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DOE OSTI2025

AC electrical transport detection of magnetic properties of small, granular, and heterogeneous samples

Experimental constraints and sample limitations can preclude ideal measurements of electrical transport properties of materials. In such situations, AC electrical transport methods are often employed due to a significant increase in signal-to-noise ratio they can provide. However, dynamic effects that are not often accounted for may be present that may modify the signals in these measurements. In particular, dynamic filtering effects are prominent in small, granular, and heterogeneous materials. We demonstrate that a lock-in amplifier based circuit can distinguish between these DC transport and AC filtering effects. Here, we further demonstrate that this filtering can reveal distinct signatures of magnetic transitions while providing a measure of sample quality.

47 OTHER INSTRUMENTATION↗

DOE OSTI2022

Structured illumination with thermal imaging (SI-TI): A dynamically reconfigurable metrology for parallelized thermal transport characterization

The recent push for the “materials by design” paradigm requires synergistic integration of scalable computation, synthesis, and characterization. Among these, techniques for efficient measurement of thermal transport can be a bottleneck limiting the experimental database size, especially for diverse materials with a range of roughness, porosity, and anisotropy. Traditional contact thermal measurements have challenges with throughput and the lack of spatially resolvable property mapping, while non-contact pump-probe laser methods generally need mirror smooth sample surfaces and also require serial raster scanning to achieve property mapping. Here, we present structured illumination with thermal imaging (SI-TI), a new thermal characterization tool based on parallelized all-optical heating and thermometry. Experiments on representative dense and porous bulk materials as well as a 3D printed thermoelectric thick film (~50 μm) demonstrate that SI-TI (1) enables paralleled measurement of multiple regions and samples without raster scanning; (2) can dynamically adjust the heating pattern purely in software, to optimize the measurement sensitivity in different directions for anisotropic materials; and (3) can tolerate rough (~3 μm) and scratched sample surfaces. Here, this work highlights a new avenue in adaptivity and throughput for thermal characterization of diverse materials.

42 ENGINEERING↗

DOE OSTI2020

Determining plasmonic hot-carrier energy distributions via single-molecule transport measurements

Hot carriers in plasmonic nanostructures, generated via plasmon decay, play key roles in applications such as photocatalysis and in photodetectors that circumvent bandgap limitations. However, direct experimental quantification of steady-state energy distributions of hot carriers in nanostructures has so far been lacking. We present transport measurements from single-molecule junctions, created by trapping suitably chosen single molecules between an ultrathin gold film supporting surface plasmon polaritons and a scanning probe tip, that can provide quantification of plasmonic hot-carrier distributions. Our results show that Landau damping is the dominant physical mechanism of hot-carrier generation in nanoscale systems with strong confinement. The technique developed in this work will enable quantification of plasmonic hot-carrier distributions in nanophotonic and plasmonic devices.

Science & Technology - Other Topics↗

DOE OSTI2023

Remarkable heat conduction mediated by non-equilibrium phonon polaritons

Surface waves can lead to intriguing transport phenomena. In particular, surface phonon polaritons (SPhPs), which result from coupling between infrared light and optical phonons, have been predicted to contribute to heat conduction along polar thin films and nanowires. However, experimental efforts so far suggest only very limited SPhP contributions. Through systematic measurements of thermal transport along the same 3C-SiC nanowires with and without a gold coating on the end(s) that serves to launch SPhPs, here we show that thermally excited SPhPs can substantially enhance the thermal conductivity of the uncoated portion of these wires. The extracted pre-decay SPhP thermal conductance is more than two orders of magnitude higher than the Landauer limit predicted on the basis of equilibrium Bose–Einstein distributions. Here, we attribute the notable SPhP conductance to the efficient launching of non-equilibrium SPhPs from the gold-coated portion into the uncoated SiC nanowires, which is strongly supported by the observation that the SPhP-mediated thermal conductivity is proportional to the length of the gold coating(s). The reported discoveries open the door for modulating energy transport in solids by introducing SPhPs, which can effectively counteract the classical size effect in many technologically important films and improve the design of solid-state devices.

42 ENGINEERING↗

DOE OSTI2023

Magnetic flux trapping in hydrogen-rich high-temperature superconductors

Recent discoveries of superconductivity in various hydrides at high pressures have shown that a critical temperature of superconductivity can reach near-room-temperature values. However, experimental studies are limited by high-pressure conditions, and electrical transport measurements have been the primary technique for detecting superconductivity in hydrides. Here we implement a non-conventional protocol for the magnetic measurements of superconductors in a SQUID magnetometer and probe the trapped magnetic flux in two near-room-temperature superconductors H 3 S and LaH 10 at high pressures. Contrary to traditional magnetic susceptibility measurements, the magnetic response from the trapped flux is almost unaffected by the background signal of the diamond anvil cell due to the absence of external magnetic fields. The behaviour of the trapped flux generated under zero-field-cooled and field-cooled conditions proves the existence of superconductivity in these materials. We reveal that the absence of a pronounced Meissner effect is associated with the very strong pinning of vortices inside the samples. This approach can also be a tool for studying multiphase samples or samples that have a low superconducting fraction at ambient pressure.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Numerical Study of Mineral Nucleation and Growth on a Substrate

We report nucleation and growth processes of minerals and other crystals can significantly affect one another due to the transport limitations and local depletion of reactive ions in the solution. Most numerical models and experimental measurements have typically focused on either growth or nucleation, but not both. In this work, we incorporate a heterogeneous nucleation process based on classical nucleation theory into a microcontinuum model that implements the Darcy–Brinkman–Stokes approach to study the interplay between nucleation and crystal growth on a substrate in diffusive systems. We demonstrate how the Damköhler number (reaction rate) and nucleation rate prefactor change the effective nucleation rate on a substrate. Higher surface growth rates deplete the solute concentration around the nuclei that appear initially on the substrate, creating islands that screen against further nucleation. The model predicts that measured nucleation rates may be affected by the history of crystal nucleation on the substrate. In the extreme case of high growth rates relative to diffusion, it predicts that the rate of subsequent nucleation is limited by reactant depletion. We introduce a nondimensional number α to represent the relation between surface propagation rate during growth and the heterogeneous nucleation rate. We show that it is important to control Damköhler number and α to achieve similar precipitation regimes at different reaction and nucleation rates. We suggest that the observed universality can guide the interpretation of experimental results on nucleation rates, since matching experiment can be achieved by tuning transport, reaction, and nucleation parameters simultaneously. In addition, we show how the bulk solution concentration affects the structure and topology of precipitation on a substrate.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Application of Machine Learning Algorithms to Identify Problematic Nuclear Data

In this work we aim to show that Machine learning algorithms are promising tools for the identification of nuclear data that contribute to increased errors in transport simulations. We demonstrate this through an application of a machine learning algorithm (Random Forest) to the Whisper/MCNP6 criticality validation library to identify nuclear data that are associated with an increase of the bias (simulated - experimental $k_{eff}$) in the calculations. Specifically, the $k_{eff}$ sensitivity profiles (w.r.t. nuclear data) of 233 U solution benchmarks are used to predict the bias and Shapley Additive Explanations (SHAP) are used to explain how the sensitivities are related to the predicted bias. The SHAP values can be interpreted as sensitivity coefficients of the machine learning model to the $k_{eff}$ sensitivities which are used to make predictions of bias. Using the SHAP values we can identify specific subsets of nuclear data which have the highest probability of influencing bias. We demonstrate the utility of this method by showing how SHAP values were used to identify an inconsistency in the 19 F inelastic scattering nuclear data. The methodology presented here is not limited to transport problems and can be applied to other simulations if there are experimental measurements to compare against, simulations of those experimental measurements, and the ability to calculate sensitivities of the model output with respect to the data inputs.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2021

Membrane hydrophobicity determines the activation free energy of passive lipid transport

The collective behavior of lipids with diverse chemical and physical features determines a membrane's thermodynamic properties. Yet, the influence of lipid physicochemical properties on lipid dynamics, in particular interbilayer transport, remains underexplored. Here, we systematically investigate how the activation free energy of passive lipid transport depends on lipid chemistry and membrane phase. Through all-atom molecular dynamics simulations of 11 chemically distinct glycerophospholipids, we determine how lipid acyl chain length, unsaturation, and headgroup influence the free energy barriers for two elementary steps of lipid transport: lipid desorption, which is rate limiting, and lipid insertion into a membrane. Consistent with previous experimental measurements, we find that lipids with longer, saturated acyl chains have increased activation free energies compared to lipids with shorter, unsaturated chains. Lipids with different headgroups exhibit a range of activation free energies; however, no clear trend based solely on chemical structure can be identified, mirroring difficulties in the interpretation of previous experimental results. Compared to liquid-crystalline phase membranes, gel phase membranes exhibit substantially increased free energy barriers. Overall, we find that the activation free energy depends on a lipid's local hydrophobic environment in a membrane and that the free energy barrier for lipid insertion depends on a membrane's interfacial hydrophobicity. Both of these properties can be altered through changes in lipid acyl chain length, lipid headgroup, and membrane phase. Thus, the rate of lipid transport can be tuned through subtle changes in local membrane composition and order, suggesting an unappreciated role for nanoscale membrane domains in regulating cellular lipid dynamics.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2022

Magnetic field screening in hydrogen-rich high-temperature superconductors

In the last few years, the superconducting transition temperature, T c , of hydrogen-rich compounds has increased dramatically, and is now approaching room temperature. However, the pressures at which these materials are stable exceed one million atmospheres and limit the number of available experimental studies. Superconductivity in hydrides has been primarily explored by electrical transport measurements, whereas magnetic properties, one of the most important characteristic of a superconductor, have not been satisfactory defined. Here, we develop SQUID magnetometry under extreme high-pressure conditions and report characteristic superconducting parameters for Im-3m-H 3 S and Fm-3m-LaH 10 —the representative members of two families of high-temperature superconducting hydrides. We determine a lower critical field H c1 of ~0.82 T and ~0.55 T, and a London penetration depth λ L of ~20 nm and ~30 nm in H 3 S and LaH 10 , respectively. The small values of λ L indicate a high superfluid density in both hydrides. These compounds have the values of the Ginzburg-Landau parameter κ ~12–20 and belong to the group of “moderate” type II superconductors, rather than being hard superconductors as would be intuitively expected from their high T c s.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2023

Moisture-driven CO 2 pump for direct air capture

Direct Air Capture, the chemical separation of carbon dioxide (CO 2 ) from air, is considered a necessary approach to generate negative carbon emissions and in turn limit global warming, though energetic and monetary costs must continue to decline to meet the needed gigaton scale. The promise of energy-efficient and continuous carbon dioxide membrane separation has only recently been investigated with the development of facilitated chemical transport and novel electrochemically driven methods. This work demonstrates the potential for continuous pumping of CO 2 from air using commercial anion exchange membranes driven solely by a water vapor gradient. A reactive transport model that couples ionic transport with moisture sensitive bicarbonate chemistry in charged polymers, also termed moisture swing sorption, was developed alongside experimentally measured equilibrium and transport properties of CO 2 and water vapor in Fumasep FAA-3 to determine the mass transport limits of such a system. The results show that the commercial membrane is kinetically limited by the moisture sensitive chemistry, enabling a CO 2 current of 1.1 μmol/m 2 • s. In diffusion limited materials, a CO 2 pumping flux can reach 11 μmol/m 2 • s in and peak performance is expected with a dry air relative humidity around 50% pumping into a saturated water vapor permeate. In all configurations, water loss becomes the major cost in such a separation and must be managed through optimal polymer design or water recovery mechanisms. The work demonstrates the applicability of a new driving force, the evaporation of water, to meet the energetic demand of CO 2 separation from air.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Tritium Transport Phenomena in Molten-Salt Reactors: Molten Salt Tritium Transport Experiment Design

Tritium is produced from neutron interactions with both lithium and beryllium. Large quantities of tritium are generated in Molten Salt Reactors (MSRs) which use LiF/BeF2 (FLiBe) as the fuel salt. Tritium is unique among the radionuclide hazards as it readily permeates through metal structural materials at high temperatures. All metal surfaces are potential release paths for tritium. For adequate safety analysis and eventual licensing of new reactors, predictive models for tritium transport and release from MSRs must be developed. These models must account for the multiple transport phenomena involved with tritium: fuel salt phase mass transport, dissociation/recombination reactions on metal surfaces, interstitial diffusion through the metal structure, and salt or gas phase mass transport in the downstream fluid. These models also must also be validated with representative experiments. Our previous report outlined tritium transport phenomena involved in MSRs, made suggestions on gaps in the transport dataset, and proposed an experimental test stand to test combined transport effects – tritium transport through pipe walls in a convective salt flow. In this report, we summarize an updated analysis framework for tritium transport in MSRs, report our results on hydrogen and deuterium permeation through Hastelloy N, and describe the final design of the Molten Salt Tritium Transport Experiment (MSTTE, pronounced “misty”). The MSRE provides the only wholistic experimental data set for tritium transport in MSRs and understanding the transport phenomena involved in the MSRE is crucial for future model development. One set of parameters in our analysis framework was unknown for the MSRE—surface reaction rates for tritium on Hastelloy N. This warranted our hydrogen and deuterium permeation campaign to assess the permeability, diffusivity, and solubility of hydrogen isotopes in clean Hastelloy N. Surface reaction rate constants were probed by low pressure measurements, however, no surface effects were observed in the limits of our permeation apparatus. Permeation experiments on oxidized Hastelloy N were not performed for this report but are planned in future work. The experimental test stand, MSTTE, measures combined transport properties of the salt-metal system. MSTTE is a forced convection FLiBe loop with custom designed test section to measure tritium transport through candidate structural materials. We use MSRE relevant dimensionless numbers to design and scale the test section. Hastelloy N is a candidate loop and test section material due to the relevance for the MSRE and related designs, however, other metals are being considered (e.g. 316H SS) which may better align with current vendor concepts.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2022

Thermal transport properties and some hydrodynamic-like behavior in three-dimensional topological semimetal $\mathrm{ZrTe}_5$

We report hydrodynamic fluidity in condensed matter physics has been experimentally demonstrated only in a limited number of compounds due to the stringent conditions that must be met. Herein, we performed thermal and electrical transport experiments in three-dimensional topological semimetal ZrTe 5 . By measuring the thermal properties in a wide temperature range, two representative experimental evidences of the hydrodynamics are observed in temperature window between the ballistic and diffusive regimes: a faster evolution of the thermal conductivity than in the ballistic regime and the non-monotonic temperature-dependent effective quasiparticle mean-free-path. In addition, magneto-thermal conductivity results indicate that charged quasiparticles, as well as phonons, may also play an important role in this hydrodynamic-like flow in ZrTe 5 .

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Mass Transport Limitations and Kinetic Consequences of Corn Stover Deacetylation

Alkaline pretreatment of herbaceous feedstocks such as corn stover prior to mechanical refining and enzymatic saccharification improves downstream sugar yields by removing acetyl moieties from hemicellulose. However, the relationship between transport phenomena and deacetylation kinetics is virtually unknown for such feedstocks and this pretreatment process. Here, we report the development of an experimentally validated reaction–diffusion model for the deacetylation of corn stover. A tissue-specific transport model is used to estimate transport-independent kinetic rate constants for the reactive extraction of acetate, hemicellulose and lignin from corn stover under representative alkaline conditions (5–7 g L -1 NaOH, 10 wt% solids loadings) and at low to mild temperatures (4–70°C) selected to attenuate individual component extraction rates under differential kinetic regimes. The underlying transport model is based on microstructural characteristics of corn stover derived from statistically meaningful geometric particle and pore measurements. These physical descriptors are incorporated into distinct particle models of the three major anatomical fractions (cobs, husks and stalks) alongside an unsorted, aggregate corn stover particle, capturing average Feret lengths of 917–1239 μm and length-to-width aspect ratios of 1.8–2.9 for this highly heterogeneous feedstock. Individual reaction–diffusion models and their resulting particle model ensembles are used to validate and predict anatomically-specific and bulk feedstock performance under kinetic-controlled vs. diffusion-controlled regimes. In general, deacetylation kinetics and mass transfer processes are predicted to compete on similar time and length scales, emphasizing the significance of intraparticle transport phenomena. Critically, we predict that typical corn stover particles as small as ~2.3 mm in length are entirely diffusion-limited for acetate extraction, with experimental effectiveness factors calculated to be 0.50 for such processes. Debilitatingly low effectiveness factors of 0.021–0.054 are uncovered for cobs—implying that intraparticle mass transfer resistances may impair observable kinetic measurements of this anatomical fraction by up to 98%. These first-reported quantitative maps of reaction vs. diffusion control link fundamental insights into corn stover anatomy, biopolymer composition, practical size reduction thresholds and their kinetic consequences. These results offer a guidepost for industrial deacetylation reactor design, scale-up and feedstock selection, further establishing deacetylation as a viable biorefinery pretreatment for the conversion of lignocellulosics into value-added fuels and chemicals.

09 BIOMASS FUELS↗

DOE OSTI2025

Evaluating nonlocal heat transport in directly driven chromium spheres using x-ray spectroscopy

We report on experiments investigating heat transport in laser-generated plasmas using directly driven chromium spheres. The spheres are fielded at the OMEGA laser facility and are driven with laser intensities of 5×10 14 Wcm −2 . Plasma conditions in the corona and scattered light are measured experimentally and compared against predictions from two-dimensional (2D) radiation-hydrodynamic simulations using different heat transport models. Spectroscopic analysis of x-ray self-emission is used as an additional diagnostic. X-ray emission is integrated over a large region of the plasma, probing regions that are not observed by localized optical Thomson scattering. In particular, x-ray emission peaks near the plasma critical density, so emission from optically thin lines provides information on plasma conditions where nonlocal transport is most likely to be significant. Three common heat transport models are considered: local transport with flux limiters f = 0.15 and f = 0.03, and the nonlocal Schurtz–Nicolai–Busquet (SNB) model. Consistent with previous work, both the high-flux (f = 0.15) and SNB models show good agreement with experimentally measured plasma conditions in the corona despite overpredicting laser absorption, whereas the low-flux (f = 0.03) model fails to match any experimental data. Conditions inferred from x-ray self-emission line ratios support this conclusion during the period of laser peak power, although synthetic spectra for all models fail to match the experiment during the transient portions of the pulse. For these reasons, the low-flux model is again rejected.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2023

Isotope dependence of transport in ST40 hot ion mode plasmas

The ST40 compact, high-field spherical tokamak, operating at 2.1 T and with 1.8 MW of neutral beam heating, achieved central carbon impurity ion temperatures in excess of 10 keV, surpassing their business milestone of 100 M °C (8.6 keV). The high temperature discharges were in the hot ion mode, with $T_i \gg T_e$, and they were achieved in both hydrogen and deuterium plasmas with deuterium neutral beam injection. In order to achieve the high temperature scenarios, careful wall conditioning and scenario optimization was carried out in $H^0 \rightarrow H^+$, $D^0 \rightarrow H^+$, and finally in $D^0 \rightarrow D^+$ plasmas. The TRANSP transport code was employed to study the dependence of confinement and transport on isotopic mass, and the conditions that led to the high measured central ion temperatures in the $D^0 \rightarrow H^+$ and $D^0 \rightarrow D^+$ plasmas. The kinetic profiles input into TRANSP were inferred from line-of-sight and limited radial measurements as well as consistency with a number of other experimental constraints. The TRANSP results first showed that the main species central ion temperature was only 0.5–1 keV lower than the measured carbon impurity temperature, and thus in the high performance plasmas also surpassed the 100 M °C level. TRANSP also showed that while the electron thermal conduction loss was dominant, reductions in central ion transport, and an effective decoupling of the ions from the electrons, led to an increase in central ion temperatures with increasing plasma mass. In fact, the associated confinement times exhibited a strong dependence on the isotopic mass of the thermal plasma. These preliminary results are foundations for dedicated experiments with full kinetic profile measurements on ST40 in the next run campaign.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2025

Measurement of turbulent velocity and bounds for thermal diffusivity in laser shock compressed foams by x-ray photon correlation spectroscopy

Experimental benchmarking of transport coefficients under extreme conditions is required for validation of differing theoretical models. To date, measurement of transport properties of dynamically compressed samples remains a challenge with only a limited number of studies able to quantify transport in high pressure and temperature matter. x-ray photon correlation spectroscopy utilizes coherent x-ray sources to measure time correlations of density fluctuations, thus providing measurements of length and timescale-dependent transport properties. Here, we present a first-of-a-kind experiment to conduct x-ray photon correlation spectroscopy in laser shock compression experiments. We report measurement of the turbulent velocity in the wake of a laser driven supersonic shock and place an upper bound on thermal diffusivity in a solid density plasma on nanosecond timescales.

High-energy-density plasmas↗

DOE OSTI2020

Plasma stopping-power measurements reveal transition from non-degenerate to degenerate plasmas

Physically realized electron gas systems usually reside in either the quantum non-degenerate or fully degenerate limit, where the average de Broglie wavelength of the thermal electrons becomes comparable with the interparticle distance between electrons. A few systems, such as young brown dwarfs and the cold dense fuels created in imploded cryogenic capsules at the National Ignition Facility, lie between these two limits and are partially degenerate. The National Ignition Facility has the unique capability of varying the electron quantum degeneracy by adjusting the laser drive used to implode the capsules. This allows experimental studies of the effects of the degeneracy level on plasma transport properties. By measuring rare nuclear reactions in these cold dense fuels, we show that the electron stopping power, which is the rate of energy loss per unit distance travelled by a charged particle, changes with increasing electron density. We observe a quantum-induced shift in the peak of the stopping power using diagnostics that measure above and below this peak. The observed changes in the stopping power are shown to be unique to the transition region between non-degenerate and degenerate plasmas. Furthermore, our results support the screening models applied to partially degenerate astrophysical systems such as young brown dwarfs.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2025

Toward Optimization of Polymer Electrolytes by Electrochemical Characterization: Poly(pentyl malonate) versus Poly(ethylene oxide)

Ion transport in two polymer electrolytes, poly(ethylene oxide) (PEO) and poly(pentyl malonate) (PPM), mixed with lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) is studied in the vicinity of the limiting current. The experimental measurements are in quantitative agreement with theoretical predictions based on the concentrated solution theory. The properties of two electrolytes are compared using a new plot wherein the length-normalized limiting current, i lim L, is plotted as a function of the length-normalized potential drop, Φlim/L, in symmetric cells with electrolyte thickness, L. We propose that electrolyte design should aim to obtain the largest values of i lim L and the smallest values of Φlim/L. Using this criterion, PPM/LiTFSI is a better polymer electrolyte than PEO/LiTFSI. We hope that PPM/LiTFSI will serve as a benchmark for developing next-generation polymer electrolytes.

Lee, Jaeyong↗