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DOE OSTI2021

Evaluation of Oxygen Consumption as a Sensitive Measure of Electrical Cable Polymer Insulation Degradation

Polymers used as dielectric materials in nuclear grade electrical cables, such as cross-linked polyethylene (XLPE) and ethylene-propylene rubber (EPR), are long-lived and durable. Estimating the decades-long useful service life of polymers experimentally in a feasible timeframe of weeks or months requires greatly accelerated aging in the laboratory at elevated temperatures and/or gamma dose rates. Many limitations of accelerated aging, such as due to artefacts of the process including diffusion limited oxidation and dose rate effects, have been identified that can make accurate lifetime prediction at service conditions challenging. This can be due to differences in degradation mechanisms between rapid and extended aging or to the presence of induction periods during which early aging is undetectable using common metrics of polymer insulation characterization such as tensile elongation at break. Conceptually, an ideal measure of aging would track clearly and predictably with material changes throughout the lifecycle of the evolving material state from early aging through end of useful life. With such a metric accelerated aging could be performed at much milder conditions, conditions closer to those found in long term service, and end of life calculated from the early data. Oxygen consumption has previously been proposed as a sensitive measure of insulation polymer oxidation that might meet such desirable characteristics. In this work, nuclear cable insulation samples of the two most common types, XLPE and EPR, from two of the most sourced manufacturers, RSCC and The Okonite Company, were subjected to gamma irradiation at dose rates of 100, 200, and 300 Gy/hr for up to 42 days at 26°C. The aged samples were used to evaluate oxygen consumption as a sensitive measure of aging for these materials and these conditions. For comparison and validation, the aged samples were also characterized using the more conventional tests of mass change, density, carbonyl index, and yellowness index. For both materials, oxygen consumption during irradiation was found to track consistently with applied dose—oxygen consumption rate was linear with time. Mass change and carbonyl index were also clearly proportional to exposure dose. Yellowness index, a surface sensitive measure, was observed to increase linearly with dose at low exposure levels before plateauing. Sample density was not observed to change under the conditions explored. Oxygen consumption was found to be a particularly sensitive metric to measure the degradation of polymeric cable insulation exposed to radiation. Oxygen consumption was compared to Arrhenius and time-temperature-superposition methods for activation energy calculation using literature date and found to be a useful and viable alternative for lifetime prediction. The techniques developed in this work are anticipated to be valuable in the estimation of insulation aging rates under mild conditions approaching service conditions. Direction comparison of useful life prediction by oxygen consumption with prediction via Arrhenius methodology for thermal aging and existing methods for radiation and combined thermal/radiation aging would serve to further validate this promising approach and refine our understanding of material-specific aging rates.

36 MATERIALS SCIENCE↗

NASA NTRS1982

Diffusive-convective physical vapor transport of PbTe from a Te-rich solid source

Crystal growth of PbTe by physical vapor transport (sublimation) in a closed ampoule is governed by the vapor species in thermal equilibrium with the solid compound. Deviations from stoichiometry in the source material cause diffusion limitation of the transport rate, which can be modified by natural (gravity-driven) convection. Mass-transport experiments have been performed using Te-rich material wherein sublimation rates have been measured in order to study the effects of natural convection in diffusion-limited vapor transport. Linear velocities for both crystal growth and evaporation (back sublimation) have been measured for transport in the direction of gravity, horizontally, and opposite to gravity. The experimental results are discussed in terms of both the one-dimensional diffusive-advective model and current, more sophisticated theory which includes natural convection. There is some evidence that convection effects from radial temperature gradients and solutal density gradients have been observed.

Zoutendyk, J.↗

NASA NTRS1985

Transport of ions in presence of induced electric field and electrostatic turbulence - Source of ions injected into ring current

The transport of ions from the polar ionosphere to the inner magnetosphere during stormtime conditions has been computed using a Monte Carlo diffusion code. The effect of the electrostatic turbulence assumed to be present during the substorm expansion phase was simulated by a process that accelerated the ions stochastically perpendicular to the magnetic field with a diffusion coefficient proportional to the energization rate of the ions by the induced electric field. This diffusion process was continued as the ions were convected from the plasma sheet boundary layer to the double-spiral injection boundary. Inward of the injection boundary, the ions were convected adiabatically. By using as input an O(+) flux of 2.8 x 10 to the 8th per sq cm per s (w greater than 10 eV) and an H(+) flux of 5.5 x 10 to the 8th per sq cm per s (w greater than 0.63 eV), the computed distribution functions of the ions in the ring current were found to be in good agreement, over a wide range in L (4 to 8), with measurements made with the ISEE-1 satellite during a storm. This O(+) flux and a large part of the H(+) flux are consistent with the DE satellite measurements of the polar ionospheric outflow during disturbed times.

Cladis, J. B.↗

NASA NTRS2023

Oxidation of Silicon Particles Suspended in Mullite Matrix With Dual-Mode Vacancy Diffusion of Oxygen

Mullite bond coats filled with silicon particles have recently been proposed for the next generation of environmental barrier coatings (EBCs). The sacrificial oxidation of the silicon particles eliminates some of the environmental durability issues associated with traditional EBC designs. To investigate this novel design approach, a mathematical formulation and resulting numerical method have been developed for simulating the oxidation of silicon particles embedded in a mullite matrix. The focus is on the oxidation of the silicon in a dry oxygen environment where the oxidant is presumably oxygen. Oxygen transport from the exterior environment through the mullite is assumed to occur via two lattice defect diffusion mechanisms. As a result, the rate of oxygen transport is dictated by the self-diffusivity of the lattice defects. The numerical method is implemented using the COMSOL Multiphysics® program (COMSOL, Inc.). The method is applied to simulate the oxidation of silicon particles in a mullite pellet in recent oxidation experiments. Numerical results compare favorably with the oxidation behavior observed in the oxidation experiments. The numerical method is also used to investigate the effects of various features of the mullite-silicon particle system on the oxidation behavior.

silicon oxidation↗

DOE OSTI2021

Antiphase boundary migration as a diffusion mechanism in a P3 sodium layered oxide

The electrode materials of Na-ion batteries must exhibit fast ion transport, a property that is often negatively impacted when mobile cations order. Many layered Na (and K) intercalation compounds adopt the P3 crystal structure, which tends to stabilize cation-vacancy orderings over a wide range of Na concentrations. The ordered phases have been predicted to consist of domains that are periodically separated by antiphase boundaries (APBs) to accommodate variations in Na concentration. The mechanisms and rates with which Na diffuses within such ordered phases of P3 are not understood. We have conducted a first-principles study of Na diffusion in the P3 structure, using Na x CoO 2 as a model system. We find that most simple nearest-neighbor hops in Na-vacancy ordered phases in P3 result in unstable configurations and are therefore forbidden. We identify an alternative mechanism of Na transport that is mediated by APB migration via the formation and expansion of kinks along domain boundaries. The limiting kinetic barriers for this mechanism are quite low (0.03 to 0.30 eV). Vacancy defects are not required, and furthermore have formation energies that are higher than those of the APB kink defects. Furthermore, our results suggest that APB migration is a fundamental diffusion mechanism in the P3 structure.

36 MATERIALS SCIENCE↗

NASA NTRS1987

Electrochemical performance and transport properties of a Nafion membrane in a hydrogen-bromine cell environment

The overall energy conversion efficiency of a hydrogen-bromine energy storage system is highly dependent upon the characteristics and performance of the ion-exchange membrane utilized as a half-cell separator. The electrochemical performance and transport properties of a duPont Nafion membrane in an aqueous HBr-Br2 environment were investigated. Membrane conductivity data are presented as a function of HBr concentration and temperature for the determination of ohmic voltage losses across the membrane in an operational cell. Diffusion-controlled bromine permeation rates and permeabilities are presented as functions of solution composition and temperature. Relationships between the degree of membrane hydration and the membrane transport characteristics are discussed. The solution chemistry of an operational hydrogen-bromine cell undergoing charge from 45% HBr to 5% HBr is discussed, and, based upon the experimentally observed bromine permeation behavior, predicted cell coulombic losses due to bromine diffusion through the membrane are presented as a function of the cell state-of-charge.

Baldwin, Richard S.↗

NASA NTRS2016

Materials Outgassing Rate Decay in Vacuum at Isothermal Conditions

As a laboratory for scientific research, the International Space Station has been in Low Earth Orbit for nearly 20 years and is expected to be on-orbit for another 10 years. The ISS has been maintaining a relatively pristine contamination environment for science payloads. Materials outgassing induced contamination is currently the dominant source for sensitive surfaces on ISS and modeling the outgassing rate decay over a 20 to 30 year period is challenging. Materials outgassing is described herein as a diffusion-reaction process using ASTM E 1559 rate data. The observation of -1/2 (diffusion) or non-integers (reaction limited) as rate decay exponents for common ISS materials indicate classical reaction kinetics is unsatisfactory in modeling materials outgassing. Non-randomness of reactant concentrations at the interface is the source of this deviation from classical reaction kinetics. A diffusion limited decay was adopted as the result of the correlation of the contaminant layer thicknesses on returned ISS hardware, the existence of high outgassing silicone exhibiting near diffusion limited decay, and the confirmation of non-depleted material after ten years in the Low Earth Orbit.Keywords: Materials Outgassing, ASTM E 1559, Reaction Kinetics, Diffusion, Space Environments Effects, Contamination

Huang, Alvin Y.↗

DOE OSTI2024

Sorption kinetics and stability of conventional adsorbents for mercury remediation

In-situ remediation of mercury at numerous contaminated sites worldwide is a challenging and costly endeavor due to the persistency of this contaminant. In this study, we evaluated eight commercially available sorbent media ranging from carbon-, clays- and silica-based materials (PBC– Biochar, eSorb – Sorbster, nsPAC – Powdered Activated Carbon, fsPAC – Powdered Activated Carbon with Mackinawite, F300 – Filtrasorb 300, Si-SH – Silica Thiol, eBind – RemBind, Q-Clay – Organoclay PM-199), for their effectiveness in sorbing mercury (Hg 2+ ) and mercury complexed with dissolved organic matter (Hg-DOM). Under the chosen experimental conditions of this study, results showed that in the absence of DOM, the kinetic rates of Hg 2+ sorption onto the evaluated sorbents were in the order of 0.31 min-1 (Si-SH) to 2.98 min -1 (nsPAC), whereas in the presence of DOM, the rates varied from 0.16 min-1 (F300) to 0.95 min -1 (nsPAC). The measured sorption capacity for Hg 2+ in the absence of DOM varied from 3.02 mg/g (Q-Clay) to 35.15 mg/g (Si-SH), whereas in the presence of DOM, calculated partition coefficient (KD) ranged from 69.7 mL/g (Q-Clay) to 41,510 mL/g (Si-SH). Furthermore, kinetic data suggest liquid film diffusion was the rate-limiting steps governing mercury sorption onto the studied media. Overall, the obtained study parameters (kinetics/isotherm) are particularly important in informing robust engineering designs for deployment of the vast majority of evaluated sorbents. Thus, sorbent-based strategies offer viable solutions for cost-effective cleanup of mercury at industrially contaminated sites.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1988

The effect of diffusive segregation on the fracture of hydrogen charged nickel

Hydrogen charged nickel was deformed in tension at a test temperature of 208 K to study the diffusive segregation of hydrogen during straining and the dependence of embrittlement on grain boundary hydrogen concentration and deformation rate. Tests were performed on samples in the as-quenched condition at various strain rates. An increase in the degree of embrittlement at slow strain rates can be attributed to diffusive segregation of hydrogen to grain boundaries during the test period. The embrittlement of samples with equal grain boundary hydrogen concentration was found to be relatively insensitive to strain rate, bulk hydrogen concentration and the total time at the test temperature.

Lassila, D. H.↗

DOE OSTI2020

Improved lithium storage capacity and high rate capability of nitrogen-doped graphite-like electrode materials prepared from thermal pyrolysis of graphene quantum dots

Adopting a solid-phase microwave-assisted technique followed by thermal pyrolysis of N-functionalized graphene quantum dots, novel nitrogen-doped graphite-like (NGL) electrode materials were synthesized in this work and served as the anode for Li-ion batteries. The NGL anode demonstrated reversible capacity of 530 mAh g -1 at 0.1C, superior rate capability at high C rate operation (420 mAh g -1 at 5C), remarkable initial coulombic efficiency (>95.7%), and excellent cyclic stability along with high efficiency (>99.1%) during entire cycling. The NGL anode nanostructure enables improved lithium ion mobility and reversible Li + storage during cycling. The analysis of the Ragone plots revealed that the specific energy of NGL anode reaches to ca. 840 Wh kg -1 at the power density of 4200 W kg -1 . The diffusion coefficient of Li ions was measured as 1.69 × 10 -9 cm 2 s -1 for the NGL anode material, substantially improving over commonly used graphite electrodes (15–26 times higher Li + diffusivity). The high-rate cyclability as well as the cyclic stability of the NGL anodes were also confirmed via long-term cycling of full pouch cells assembled with ternary cathode and NGL anode. The robust design of the NGL anode materials introduced in this work, paves the way for designing next-generation lithium-ion batteries operating at ultra-high C rates.

25 ENERGY STORAGE↗

NASA NTRS1974

Diffusion with chemical reaction: An attempt to explain number density anomalies in experiments involving alkali vapor

The mutual diffusion of two reacting gases is examined which takes place in a bath of inert gas atoms. Solutions are obtained between concentric spheres, each sphere acting as a source for one of the reactants. The calculational model is used to illustrate severe number density gradients observed in absorption experiments with alkali vapor. Severe gradients result when sq root k/D R is approximately 5 where k, D, and R are respectively the second order rate constant, the multicomponent diffusion constant, and the geometrical dimension of the experiment.

Snow, W. L.↗

DOE OSTI2024

Concurrent measurement of strain and chemical reaction rates in a calcite grain pack undergoing pressure solution: Evidence for surface-reaction controlled dissolution

Pressure solution is inferred to be a significant contributor to sediment compaction and lithification, especially in carbonate sediments. For a sediment deforming primarily by pressure solution, the compaction rate should be directly related to the rate of calcite dissolution, transport along grain contacts, and calcite reprecipitation. Previous experimental work has shown that there is evidence that deformation in wet calcite grain packs is consistent with control by pressure solution, but considerable ambiguity remains regarding the rate limiting mechanism. We present the results of laboratory compaction experiments designed to directly measure calcite dissolution and precipitation rates (recrystallization rates) concurrently with strain rate to test whether measured rates are consistent with predicted rates both in absolute magnitude and time evolution. Recrystallization rates are measured using trace element chemistry (Sr/Ca, Mg/Ca) and isotopes (87Sr/86Sr) of fluids flowing slowly through a compacting grain pack as it is being triaxially compressed. Imaging techniques are used to characterize the grain contacts and strain effects in the post-experiment grain pack. Our data show that calcite recrystallization rates calculated from all three geochemical parameters are in approximate agreement and that the rates closely track strain rate. The geochemically inferred rates are close to predicted rates in absolute magnitude. Uncertainty in grain contact dimensions makes distinguishing between surface reaction control and diffusion control difficult. Measured reaction rates decrease faster than predicted from standard pressure solution creep flow laws. This inconsistency may indicate that calcite dissolution rates at grain contacts are more complex, and more time-dependent, than suggested by geometric models designed to predict grain contact stresses.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2016

Ion-Scale Structure in Mercury's Magnetopause Reconnection Diffusion Region

The strength and time dependence of the electric field in a magnetopause diffusion region relate to the rate of magnetic reconnection between the solar wind and a planetary magnetic field. Here we use approximately 150 milliseconds measurements of energetic electrons from the Mercury Surface, Space Environment, GEochemistry, and Ranging (MESSENGER) spacecraft observed over Mercury's dayside polar cap boundary (PCB) to infer such small-scale changes in magnetic topology and reconnection rates. We provide the first direct measurement of open magnetic topology in flux transfer events at Mercury, structures thought to account for a significant portion of the open magnetic flux transport throughout the magnetosphere. In addition, variations in PCB latitude likely correspond to intermittent bursts of approximately 0.3 to 3 millivolts per meter reconnection electric fields separated by approximately 5 to10 seconds, resulting in average and peak normalized dayside reconnection rates of approximately 0.02 and approximately 0.2, respectively. These data demonstrate that structure in the magnetopause diffusion region at Mercury occurs at the smallest ion scales relevant to reconnection physics.

Gershman, Daniel J.↗

DOE OSTI2026

Dynamics of iodine geminate recombination in supercritical xenon solvent: Caging effect

Understanding the dynamics of chemical reactions in solutions is vital, as their rates and kinetics are significantly affected by the solvent environment. Supercritical solvents offer extensive applications in chemical reactions by enabling the manipulation of the solution environment. Here, in this study, we investigate the geminate recombination of iodine in a supercritical xenon solvent by using ReaxFF-based molecular dynamics simulations. Our findings reveal that the highest iodine recombination rate occurs near supercritical conditions, while lower-pressure conditions lead to reduced collision rates and unstable recombination, and higher-pressure conditions hinder iodine diffusion, resulting in a lower recombination rate. Our analysis shows that the xenon local density at the time of recombination is at least 2.5 times higher than the global density, confirming the presence of xenon clusters surrounding the Iodine atoms. This observation is further supported by coordination number analysis, which confirms an elevated xenon local density during recombination. In addition, the correlation between the total energy of xenon atoms within a cluster and recombined iodine atoms underscores the kinetic energy transfer process, validating the occurrence of geminate recombination. The excess kinetic energy from the recombining iodine atoms is transferred to the surrounding xenon atoms. Our examination of geminate recombination demonstrates that iodine atoms confined within xenon clusters—whether through manual insertion of atoms or the fast dissociation of an iodine molecule within xenon clusters—are more likely to recombine as primary geminate recombination. However, extending the iodine molecule dissociation time allows iodine atoms to diffuse out of the cluster, and the recombination to shift toward secondary geminate recombination.

Cage effect↗

DOE OSTI2024

Continuous Flow Photoelectrochemical Reactor with Gas Permeable Photocathode: Enhanced Photocurrent and Partial Current Density for CO 2 Reduction

Photoelectrochemical (PEC) CO 2 reduction using a photocathode is an attractive method for making valuable chemical products due to its simplicity and lower overpotential requirements. However, previous PEC processes have often been diffusion-limited leading to low production rates of the CO 2 reduction reaction, due to inefficient gas diffusion through the liquid electrolyte to the catalyst surface, particularly at high current densities. In this study, a gas-permeable photocathode in a continuous flow PEC reactor is incorporated, which facilitates the direct supply of CO 2 gas to the photocathode-electrolyte interface, unlike dark reaction-based flow reactors. This concept is demonstrated using Ag-TiO 2 on carbon paper, illuminated through a quartz window and flowing liquid electrolyte. CO 2 supply is managed via pressure and flow control on the non-illuminated side of the carbon paper. The photocurrent density is significantly influenced by the flow rates and pressure of CO 2 gas, and the electrolyte flow rates. Compared to the traditional H-cell, the continuous PEC flow reactor achieves ≈10-fold increase in CO faradaic efficiency, 30-fold increase in production rate and 16-fold increase in stability without catalyst modifications. This work provides essential insights into the design and application of continuous gas-liquid flow PEC reactor systems, highlighting their potential for other PEC reactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Observation of substrate diffusion and ligand binding in enzyme crystals using high-repetition-rate mix-and-inject serial crystallography

Here, we illustrate what happens inside the catalytic cleft of an enzyme when substrate or ligand binds on single-millisecond timescales. The initial phase of the enzymatic cycle is observed with near-atomic resolution using the most advanced X-ray source currently available: the European XFEL (EuXFEL). The high repetition rate of the EuXFEL combined with our mix-and-inject technology enables the initial phase of ceftriaxone binding to the Mycobacterium tuberculosis β-lactamase to be followed using time-resolved crystallography in real time. It is shown how a diffusion coefficient in enzyme crystals can be derived directly from the X-ray data, enabling the determination of ligand and enzyme–ligand concentrations at any position in the crystal volume as a function of time. In addition, the structure of the irreversible inhibitor sulbactam bound to the enzyme at a 66 ms time delay after mixing is described. This demonstrates that the EuXFEL can be used as an important tool for biomedically relevant research.

36 MATERIALS SCIENCE↗

NASA NTRS1995

Modeling and simulation of a turbulent far wake

Work continued on two projects which had been started during previous years. Both projects involve calculations of the subsonic, turbulent far wake of a two-dimensional object at a Reynolds number of 1000 (based on wake momentum thickness). This flow was used as a test case for direct comparison of various turbulence models and a direct numerical simulations (DNS) of this flow were undertaken. In the turbulence model comparison studies, for any particular model tested, a unique self-similar solution was obtained far enough downstream, regardless of inlet conditions. Furthermore, different turbulence models led to different far-wake equilibrium solutions. No turbulence model could correctly predict all features of the turbulent far wake. For example, the spreading rate and turbulent shear stresses were underpredicted by all the standard models (both two-equation and full Reynolds stress models). In cases where a more correct spreading rate was achieved, it was at the expense of the turbulent kinetic energy, which was overpredicted. In general, the Algebraic Dissipation Rate Model of Gatski and Speziale, 1992, when added to any of the standard models, improved the results dramatically. Also, full Reynolds stress closure models did a much better job at predicting the shapes of both the mean and turbulence profiles, but the spreading rate was not significantly improved over that predicted by the simpler two-equation models. There are two main conclusions from these studies: First, in a comparison such as this, it is not enough to compare just one parameter, like the spreading rate. A good prediction for one parameter does not necessarily imply good predictions for all parameters in a flow. Second, since no turbulence model could correctly predict the turbulent far wake, much of the important physics of turbulent free shear flows is apparently lost by the assumptions inherent in today's methods of turbulence modeling; turbulence models must be improved. Direct simulations of this flow were begun last year in order to provide a data base through which some of the deficiencies of the existing turbulence models could be identified. Quantities such as the pressure-strain correlation, turbulent diffusion, and the dissipation rate tensor can be easily calculated from the DNS results, whereas these quantities are nearly impossible to measure experimentally. Improvements to existing turbulence models (and development of new models) require knowledge about flow quantities such as these. During this summer, diagnostics codes were written which will calculate the parameters mentioned above, along with other single-point and multi-point statistics. The DNS calculations are still in progress at the time of this writing. When these calculations are complete, the diagnostics codes will be applied so that the results can aid turbulence modelers. In addition, the results will show whether or not there exists a universal equilibrium turbulent far wake, independent of initial conditions.

Cimbala, John M.↗

DOE OSTI2025

Beyond fragmented dopant dynamics in quantum spin lattices: Robust localization and non-Gaussian diffusion

The motion of dopants in magnetic spin lattices has received tremendous attention for at least four decades due to its connection to high-temperature superconductivity. Despite these efforts, we lack a complete understanding of their behavior, especially out of the equilibrium and at nonzero temperatures. In this paper, we take a significant step towards a much deeper understanding based on state-of-the-art matrix-product-state calculations. In particular, we investigate the nonequilibrium dynamics of a dopant in two-leg 𝑡−𝐽 ladders with antiferromagnetic XXZ spin interactions. In the Ising limit, we find that the dopant is localized for all investigated nonzero temperatures due to an emergent disordered potential, with a localization length controlled by the underlying correlation length of the spin lattice, which increases exponentially with decreasing temperature. The dopant, hereby, only delocalizes asymptotically in the zero temperature limit. This greatly generalizes the localization effect discovered recently in Hilbert space fragmented models [Phys. Rev. Res. 6, 023325 (2024), SciPost Phys. Core 7, 054 (2024)]. In the presence of spin-exchange processes at rate 𝛼, the dopant diffuses with a diffusion coefficient, 𝐷 ℎ , depending nonmonotonically on 𝛼. It initially increases linearly as 𝐷 ℎ ∝ 𝛼 for 𝛼 ≪ 1 before dropping off as 𝛼 −1 for 𝛼 > 1. Moreover, we show that the underlying spin dynamics at infinite temperature behaves qualitatively the same, albeit with important quantitative differences. We substantiate these findings by showing that the dynamics features self-similar scaling behavior, which strongly deviates from the Gaussian behavior of regular diffusion, especially for weak spin exchange. Finally, we show that the diffusion coefficient 𝐷 ℎ follows an Arrhenius relation at high temperatures, whereby it is exponentially suppressed upon cooling.

Anomalous diffusion↗