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DOE OSTI2022

Dual Protective Mechanism of AlPO 4 Coating on High-Nickel Cathode Material for High Energy Density and Long Cycle Life Lithium-Ion Batteries

Cathode material with high nickel content is a promising candidate for the future generation of Li-ion batteries (LIBs). However, severe structural degradation during cycling limits its practical use, especially for electric vehicles. Herein, AlPO 4 nanoparticles were synthesized and then coated onto the surface of a high-nickel layer-structured cathode via a dry coating method. The AlPO 4 nanoparticles coating significantly improved the cycling stability from 69.2% to over 80% capacity retention after 140 cycles. Furthermore, the structure and chemical composition of the AlPO 4 -coated cathode was investigated by XRD, SEM, XPS, and STEM. Compared with the non-coated cathode, we revealed a dual protective mechanism for enhanced cycling stability, where Al doping and Li 3 PO 4 coating play synergistic roles in protecting cathode material through long-term cycling. This work demonstrates a facile and environmentally friendly approach toward improving the performance of high-nickel LIB cathodes, which can be easily scaled up for industrial applications.

25 ENERGY STORAGE↗

DOE OSTI2020

Bovine adapted transmissible mink encephalopathy is similar to L-BSE after passage through sheep with the VRQ/VRQ genotype but not VRQ/ARQ

Background: Transmissible mink encephalopathy (TME) is a fatal neurologic disease of farmed mink. Evidence indicates that TME and L-BSE are similar and may be linked in some outbreaks of TME. We previously transmitted bovine adapted TME (bTME) to sheep. The present study compared ovine passaged bTME (o-bTME) to C-BSE and L-BSE in transgenic mice expressing wild type bovine prion protein (TgBovXV). To directly compare the transmission efficiency of all prion strains in this study, we considered the attack rates and mean incubation periods. Additional methods for strain comparison were utilized including lesion profiles, fibril stability, and western blotting. Results: Sheep donor genotype elicited variable disease phenotypes in bovinized mice. Inoculum derived from a sheep with the VRQ/VRQ genotype (o-bTME VV ) resulted in an attack rate, incubation period, western blot profile, and neuropathology most similar to bTME and L-BSE. Conversely, donor material from a sheep with the VRQ/ARQ genotype (o-bTME AV ) elicited a phenotype distinct from o-bTME VV , bTME and L-BSE. The TSE with the highest transmission efficiency in bovinized mice was L-BSE. The tendency to efficiently transmit to TgBovXV mice decreased in the order bTME, C-BSE, o-bTME VV , and o-bTME AV . The transmission efficiency of L-BSE was approximately 1.3 times higher than o-bTMEVV and 3.2 times higher than o-bTME AV . Conclusions: Our findings provide insight on how sheep host genotype modulates strain genesis and influences interspecies transmission characteristics. Given that the transmission efficiencies of L-BSE and bTME are higher than C-BSE, coupled with previous reports of L-BSE transmission to mice expressing the human prion protein, continued monitoring for atypical BSE is advisable in order to prevent occurrences of interspecies transmission that may affect humans or other species.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2017

Turbulent Spot Pressure Fluctuation Wave Packet Model

Wave packet analysis provides a connection between linear small disturbance theory and subsequent nonlinear turbulent spot flow behavior. The traditional association between linear stability analysis and nonlinear wave form is developed via the method of stationary phase whereby asymptotic (simplified) mean flow solutions are used to estimate dispersion behavior and stationary phase approximation are used to invert the associated Fourier transform. The resulting process typically requires nonlinear algebraic equations inversions that can be best performed numerically, which partially mitigates the value of the approximation as compared to a more complete, e.g. DNS or linear/nonlinear adjoint methods. To obtain a simpler, closed-form analytical result, the complete packet solution is modeled via approximate amplitude (linear convected kinematic wave initial value problem) and local sinusoidal (wave equation) expressions. Significantly, the initial value for the kinematic wave transport expression follows from a separable variable coefficient approximation to the linearized pressure fluctuation Poisson expression. The resulting amplitude solution, while approximate in nature, nonetheless, appears to mimic many of the global features, e.g. transitional flow intermittency and pressure fluctuation magnitude behavior. A low wave number wave packet models also recover meaningful auto-correlation and low frequency spectral behaviors.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2019

Dissipative and fast-timescale phenomena in superconductors

This project explored new effects and regimes that unfold in superconductors as they are pushed to ex treme and unprecedented conditions of electric field, power densities, vortex velocities, etc. Besides their own novelty, these phenomena yield fundamental in formation about the superconducting state and its parameters, as well as its practical limits for techno logical applications. Furthermore some of these ef fects (such as formation of phase slip processes and the acceleration of superfluid) are time dependent on time scales such as quasiparticle-phonon energy re laxation and gap relaxation. This project used fast low-duty-cycle pulsed signals to first of all access these regimes without excessive heating and secondly to observe directly in the time domain the temporal unfolding of these phenomena on nanosecond time scales. This project led to the discovery of new effects in the transport behavior in superconductors, provided new information on fundamental parameters, and helped establish intrinsic strengths and limitations of different superconducting materials for ap plications. The primary tools developed for extending the range of measurable dissipation densities and observation of short time-scale phenomena were fast pulsed-current and pulsed-voltage sources, and fast high-CM-rejection detection circuitry. This allowed conducting measurements at power densities in the 10 10 W/cm 3 range, and at E ~ 1 kV/cm and v Φ ~10 km/s. Also developed was the ability to simultaneously track current I(t) and voltage V (t) and cross correlate them with sub-nanosecond temporal resolution. A recent angle of this project was the exploration of subtle phenomena at low current densities, especially for the magnetic field orientation parallel to the plane of the films. Through modifications of the pulsed tube closed cycle cryostat, we developed methods for attaining low-noise and high temperature-stability conditions. This led to the observation of novel dimensional effects related to the mixed state and vortex matter, and to a new type of magnetoresistance oscillation.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Finite Volume Discretization of the Euler Equations in Pronghorn

Modeling flow and heat transfer in high temperature gas reactors (HTGR) requires the ability to model a wide range of flow speeds from slow (natural convection), to intermediate (forced-flow conditions), to supersonic regimes (depressurization) for a wide range of geometries including the pebble bed, upper and lower plenum, and risers. In previous work, Pronghorn has effectively modeled low-to-medium speed flows in scenarios such as the one described in the two-dimensional PBMR-400 benchmark, using its finite-element-based streamline-upwind Petrov-Galerkin (SUPG) stabilized implementation of the Euler equations. However, limitations of this method become apparent when dealing with more complicated geometries (e.g. imposing slip boundary conditions at nodes belonging to two different boundaries) and when gas speeds are fast enough for shocks and supersonic flow to occur. For these problems, the finite-element-based solver lacks robustness and is plagued by slow iterative convergence or even divergence. In order to address these challenges, the Pronghorn code at INL has been updated with new, modified versions of its original equations. The new Pronghorn models are built on the finite volume method with a Harten-Lax-van Leer-Contact (HLLC) Riemann solver based numerical flux method, which (1) allows imposing slip boundary conditions much more robustly and (2) performs well for a wide range of flow speeds. The finite-volume-based flow solver will form the basis for a robust coarse-mesh thermal-hydraulics capability in Pronghorn.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2018

Cyber Network Design for Secondary Frequency Regulation: A Spectral Approach

We present a preliminary theoretical framework based on spectral graph theory that captures how the cyber topology of a distributed secondary frequency control scheme impacts the stability, optimality, and transient performance of our power system as a cyber-physical network. We show that a collection of polynomials defined in terms of the cyber and physical Laplacian eigenvalues encode information on the interplay between cyber and physical networks. It is demonstrated that to understand the impact of adding cyber connectivity, one should separate the low-damping and high-damping regimes. Although adding cyber connectivity always improves the performance for high-damping systems, it is not the case for low-damping scenarios. Based on the theoretical study, we discuss how a good cyber network should be designed. Our empirical study shows that for practical systems, the number of communication channels that is needed to achieve near-optimal performance is usually less than twice the number of buses.

24 POWER TRANSMISSION AND DISTRIBUTION↗

DOE OSTI2022

Parametric model-order-reduction development for unsteady convection

A time-averaged error indicator with POD- h Greedy is developed to drive parametric model order reduction (pMOR) for 2D unsteady natural convection in a high-aspect ratio slot parameterized with the Prandtl number, Rayleigh number, and slot angle with respect to the gravity. The error indicator is extended to accommodate the energy equation and Leray regularization. Despite being two-dimensional and laminar, the target flow regime presents several challenges: 1) there is a bifurcation in the angle parameter space; 2) the solution can be multivalued, even at steady state; and 3) the solution exhibits spatio-temporal chaos at several points in the parameter space. The authors explore several reduced-order models (ROMs) and demonstrate that Leray-regularized Galerkin ROMs provide a robust solution approach for this class of flows. They further demonstrate that error-indicated pMOR can efficiently predict several QOIs, such as mean flow, mean Nusselt number and mean turbulent kinetic energy, even in the presence of a bifurcation. Finally, they show that spatio-temporal chaos can lead to lack of reproducibility in both the full-order model and the reduced-order model and that the variance in the full-order model provides a lower bound on the pMOR error in these cases.

leray regularization↗

DOE OSTI2017

Formal Solutions for Polarized Radiative Transfer. I. The DELO Family

The discussion regarding the numerical integration of the polarized radiative transfer equation is still open and the comparison between the different numerical schemes proposed by different authors in the past is not fully clear. Aiming at facilitating the comprehension of the advantages and drawbacks of the different formal solvers, this work presents a reference paradigm for their characterization based on the concepts of order of accuracy , stability , and computational cost . Special attention is paid to understand the numerical methods belonging to the Diagonal Element Lambda Operator family, in an attempt to highlight their specificities.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2016

Aerogel sorbents

The current invention describes methods and compositions of various sorbents based on aerogels of various silanes and their use as sorbent for carbon dioxide. Methods further provide for optimizing the compositions to increase the stability of the sorbents for prolonged use as carbon dioxide capture matrices.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

DOE OSTI2018

Aerogel sorbents

36 MATERIALS SCIENCE↗

DOE OSTI2021

Towards Efficient Uncertainty estimation in deep learning for robust energy prediction in crystal materials

In material science, recent studies have started to explore the potential of using deep learning to improve property prediction from high-fidelity simulations, e.g, density functional theory (DFT). However, the design spaces are sometimes too large and intractable to sample completely. This results in a critical question that is how to evaluate the confidence and robustness of the prediction. In this paper, we propose an efficient approach to estimate uncertainty in deep learning using a single forward pass and then apply it for robust prediction of the total energy in crystal lattice structures. Our approach is built upon the deep kernel learning (DKL) that originally introduces to leverage the expressiveness of deep neural networks as input with a probabilistic prediction of Gaussian processes (GPs) as output. Existing DKL methods have difficulties in the accuracy of predictive uncertainty, training stability, and scaling to large datasets, which lead to significant barriers in real-world applications. We propose to address these challenges by using an inducing point approximate GP in feature space combined with spectral normalization as a regularization. We finally demonstrate our robust performance on an artificial example and a real-world application from materials chemistry.

Bi, Sirui↗

DOE OSTI2025

Laser-Induced Breakdown Spectroscopy (LIBS) Sensing for Environmental and Subsurface Monitoring

Groundwater monitoring is essential to timely and accurately reflect the current situations and the trends of water quality. However, the long-term stability and survival of any potential in-situ monitoring method is threatened by the harsh conditions and the groundwater monitoring in downhole environments poses numerous challenges to the sensor community. Laser induced breakdown spectroscopy (LIBS) has been demonstrated as a promising technology for chemical monitoring in high-temperature high-pressure (HTHP) environments and hard to reach places. The technique demonstrates several advantages, such as rapid, real-time, in-situ, and simultaneous detection of multiple elements with simple or no sample preparation. This chapter includes a brief review of the field-portable LIBS systems, and development of a compact, robust, and simple LIBS instrument for downhole HTHP water quality monitoring. The fieldable prototype sensor is tested in an onsite monitoring well where trace elements’ concentrations are tracked over an extended period. The testing has verified that the fiber coupled design performs as desired. The system shows good calibration linearity for tested elements and collection times, and Limits of Detection (LODs) that are comparable to those of tabletop LIBS instruments. In addition to groundwater quality monitoring, the fabricated LIBS-based sensor could have widespread sub-surface detection applications.

Jain, Jinesh [NETL Site Support Contractor, Nation↗

DOE OSTI2023

Stabilizing a strongly nonlinear structure through shaker dynamics in fixed frequency voltage control tests

Bifurcations are commonly encountered during force controlled swept and stepped sine testing of nonlinear structures, which generally leads to the so-called jump-down or jump-up phenomena between stable solutions. There are various experimental closed-loop control algorithms, such as control-based continuation and phase-locked loop, to stabilize dynamical systems through these bifurcations, but they generally rely on specialized control algorithms that are not readily available with many commercial data acquisition software packages. A recent method was developed to experimentally apply sequential continuation using the shaker voltage that can be readily deployed using commercially available software. By utilizing the stabilizing effects of electrodynamic shakers and the force dropout phenomena in fixed frequency voltage control sine tests, this approach has been demonstrated to stabilize the unstable branch of a nonlinear system with three branches, allowing for three multivalued solutions to be identified within a specific frequency bandwidth near resonance. Recent testing on a strongly nonlinear system with vibro-impact nonlinearity has revealed jumping behavior when performing sequential continuation along the voltage parameter, like the jump phenomena seen during more traditional force controlled swept and stepped sine testing. Here, this paper investigates the stabilizing effects of an electrodynamic shaker on strongly nonlinear structures in fixed frequency voltage control tests using both numerical and experimental methods. The harmonic balance method is applied to the coupled shaker-structure system with an electromechanical model to simulate the fixed voltage control tests and predict the stabilization for different parameters of the model. The simulated results are leveraged to inform the design of a set of experiments to demonstrate the stabilization characteristics on a fixture-pylon assembly with a vibro-impact nonlinearity. Through numerical simulation and experimental testing on two different strongly nonlinear systems, the various parameters that influence the stability of the coupled shaker-structure are revealed to better understand the performance of fixed frequency voltage control tests.

42 ENGINEERING↗

DOE OSTI2016

Structure, electrical characteristics, and high-temperature stability of aerosol jet printed silver nanoparticle films

Printed electronics has emerged as a versatile eco-friendly fabrication technique to create sintered nanoparticle (NP) films on arbitrary surfaces with an excellent control over the film microstructure. While applicability of such films for high-temperature applications is not explored previously, herein we report the high-temperature electrical stability of silver (Ag) metal NP films fabricated using an Aerosol Jet based printing technique and demonstrate that this behavior is dictated by changes in the film microstructure. In-situ high temperature (24–500 °C) impedance spectroscopy measurements show that the real part of the impedance increases with increasing temperature up to 150 °C, at which point a decreasing trend prevails until 300 °C, followed again by an increase in impedance. The electrical behavior is correlated with the in-situ grain growth of the Ag NP films, as observed afterwards by scanning electron microscopy and X-ray diffraction (XRD), and could be tailored by controlling the initial microstructure through sintering conditions. Using combined diffraction and spectroscopic analytical methods, it is demonstrated the Aerosol Jet printed Ag NP films exhibit enhanced thermal stability and oxidation resistance. In addition to establishing the conditions for stability of Ag NP films, the results provide a fundamental understanding of the effect of grain growth and reduction in grain boundary area on the electrical stability of sintered NP films.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2018

Thermal stability of the complex of pyrene–β-cyclodextrin dimer with aromatic amino acids

Using the method of adsorption spectroscopy, the temperature dependence of the electronic absorption spectra of the fluorescent chemosensor (CS), based on the supramolecular pyrene–2β-cyclodextrin complex (Pyr@2βCD, PCD), was studied in the absence and in the presence of phenylalanine (Phe). The application of CS, where pyrene serves as a fluorescent probe, is based on the ability of CS to form the inclusion complexes with small organic molecules as well as with aromatic amino acids (AA) such as Phe, tryptophan (Trp), tyrosine (Tyr), and histidine (His) in aqueous solutions. Upon heating to 55 °C, the PCD complex in the presence of Phe shows a higher stability as compared to that in the absence of Phe. The molecular dynamics simulation was applied to study the thermal stability of PCD and its complexes with the above AAs in water. The PCD complex exists in two configurations. In configuration 1 the planar Pyr molecule lies in the equatorial plane of the βCD dimer, the plane of Pyr is nearly perpendicular to the vertical axis of the dimer 2βCD, and water fills up the empty part of the cavity. In configuration 2, the plane of Pyr is inclined with respect to the axis of the 2βCD dimer by ~30°. The PCD complex initially prepared in state 1 is spontaneously transformed into state 2 and remains stable up to the boiling temperature. The transition of PCD from the form 1 to 2 is provided by fluctuations in water content in its cavities. The inclusion complexes of amino acids 2AA@PCD exist in a single conformation 1. Complexes of PCD with Trp and Phe are stable up to the boiling temperature, i.e., these AAs are preserved within the PCD cavities even at the elevated temperature. The complex with Tyr decays at 60 °C, and the complex with His is unstable at room temperature and above.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Dynamics of Gas Flow and Hydrate Formation within the Hydrate Stability Zone

Methane hydrate comprises a significant piece of the global carbon cycle and is an important potential energy resource. Thick marine sands around the world contain free gas beneath and high concentrations of methane hydrate far above the base of the hydrate stability zone. The mechanisms controlling gas transport and hydrate formation within the region where hydrate is stable remains an important research question. I developed a new experimental method to investigate the fundamental behaviors associated with hydrate formation during gas flow into the hydrate stability zone. First, I performed a set of experiments at the same experimental conditions, to determine the repeatability of this behavior. I compared these results to those from an experiment performed outside the hydrate stability zone to elucidate the change in intrinsic gas flow behavior due to hydrate formation. Second, I performed additional experiments at a range of flow rates as well as several shut-in experiments, where I observed long-term hydrate formation after flow took place. I analyzed the bulk and core-scale behaviors of these experiments using a combination of mass balance and computed-tomography analyses. I found that many of my experimentally observed behaviors are not accurately described by previous models and that the mechanism for gas transport was fundamentally different than typically assumed. I proposed that hydrate formation at the gas-brine interface separates the gas and brine phases and limits hydrate formation to methane transport through the hydrate. This behavior produced temporary flow blockages that were mitigated when the hydrate skin fails due to pressure gradients across the sample. This behavior also produced different thermodynamics states on either side of the hydrate that could persist for hundreds to thousands of years. These results provide an alternative mechanism for gas transport and hydrate formation through the hydrate stability zone that does not require the gas, hydrate, and brine to be at three-phase equilibrium. This mechanism provides a first-order connection between experimentally observed micro-scale phenomena and field-scale gas transport and hydrate formation behaviors in these reservoirs.

03 NATURAL GAS↗

DOE OSTI2018

Highly Selective and Stable Multivariable Gas Sensors for Enhanced Robustness and Reliability of SOFC Operation

GE Global Research, in partnership with SUNY Polytechnic Institute (SUNY Poly) and GE–Fuel Cells LLC, designed, built, and tested multi-gas sensor prototypes for in situ monitoring of gases produced during steam reforming in solid oxide fuel cell (SOFC) systems. To be widely adopted and to deliver a lower operating cost for customers, SOFC systems should enhance their operation reliability and improve stack robustness. These needs can be achieved by early diagnostics of potential upsets by using in-situ gas sensors for the real-time monitoring of gas mixture compositions. Thus, this project objective was to achieve selectivity and stability of sensing of gases for SOFC applications by implementing a new generation of gas sensors, known as multivariable sensors. Such sensors are intended to complement the mature traditional analytical instruments based on sensor performance and design characteristics. The key sensor-performance characteristics include accurate detection and quantitation of several gases in their mixtures and stability of operation in unattended applications. The key design characteristics of sensors include their unobtrusive form factor and cost-effectiveness. The duration of the project was 18 months with the project structure that included three technical tasks such as (1) design and laboratory validation of multivariable sensors for selective detection of H 2 and CO gases, (2) laboratory validation of sensor stability over a two-week testing, and (3) field-validation of the developed multivariable sensor system prototype at GE–Fuel Cells factory. Multi-gas detection was achieved with multivariable photonic sensors designed to operate at elevated temperature. The sensor design was based on three-dimensional (3D) bio-inspired photonic nanostructure that was fabricated using materials responsive to gases of interest such as H 2 and CO. The gas discrimination and the rejection of interferences such as CH 4 , H 2 O, and others was performed by optimizing the design parameters of the 3D photonic nanostructures such as their composition and morphology. Planar sol-gel and sputtered sensing films were fabricated as controls. As a result of the fabrication, functionalization, excitation, and performance testing of 3D photonic sensors, we developed initial design rules for high temperature multivariable sensors. These design rules pave the way for the new generation of cost-effective industrial sensors. Stability of sensor operation was tested in the laboratory conditions under variations of the ambient environments. Stability tests were designed in the order of enhanced complexity and realism of sensor operation and included quantitation of a single gas, quantitation of a single gas in the presence of interferences, and quantitation of two and three gases. We have found that conventional machine learning data analysis stools were unable to correct for the sensor drift. Thus, we have developed new methods of machine learning data analysis that provided us with needed performance stability. Such performance improvement in gas sensing was a significant milestone in bringing our multivariable sensors to practical applications. The project culminated with initial field validation of developed multivariable sensor prototypes at GE–Fuel Cells LLC. The in situ data generated by the sensor system in the lab and field conditions provided inputs that advanced our fundamental understanding of gas sensing at high temperatures to enable sensors for SOFC applications and allowed development of the recommendations for further deliverables.

47 OTHER INSTRUMENTATION↗

DOE OSTI2021

Comparison of Electromagnetic Transient and Phasor-based Simulation for the Stability of Grid-Forming-Inverter-based Microgrids

The increasing interest in studying feeder-level, inverter-based microgrids requires appropriate simulation methods that can effectively simulate the dynamics of distribution feeders that typically have thousands of nodes. To examine the accuracy of phasor-based simulation for the stability of feeder-level, inverter-based microgrids, a comparative study between electromagnetic transient (EMT) and phasor-based simulation was conducted. Case studies of a two-inverter small microgrid and a modified version of the IEEE 34-Node Test System that has seven grid-forming inverters show that phasor-based simulation agrees well with EMT simulation when the P-f droop gains of grid-forming inverter controllers are within normal ranges. However, under extremely high P-f droop gains, phasor-based simulation can result in over-optimistic stability results. This study provides insight into the applicability of phasor-based simulation for the stability of feeder-level, inverter-based microgrids.

Du, Wei↗