylindrical tubes where helium flows through a slot in the inner tube, forming an approximately planar jet that impinges upon and cools the inner surface of the pressure boundary (namely, the outer tube) and the ~15-cm 2 plasma-facing W target. The objective of this work is to demonstrate that large eddy simulations (LESs) accurately simulate the thermal transport in canonical flows that comprise the cooling flow in the T-tube, as well as validate temperatures from LES with experimental measurements in a simplified T-tube geometry. Wall‑resolved LESs, validated by experimental data and verified by direct numerical simulations (DNSs), provide benchmark data for two canonical flows in the T‑tube, namely, planar impinging and wall jets, for Reynolds numbers Re B = 4 × 10 3 to 2 × 10 4 . Our LES results are within 4% to 12% root-mean-square error (RMSE) of surface Nusselt number distributions (Nu) from experiments and DNSs. The validated LES results are then used as the ground truth to evaluate four Reynolds‑averaged Navier-Stokes (RANS) turbulence closures, namely, the k‑ω SST, realizable k‑ε, GEKO, and γ‑SST models. The k‑ω SST model has the best overall performance in terms of heat transfer, giving surface Nu within 12% RMSE of the LES results for high‑ReB impinging jets and reduced overprediction in the wall‑jet region. The GEKO model with default constants has the next best performance, providing slightly better Nu predictions for low ReB impinging jets (versus k-ω SST) but worse overall performance over the full range of ReB studied here. The realizable k‑ε turbulence model significantly overestimates turbulence near the stagnation point, while the γ‑SST model suppresses near‑wall production, biasing the simulations toward simulating laminar surface heat transfer. Simulations of the simplified T‑tube show that LES and RANS simulations with the k‑ω SST model give nearly identical average heat transfer coefficients (HTCs) over the impingement surface. The realizable k‑ε model predicts significantly lower wall temperatures due to overestimation of HTC in the outlet flow.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2023

High-speed mapping of surface charge dynamics using sparse scanning Kelvin probe force microscopy

Unraveling local dynamic charge processes is vital for progress in diverse fields, from microelectronics to energy storage. This relies on the ability to map charge carrier motion across multiple length- and timescales and understanding how these processes interact with the inherent material heterogeneities. Towards addressing this challenge, we introduce high-speed sparse scanning Kelvin probe force microscopy, which combines sparse scanning and image reconstruction. This approach is shown to enable sub-second imaging (>3 frames per second) of nanoscale charge dynamics, representing several orders of magnitude improvement over traditional Kelvin probe force microscopy imaging rates. Bridging this improved spatiotemporal resolution with macroscale device measurements, we successfully visualize electrochemically mediated diffusion of mobile surface ions on a LaAlO 3 /SrTiO 3 planar device. Such processes are known to impact band-alignment and charge-transfer dynamics at these heterointerfaces. Furthermore, we monitor the diffusion of oxygen vacancies at the single grain level in polycrystalline TiO 2 . Through temperature-dependent measurements, we identify a charge diffusion activation energy of 0.18 eV, in good agreement with previously reported values and confirmed by DFT calculations. Together, these findings highlight the effectiveness and versatility of our method in understanding ionic charge carrier motion in microelectronics or nanoscale material systems.

25 ENERGY STORAGE↗

DOE OSTI2020

Investigation of the electrical conduction mechanisms in P-type amorphous germanium electrical contacts for germanium detectors in searching for rare-event physics

For the first time, electrical conduction mechanisms in the disordered material system is experimentally studied for p-type amorphous germanium (a-Ge) used for high-purity Ge detector contacts. The localization length and the hopping parameters in a-Ge are determined using the surface leakage current measured from three high-purity planar Ge detectors. The temperature dependent hopping distance and hopping energy are obtained for a-Ge fabricated as the electrical contact materials for high-purity Ge planar detectors. As a result, we find that the hopping energy in a-Ge increases as temperature increases while the hopping distance in a-Ge decreases as temperature increases. The localization length of a-Ge is on the order of 2.13$^{-0.05}_{+0.07}$A° to 5.07$^{0.83}_{+2.58}$A°,depending on the density of states near the Fermi energy level within bandgap. Using these parameters, we predict that the surface leakage current from a Ge detector with a-Ge contacts can be much smaller than one yocto amp (yA) at helium temperature, suitable for rare-event physics searches.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2021

The reflection of a blast wave by a very intense explosion

We demonstrate that the geometric similarity of Taylor’s blast wave persists beyond reflection from an ideal surface. Upon impacting the surface, the spherical symmetry of the blast wave is lost but its cylindrical symmetry endures. As the flow acquires dependence on a second spatial dimension, an analytic solution of the Euler equations becomes elusive. However, the preservation of axisymmetry, geometric similarity and planar symmetry in the presence of a mirror-like surface causes all flow solutions to collapse when scaled by the height of burst (HOB) and the shock arrival time at the surface. The scaled blast volume for any yield, HOB and ambient air density follows a single universal trajectory for all scaled time, both before and after reflection.

45 MILITARY TECHNOLOGY, WEAPONRY, AND NATIONAL DEF↗

DOE OSTI2025

Surface and sub-surface porosity effects on the initial free surface expansion in shocked single crystal aluminum

Defects and roughness at a material’s surface can allow for the formation of a material jet when a shockwave reaches a surface. The formation of a jet can lead to significant material damage of the shocked material, as well as the downstream material that the jet impacts. Here, we utilize planar shocks in single crystal aluminum to assess initial jetting formation for surface notches and sub-surface porosity. In the case of surface notches, we find that changing the width of the notch can cause the shock breakout response to transition from a standard jetting mechanism to an atomic atomization at high velocities. This transition occurs due to the mechanisms associated with lateral relaxations within the notch and how this interacts with the shock focusing event that induces jetting. For sub-surface pores, the pore collapse induces a re-shock, localized near the pore, that is stronger than the initial shock, but unsupported. Changing the pore dimensions and location relative to the surface influences the strength of the shock that emanates from its collapse when it reaches the surface, leading to a variety of different breakout conditions including jetting and localized material failure.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Squeezing a Prism into a Surface: Emulating Bulk Optics with Achromatic Metasurfaces

Metasurfaces promise to replace bulky prisms and lenses with 2D surfaces, revolutionizing wavefront control with technologically significant advantages in size, weight, and planar fabrication. However, conventional implementations suffer from large chromatic aberrations and cannot sustain performance over practical bandwidths of real-world signals because of the limited phase modulation margin available in a surface. How can an infinitely thin surface generate the arbitrarily large, broadband phase delay that bulk phase accumulation can provide? Here, equivalence between bulk optics and certain multiresonant metasurfaces is demonstrated, where phase delay arises from trains of multiple resonances in the effective sheet conductivities of the surface itself instead of accumulation of propagation phase. The fundamentally required electromagnetic surface conductivities of a purely achromatic metasurface are derived and general design rules for arbitrarily broadband beam steering and lensing are obtained. Both operation in transmission and reflection can be achieved in a unified way by proper alignment of the resonances, enabling 360° directionality. The arbitrary spectral bandwidth, dual reflection/transmission operation, and complete dispensability of propagation phase constitute a major advance in the state of the art of achromatic metasurfaces for wavefront manipulation.

36 MATERIALS SCIENCE↗

DOE OSTI2024

A Techno-Economic Analysis of a 50MWth Light-Trapping Cavity-Planar Solar Receiver Tower Capital Expenditures and its Cost Mitigation Strategies

To maximize thermal efficiency, the National Renewable Energy Laboratory (NREL) has proposed a light-trapping cavity-planar receiver design intended to capture energy from reradiating surfaces. This system implements a macroscale light trapping mechanism induced by panels with triangular channels, this mechanism allows for elevated temperatures on the receiver panels and in turn the temperature of the HTF; using this design coupled with the implementation of a fluidized particle flow as the HTF, it can be expected for some components to reach a peak working temperature of nearly 1000 degrees C cyclically throughout each day-night cycle. While these temperatures correlate to higher efficiency of the CSP tower they also demand intense thermomechanical properties from the materials used to make the receiver panels. In this analysis, we will list our assumptions to provide clarity on the significance of our calculation. This cost analysis will be conducted using a combination of both case study data and surveying industry to determine costs that are relevant to the current market trends. This analysis represents an early attempt to establish the Capital Expenditures required for a CSP tower of such design to determine the feasibility of implementing such a system in the industry.

concentrated solar power (CSP)↗

DOE OSTI2021

Broadband 2DES detection of vibrational coherence in the S x state of canthaxanthin

The nonadiabatic mechanism that mediates nonradiative decay of the bright S 2 state to the dark S 1 state of carotenoids involves population of a bridging intermediate state, S x , in several examples. The nature of S x remains to be determined definitively, but it has been recently suggested that S x corresponds to conformationally distorted molecules evolving along out-of-plane coordinates of the isoprenoid backbone near a low barrier between planar and distorted conformations on the S 2 potential surface. Here, the electronic and vibrational dynamics accompanying the formation of S x in toluene solutions of the ketocarotenoid canthaxanthin (CAN) are characterized with broadband two-dimensional electronic spectroscopy (2DES) with 7.8 fs excitation pulses and detection of the linear polarization components of the third-order nonlinear optical signal. A stimulated-emission cross peak in the 2DES spectrum accompanies the formation of S x in <20 fs following excitation of the main absorption band. S x is prepared instantaneously, however, with excitation of hot-band transitions associated with distorted conformations of CAN’s isoprenoid backbone in the low frequency onset of the main absorption band. Vibrational coherence oscillation maps and modulated anisotropy transients show that S x undergoes displacements from the Franck–Condon S 2 state along out-of-plane coordinates as it passes to the S 1 state. The results are consistent with the conclusion that CAN’s carbonyl-substituted β-ionone rings impart an intramolecular charge-transfer character that frictionally slows the passage from S x to S 1 compared to carotenoids lacking carbonyl substitution. Despite the longer lifetime, the S 1 state of CAN is formed with retention of vibrational coherence after passing through a conical intersection seam with the S x state.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Visualizing Size-Dependent Dynamics of CeO 2-δ {100}-Supported CoO x Nanoparticles Under CO 2 Hydrogenation Conditions

Carbon dioxide is a major greenhouse gas. In order to optimize processes focused on its chemical valorization, one needs detailed information about the effects of CO 2 and/or CO 2 /H 2 mixtures on the structure and morphology of metal/oxide catalysts. Here, in this study, the evolution of a catalyst with cobalt supported on CeO 2 -cube nanostructures under CO 2 hydrogenation conditions was investigated by using a set of in situ characterization techniques (X-ray absorption fine structure, X-ray diffraction, diffuse reflectance infrared Fourier transform spectroscopy, and environmental transmission electron microscopy (TEM)). The {100} facets of the ceria support displayed an unexpectedly high stability due to strong interactions with the aggregates of cobalt oxide. A significant influence of interfacial bonding between CoO x and CeO 2-δ {100} is evident through a clear preference in the orientation of CoO x nanoparticles (NPs) with respect to the substrate. For initially reduced Co/CeO 2 -cube nanostructures, a kinetically controlled oxidation of cobalt upon the introduction of CO 2 was observed during the early stages of CO 2 hydrogenation. Environmental TEM revealed the size-dependent morphological behavior of cobalt oxide NPs due to strong interactions with the CeO 2 {100} surface. When the environment was switched from H 2 to a mixture of H 2 and CO 2 at 250 °C, small CoO x NPs (in the largest dimension < 2.5 nm) rapidly transformed from a pyramidal three-dimensional (3D) form to a planar, monatomic layer attached to the concurrently oxidized CeO 2-δ {100} surface. This maximizes the number of sites available for the binding of CO 2 or reaction intermediates. The shape transformation reflected the oxophilic character of cobalt and strong metal–support interactions. The removal of CO 2 from the gas phase led to a reduction of the cobalt oxide NPs by hydrogen and a reversible two-dimensional → 3D transformation. In contrast, no significant morphological changes, apart from further oxidation, were observed for big CoO x NPs (in the largest dimension > 3 nm). These trends are not seen for nanoparticles of noble metals. The observed morphological and structural changes in the small CoO x NPs affected the stability of reaction intermediates and modified the selectivity of the CoO x /CeO 2 catalyst system for methane production.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Induction heating cells with controllable thermal expansion of bladders and methods of using thereof

Disclosed herein are induction heating cells and methods of using these cells for processing. An induction heating cell may be used for processing (e.g., consolidating and/or curing a composite layup having a non-planar portion. The induction heating cell comprises a caul, configured to position over and conform to this non-planar portion. Furthermore, the cell comprises a mandrel, configured to position over the caul and force the caul again the surface of the feature. The CTE of the caul may be closer to the CTE of the composite layup than to the CTE of the mandrel. As such, the caul isolates the composite layup from the dimensional changes of the mandrel, driven by temperature fluctuations. At the same time, the caul may conform to the surface of the mandrel, which can be used to define the shape and transfer pressure to the non-planar portion.

42 ENGINEERING↗

DOE OSTI2021

Induction heating cells with cauls over mandrels methods of using thereof

Matsen, Marc R.↗

DOE OSTI2024

Off-axis and nonplanar slicing

Traditionally, slicing processes have assumed a horizontal plane that moves up the Z axis to produce layers. However, through relatively straightforward modifications, this process can be extended to allow planar slicing at any angle and along any axis in a process referred to as off-axis slicing. Additionally, more advanced pathing solutions are moving away from planar approaches entirely by printing directly on non-flat surfaces. Both of these alternative approaches to slicing, as well as some common issues associated with them, are discussed in this chapter to provide a foundation for more advanced pathing solutions.

Borish, Michael↗

DOE OSTI2025

Curvature Induced Modifications of Chirality and Magnetic Configuration in Perpendicular Films

Designing curvature in three-dimensional (3D) magnetic nanostructures enables controlled manipulation of local energy landscapes, allowing for the modification of noncollinear spin textures relevant for next-generation spintronic devices. In this study, we experimentally investigate 3D magnetization textures in a Co/Pd multilayer film, exhibiting strong perpendicular magnetic anisotropy (PMA), deposited onto curved Cu nanowire meshes with diameters as small as 50 nm and lengths of several microns. Utilizing magnetic soft X-ray nanotomography, we achieve reconstructions of 3D magnetic domain patterns at approximately 30 nm spatial resolution. This approach provides detailed information on both the orientation and magnitude of magnetization within the film. Our results reveal that interfacial anisotropy in the Co/Pd multilayers drives the magnetization toward the local surface normal. In contrast to typical labyrinth domains observed in planar films, the presence of curved nanowires significantly alters the domain structure, with domains preferentially aligning along the nanowire axis in close proximity, while adopting random orientations farther away. We report direct experimental observation of a curvature-induced Dzyaloshinskii-Moriya interaction (DMI), which is quantified to be approximately one-third of the intrinsic DMI in Co/Pd stacks. The curvature induced DMI enhances stability of Néel-type domain walls. These experimental observations are further supported by micromagnetic simulations. Altogether, our findings demonstrate that introducing curvature into magnetic nanostructures provides a powerful strategy for tailoring complex magnetic behaviors, paving the way for the design of advanced 3D racetrack memory and neuromorphic computing devices.

Raftrey, David↗