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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Preparation and Characterization Methods of Thin Layer Samples for Standoff Detection

Detection of analytes deposited on surfaces is crucial for many applications: Development of methods to prepare thin layers (e.g. ~5 to 100 µm) is important for both system design and field studies. In this work, solid and liquid analytes were deposited on painted and bare substrates including aluminum, glass, plastic, and concrete using an ExactaCoat ultrasonic spray coater. Laboratory hemispherical reflectance (HRF) spectra were collected for samples with different layer thicknesses so as to characterize both the composition and layer thickness. Preliminary results demonstrate that to prepare homogenous layers on surfaces, parameters such as substrate type, analyte solubility, vapor pressure, paint color, surface porosity, and surface roughness are all important. Liquid chemicals posed several issues during deposition: Diisopropyl methyl phosphonate evaporated from surfaces more quickly than the other chemicals and was thus not detected in the HRF experiments. Less volatile liquids, such as tributylphosphate, remained on the surface for the duration of the test, but a uniform layer thickness could not be obtained as the liquid pooled to one side when mounted at an angle. The deposition of solids (e.g., acetaminophen, caffeine and methylphosphonic acid) from volatile solvents such as chloroform also proved problematic due to streaking caused by rapid solvent evaporation. Solids deposited from ethanol, however, worked well on bare substrates. For most samples plotting the integrated infrared band strength vs. surface thicknesses showed a linear relationship, confirming that the surface loading can be controlled by programming the concentration and the number of passes on the ultrasonic sprayer.

Thin layer, deposition, infrared standoff, Hemisph↗
DOE OSTI2023

Accelerated test protocols to predict service life and durability of solid oxide fuel cells

Reliable accelerated test protocols are needed for solid oxide fuel cell research to facilitate rapid learning on key durability issues, identify potential modes of failure expeditiously, and eventually predict the calendar lifetime of an electrochemical cell. In this work, solid oxide fuel cells operated at a constant current density were compared to cells undergoing accelerated measurements, which are composed of intermittent current injection to the cell. A general accelerated test profile was developed by cycling a solid oxide fuel cell from open circuit to a predetermined operating current density that is the same as the current density during a steady-state operation, to accelerate the local redox environment. The following parameters were studied: current density, operation temperature, moist level, sintering temperature, cycling current, cycling frequency, and operation time. Up to 1,320,000 cycles were generated in this work. The cell degradation was accelerated by nearly 10 times, suggesting the feasibility of using this protocol for acceleration test to predict life performance and durability of solid oxide fuel cells.

08 HYDROGEN↗
DOE OSTI2023

Triplet Generation Through Singlet Fission in Metal-Organic Framework: An Alternative Route to Inefficient Singlet-Triplet Intersystem Crossing

High quantum yield triplets, populated by initially prepared excited singlets, are desired for various energy conversion schemes in solid working compositions like porous MOFs. However, a large disparity in the distribution of the excitonic center of mass, singlet-triplet intersystem crossing (ISC) in such assemblies is inhibited, so much so that a carboxy-coordinated zirconium heavy metal ion cannot effectively facilitate the ISC through spin-orbit coupling. Circumventing this sluggish ISC, singlet fission (SF) is explored as a viable route to generating triplets in solution-stable MOFs. Efficient SF is achieved through a high degree of interchromophoric coupling that facilitates electron super-exchange to generate triplet pairs. Here we show that a predesigned chromophoric linker with extremely poor ISC efficiency (k ISC ) but E S 1 ≥ 2E T 1 form triplets in MOF in contrast to the frameworks that are built from linkers with sizable k ISC but E S 1 ≤ 2E T 1 . Finally, this work opens a new photophysical and photochemical avenue in MOF chemistry and utility in energy conversion schemes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Increased damping through captured powder in additive manufacturing

This paper describes the retention of metal powder within additively manufactured structures to achieve increased damping. In this work, solid and hollow (powder filled) aluminum cylinders were fabricated in using laser powder bed fusion where the internal, captured powder in the hollow cylinders served as an energy dissipation mechanism. Impact testing was completed to compare the frequency response functions of three cylinder geometries: one solid cross-section and two hollow cross-sections with different inner diameters and, therefore, different powder volumes. Increased damping with larger inner diameter was observed. The damping was quantified using a structural damping model.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Synthesis and characterization of polylactic acid microspheres via emulsion-based processing

Polylactic acid (PLA) microspheres are primarily used in drug delivery applications and rarely manufactured commercially. In encapsulation, the drug encapsulation and microsphere synthesis process happen simultaneously. Simultaneous synthesis necessitates conditions that ensure the drugs to be encapsulated remain viable in the synthesis process. Here, in the present work, solid pure PLA microspheres are prepared using a repeatable centrifugal mixing method to create a single emulsion system. A planetary thinky mixer is used to achieve centrifugal mixing. PLA acts as the dispersed phase of the emulsion, whereas Polyvinyl alcohol (emulsifier) dissolved in deionized water serves as the bulk phase. The emulsions are stirred for about 4 min at 2000 rpm. Microspheres prepared by mechanical mixing are compared with microspheres prepared by centrifugal mixing. The microspheres prepared by centrifugal mixing proved to be narrower and closer to a normal distribution with a mean size (D x 50) of 30 microns. The size distribution of planetary mixed microspheres did not change from one batch to another.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Assessment of diffuse-interface methods for compressible multiphase fluid flows and elastic-plastic deformation in solids

This work describes three diffuse-interface methods for the simulation of immiscible, compressible multiphase fluid flows and elastic-plastic deformation in solids. The first method is the localized-artificial-diffusivity approach of Cook, Subramaniam et al., and Adler and Lele, in which artificial diffusion terms are added to the individual phase mass fraction transport equations and are coupled with the other conservation equations. The second method is the gradient-form approach that is based on the quasi-conservative method of Shukla et al., in which the diffusion and sharpening terms (together called regularization terms) are added to the individual phase volume fraction transport equations and are coupled with the other conservation equations. The third approach is the divergence-form approach that is based on the fully conservative method of Jain et al., in which the regularization terms are added to the individual phase volume fraction transport equations and are coupled with the other conservation equations. In the present study, all three diffuse-interface methods are used in conjunction with a four-equation, multicomponent mixture model, in which pressure and temperature equilibria are assumed among the various phases. The primary objective of this work is to compare these three methods in terms of their ability to: maintain constant interface thickness throughout the simulation; conserve mass, momentum, and energy; and maintain accurate interface shape for long-time integration. The second objective of this work is to consistently extend these methods to model interfaces between solid materials with strength. To assess and compare the methods, they are used to simulate a wide variety of problems, including (1) advection of an air bubble in water, (2) shock interaction with a helium bubble in air, (3) shock interaction and the collapse of an air bubble in water, and (4) Richtmyer–Meshkov instability of a copper–aluminum interface. The current work focuses on comparing these methods in the limit of relatively coarse grid resolution, which illustrates the true performance of these methods. In conclusion, this is because it is rarely practical to use hundreds of grid points to resolve a single bubble or drop in large-scale simulations of engineering interest.

97 MATHEMATICS AND COMPUTING↗
DOE OSTI2020

Challenges for and Pathways Toward Solid-State Batteries

Solid-state batteries utilizing lithium metal anodes have the potential to enable batteries with a specific energy of >500 Wh/kg and an energy density of >1,500 Wh/L for thousands of cycles. When optimized they will improve the energy efficiency, operating temperature range, sustainability, and safety at a lower cost compared to projections for advanced Li-ion batteries. This improved performance is critical for the widespread adoption of electric vehicles and may enable future applications such as electric aviation. Expectations for solid-state batteries are high, there are significant materials and processing challenges that need to be overcome. Some of these challenges are well known; others are more subtle and are just becoming known. The challenges and their solutions must be clearly identified to realize high-energy solid-state Li metal batteries. In the United States, the U.S. Department of Energy (DOE) funds the majority of energy storage research and development, including solid state battery research. Web of Science publication analysis shows that worldwide DOE is second largest funder. Work on solid state batteries is distributed across different arms of DOE and is coordinated at headquarters to ensure a broad national portfolio for advanced batteries, including lithium batteries and solid-state battery devices. We note that university and national laboratory researchers in the US with a long-standing interest in solid state batteries is a small, integrated community with recognized impact for publications, patents and startup companies. The opportunity for this group to engage for research with international colleagues is growing, fostered by periodic bilateral meetings supported by DOE and by the recent joint US German research program for lithium battery interface studies. These are valuable opportunities to speed solid-state battery development. The ORNL led virtual workshop, overviewed here, confirms the community’s shared vision of the exciting advances, opportunities, and challenges. Further, we are seeing that this workshop has spawned several new informal collaborations and draft proposals. This encourages us to propose future discussion. On May 11, 2020, Oak Ridge National Laboratory (ORNL) hosted a 6-hour, on-line national workshop to discuss recent advances and most the prominent obstacles to realizing solid-state Li metal batteries. The workshop included more than 30+ experts from national laboratories, universities, and companies, all of whom have worked on solid-state batteries for multiple years. The participants shared recent advances, many not yet in print, illustrating that the community has gained significant new insights for solid-state Li battery materials over the last 5 years. In this report, the major outcomes of the workshop are organized to identify the gaps in our scientific knowledge for four core materials science areas: (1) Li metal anodes, (2) the solid electrolyte in contact with Li metal, (3) active cathode materials and solid-state composite cathodes, and (4) solid electrolytes. Illustrative examples and discussions are reported with the more comprehensive issues in the report. Discussion of additional challenges related to processing of solid-state battery materials and to the designs and architectures for mechanically robust, long-lived batteries received less attention due to time constraints. These are good themes for deeper discussion at a follow-on workshop, where a complete list of critical research topics can be identified.

25 ENERGY STORAGE↗
DOE OSTI2020

Synthesis, structure, and transport properties of Ba 8 Cu 16 – x Au x P 30 clathrate solid solution

In this work, a new clathrate solid solution Ba 8 Cu 16 – x Au x P 30 ( x = 4, 8, 12) was synthesized by a high-temperature solid-state annealing method. The crystal structures of Ba 8 Cu 16 – x Au x P 30 were determined by single crystal x-ray diffraction. This clathrate solid solution crystallizes in the orthorhombic superstructure of clathrate-I type with 23 crystallographically independent framework sites, eight of them are occupied by Au/Cu and 15 are exclusively occupied by P atoms. The distribution of Au and Cu atoms over these eight framework sites is not random with a clear preference for Au to occupy the largest (Au/Cu)P 4 tetrahedra in the framework. The thermal stability and thermoelectric properties of the Ba 8 Cu 16 – x Au x P 30 solid solution were evaluated. Low thermal conductivity was achieved for Ba 8 Cu 16 – x Au x P 30 due to the combination of the host–guest crystal structure with rattling Ba atoms with the presence of heavy Au atoms and substitutional Cu/Au disorder in the clathrate framework.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Morphology selection in dealloying: A phase field study of the coupling among kinetic mechanisms

A phase field model is used to investigate how the corrosion rate and morphology of a dealloying metal is controlled by the kinetic rates of bulk solid diffusion, interfacial diffusivity, and interface dissolution. A specific focus is investigating the manner by which variations in these kinetic parameters synergistically influence the onset of a morphological instability at the solid-liquid interface, which is known to precede rapid dealloying corrosion towards highly topologically complex structures such as bicontinuous porous solids. This work demonstrates that this instability can be suppressed by either an increase of interdiffusion in the solid alloy, or by a decreasing rate of dissolution at the solid-liquid interface. When the instability is suppressed, the result is a relatively planar, passivated dealloying front. Importantly, however, coupled changes in kinetic parameters can also promote the morphological instability and sustain fine-scale ligament and pore formation. Finally, the relevance of the solid-liquid interfacial diffusion for determining the rate of dealloying and ligament formation is highlighted. By elucidating the mechanistic influence of bulk and interfacial kinetic factors on the dealloyed morphology, this work helps to rationalize the contrasting morphologies observed in various dealloying systems.

Diffusion↗
DOE OSTI2026

All‐Solid‐State Batteries With Mechanically Stable Interfaces Consisting of a Zero‐Strain Cation‐Disordered Rocksalt Cathode

Interface stabilization is critical to the development of working all‐solid‐state batteries. Rigid cathode/solid electrolyte interfaces often disintegrate due to anisotropic volume change of cathode‐active materials, resulting in irreversible capacity loss. Herein, we demonstrate that Li 1.211 Mo 0.467 Cr 0.3 O 2 (LMCO), a pioneering cation‐disordered rocksalt oxide (DRX) cathode that has intrinsically small volume change upon lithium intercalation, can be integrated with a thiophosphate‐based solid electrolyte for all‐solid‐state batteries. Interface stability of the all‐solid LMCO cell was investigated by electrochemical impedance spectroscopy, X‐ray micro‐computed tomography, and electron microscopy. Since LMCO was initially synthesized as a layered phase exhibiting a large volume change, interface disintegration can be observable in the early cycles. As layered LMCO phase‐transformed into DRX LMCO in subsequent cycles, reintegration of the interfaces occurs within a pressurized cell as a result of its zero‐stain behavior. Consequently, the DRX LMCO cathode maintains interface integrity, and thus electrical wiring, over an extended number of cycles, leading to improved capacity retention with small internal cell resistance.

DRX↗
DOE OSTI2020

Ultrasonic waves from radial mode excitation of a piezoelectric disc on the surface of an elastic solid

In this work, we discuss the ultrasonic wave propagation characteristics in an isotropic elastic solid due to the radial mode excitation of a piezoelectric disc actuator bonded to its surface. Finite element simulations using coupled electromechanical modeling is employed to investigate the wave propagation behavior. We find that the radial mode vibrations on the surface of the elastic solid generates all the three types of ultrasonic waves: longitudinal, shear, and surface waves. The waves in the solid are comprised of a central lobe and multiple side lobes based on the frequency of the radial mode excitation. The central lobe is predominantly composed of longitudinal waves and the side lobes are composed of shear waves. While the longitudinal waves have a strong central lobe and weak side lobes that are not fully developed, shear waves consists of fully developed side lobes. In addition, we observe that the longitudinal waves have fewer side lobes inside the solid compared to the shear waves. A semi-analytical approach is presented to explain the above observations. The interface traction boundary condition between the piezoelectric disc and the elastic solid is approximated as a truncated 'Bessel' excitation over the area of the piezoelectric disc in contact with the solid. A Fourier–Bessel series expansion technique is used to investigate the wave propagation behavior from the above traction boundary condition. The results obtained explain the observations from the finite element simulations with regard to the number and distribution of side lobes pertaining to the longitudinal and shear waves generated from the radial modes of the piezoelectric disc. The proposed semi-analytical approach is general and can be applied to any arbitrary axisymmetric excitations on the surface of an elastic solid.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Perovskite Oxide–Halide Solid Solutions: A Platform for Electrocatalysts

The successful integration or hybridization of perovskite oxides with their halide cousins would enable the formation of both multi-anionic and multi-cationic solid solutions with unique metal-ion sites and synergistic properties that could potentially surpass the performance of classic perovskites. However, such solid solutions had not been produced previously owing to their distinct formation energies and different synthesis conditions. Solid solutions combining perovskite oxides with fluorides were produced in this study by mechanochemical synthesis. The obtained perovskite oxide–halide solid solutions had highly mixed elements and valences, uniform element distributions, and single-phase crystalline structures. In this work, the solid solution with an optimized combination of oxides and fluorides exhibited enhanced catalytic performance in the oxygen evolution reaction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Locally developed electronic conduction in a yttria stabilized zirconia (YSZ) electrolyte for durable solid oxide fuel cells

In the present work, anode supported solid oxide fuel cells (SOFCs) based on a YSZ single layer electrolyte with locally developed electronic conduction near the anode side is fabricated to improve the cell durability under negative voltage conditions. A ceria added Ni/YSZ anode functional layer is utilized and co-sintered with the YSZ electrolyte at 1460 °C. Cerium ions are diffused into a limited region of the YSZ layer (~6 μm), establishing a ceria doped YSZ region. We successfully demonstrate that this YSZ single layer cell can operate stably for ~100 h without anode/electrolyte interface delamination, even under a negative voltage. The embedded probe technique and theoretical calculation reveal that the internal oxygen partial pressure (near the anode) is substantially reduced (stabilized) by means of local electronic conduction of ceria doped YSZ. Thus, we propose an SOFC electrolyte design comprising a YSZ single layer with a ceria added anode functional layer (locally formed ceria doped YSZ in the electrolyte) as a protection method against fuel cell stack degradation caused by negative voltage operation.

25 ENERGY STORAGE↗
DOE OSTI2023

Characterization of solid particle candidates for application in thermal energy storage and concentrating solar power systems

Thermal energy storage (TES) enables concentrating solar power to remain competitive in the renewable energy mix by firming up intermittent solar resource and providing grid services such as load shifting. Free from siting constraints, stand-alone TES systems show promise as a low-cost alternative to traditional pumped-storage hydropower or compressed air energy storage. At the core of all TES technologies is a storage medium, the selection of which governs many aspects of system design and operation. Although the majority of commercial installations utilize molten salts, solid particles can demonstrate stability over wider temperature ranges. This amounts to increased energy storage densities and corresponding reductions in system cost which is essential in achieving low-cost energy storage. In this work, eight solid particle candidates are systematically identified and screened for application in a specific particle-TES system. The five most promising candidates (CARBO CP and HSP, calcined flint clay (CFC), brown fused alumina (BFA), and silica sand) are further characterized by size and morphology for fluidization suitability, flowability for particle transport, and thermal stability. Calcined flint clay and brown fused alumina are eventually down-selected due to thermal instability at the target operational temperature of 1200 °C. Although the physical characteristics of CARBO outperform silica sand in all categories examined, the marginal performance gains are considered insufficient to justify the additional media cost so silica sand is selected as the leading candidate. Within the silica sand (α-quartz) space, the high end of Geldart Group B particles is identified to satisfy the target fluidization regime for the application of interest without compromising particle flowability. Here, in focused testing, Silica 460 is shown to exhibit sufficient stability through long-duration (500-hour) thermal and cyclic testing (1200 °C), 10-hour testing at 1400 °C, and in contact with candidate refractory containment materials. Finally, an average heat capacity of 1.1 J/g∙ °C is measured over 300-1200 °C with a quartz inversion enthalpy (ΔH α-β ) of 10.7J/g.

14 SOLAR ENERGY↗
DOE OSTI2025

In Situ Diffraction and Ex Situ Transmission X‐Ray Microscopy Studies of Solid‐State Upcycling for NMC Cathodes

Upcycling of recycled LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622) cathodes offers an economical route to produce cathode materials with increased energy density (i.e., LiNi 0.8 Mn 0.1 Co 0.1 O 2 , NMC811) that meet the performance needs of present-day electric vehicles. In this work, solid-state upcycling of NMC622 via calcination with Ni(OH) 2 and LiOH was monitored using in situ synchrotron powder X-ray diffraction measurements. Sequential Rietveld refinements indicate that the calcination proceeds by initially converting Ni(OH) 2 to a rocksalt NiO phase followed by lithiation of NiO to form LiNiO 2 (LNO), with both NMC and LNO phases present in nearly equal proportions at the calcination endpoint. Variable-energy transmission X-ray microscopy tomograms of upcycled samples reveal that the NMC and LNO domains are intermixed at sub-micron length scales. Depth-dependent analysis of multi-elemental fitting maps matches the expected NMC811 composition at the secondary particle level and indicates that transition metal diffusion is not limited by the secondary particle size.

cathode upcycling↗
DOE OSTI2022

Fully self-consistent finite-temperature $GW$ in Gaussian Bloch orbitals for solids

In this work, we present algorithmic and implementation details for the fully self-consistent finite-temperature $GW$ method in Gaussian Bloch orbitals for solids. Our implementation is based on the finite-temperature Green's function formalism in which all equations are solved on the imaginary axis, without resorting to analytical continuation during the self-consistency. No quasiparticle approximation is employed and all matrix elements of the self-energy are explicitly evaluated. The method is tested by evaluating the band gaps of selected semiconductors and insulators. We show agreement with other, differently formulated, finite-temperature sc ⁢$GW$ implementations when finite-size corrections and basis-set errors are taken into account. By migrating computationally intensive calculations to graphics processing units, we obtain scalable results on large supercomputers with nearly optimal performance. Our work demonstrates the applicability of Gaussian orbital based sc⁢ $GW$ for ab initio correlated material simulations and provides a sound starting point for embedding methods built on top of $GW$.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Spin Glass Behavior and Giant Magnetoresistance via Aliovalent Fe/Ni Alloying in Amorphous Tetrathiafulvalene-Tetrathiolate Coordination Polymers

The discovery of materials with programmable combinations of charge transport and magnetic properties is a major goal in synthetic chemistry. Molecular materials, such as coordination polymers (CPs), are emerging candidates in this field due to their synthetic modularity. While there are many conductive or magnetic CPs, single-component examples with both properties are still emerging. Here, in this work, we demonstrate how alloying paramagnetic Fe(III) centers into a highly conductive Ni-based CP results in novel amorphous materials with high conductivity and giant magnetoresistance. Aliovalent doping with paramagnetic Fe centers engenders spin-glass transitions, while Ni and the strong π-stacking interactions of tetrathiafulvalene-2,3,6,7-tetrathiolate (TTFtt) ligands support conductivity. Ni 0.69 Fe 0.31 TTFtt has σ ≈ 200 S/cm and a 1.8 K magnetoresistance of −52% at 5 T, among the largest for any coordination solid. This work demonstrates not only how magnetic properties can be rationally incorporated into conductive CPs, but also an unexpected potential for amorphous materials in spintronic applications.

amorphous materials↗
DOE OSTI2021

Implementation of an Experimental Setup Based on the Three-Omega Method for Thermal Conductivity Measurements of Molten Salts

Molten salt reactors (MSRs) are one of the most promising next-generation nuclear reactor designs which use molten salts as the fuel and coolant. To design, model, predict, license, and operate MSRs, the behavior of the fuel and coolant must be understood as a function of temperature and irradiation, i.e., burnup. Of particular importance and complexity is the reliable and reproducible measurement of thermal conductivity of molten salts at high temperatures (> 500 °C). Thermal conductivity provides information on the rate at which heat passes through a specified material and is dependent on chemical composition. Currently, in the national laboratory complex, several methods for measuring thermal conductivity on molten salt systems are under development, however, to date, consistent data have not been produced. Typically, thermal conductivity measurements of high-temperature melts have been conducted by using the Transient Hot Wire (THW) method where thermal conductivity is determined by the change in temperature over time at a certain distance from a heating wire. Another time-dependent technique is the laser flash method, commonly used for solid samples. Laser flash requires prior measurements of density and heat capacity to calculate the thermal conductivity of the sample, introducing additional measurement errors. Steady state and time-dependent measurements such as THW and laser flash have errors from convection and ambient temperature fluctuations (heat radiation). In order to produce high fidelity thermal conductivity data, a measurement technique needs to be developed that will reduce the effect of convection at high temperatures by measuring in a very fast time window. In addition, to measure on actinide and irradiated salts the sample size should be small. Therefore, this project aims to develop a frequency-domain technique based on the three-omega (3?) method, previously proven to work on solids, nanofluids and low temperature solar salts (25 to 250 °C). If the 3?-device can be designed with materials that can withstand high temperatures (>500 °C) and can be configured to reduce errors due to convection, then it would prove to be a valuable technique for ensuring thermal conductivity on molten salt systems needed for MSR development. For this proposal, the 3? instrument will be designed, assembled, and tested on non-radioactive salts before being used on actinide bearing salts. In addition, a thermal model will be developed to determine the thermal conductivity of the sample from the measured thermal oscillation of the sensor. Because 3? is a direct method that requires a small volume of sample and works in a very fast time window, it will aid in suppressing the interference due to convection which is ideal when working with high temperature liquid samples.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗