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At least 253 records · Page 14

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DOE OSTI2024

Competitive Valerate Binding Enables RuO 2 -Mediated Butene Electrosynthesis in Water

The (non)-Kolbe oxidation of valeric acid, sourced from a hydrolysis product of cellulose, provides a sustainable synthetic route to access value-added products, such as butene. An essential mechanistic step preceding product formation involves the oxidative and decarboxylative cleavage of a C–C bond. Yet, the role of the electrode surface in mediating this oxidative step remains an open question: the electron transfer can occur either via an inner-sphere or outer-sphere mechanism. Here, we report the electrochemical, in situ spectroscopic, computational, and reactivity studies of RuO 2 -mediated oxidative decarboxylation of valeric acid to butene in aqueous electrolytes. We find that carboxylates bind to RuO 2 anode surfaces at potential values where decarboxylation products are observed. Our results are consistent with a reaction scheme where the competitive and catalytic oxygen evolution reaction (OER) is impeded by these bound carboxylate species while these species are inert toward butene formation. Our results implicate an outer-sphere electron transfer mechanism for decarboxylation where the surface chemistry of the RuO 2 electrode serves to enable higher non-Kolbe reaction selectivity by suppressing the parasitic OER. Furthermore, our findings delineate interfacial design principles for selective electrochemical systems that utilize water as the ultimate oxidant for sustainable decarboxylation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Penrose process for a charged black hole in a uniform magnetic field

Spinning black holes create electromagnetic storms when immersed in ambient magnetic fields, illuminating the otherwise epically dark terrain. In an electromagnetic extension of the Penrose process, tremendous energy can be extracted, boosting the energy of radiating particles far more efficiently than the mechanical Penrose process. We locate the regions from which energy can be mined and demonstrate explicitly that they are no longer restricted to the ergosphere. Here we also show that there can be toroidal regions that trap negative energy particles in orbit around the black hole. We find that the effective charge coupling between the black hole and the superradiant particles decreases as energy is extracted, much like the spin of a black hole decreases in the mechanical analogue. While the effective coupling decreases, the actual charge of the black hole increases in magnitude reaching the energetically-favored Wald value, at which point energy extraction is impeded. We demonstrate the array of orbits for products from the electromagnetic Penrose process.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2023

Origin of the lithium metal anode instability in solid-state batteries during discharge

Enabling the lithium metal anode (LMA) in solid-state batteries (SSBs) would increase energy density and specific energy compared with lithium-ion batteries. However, pore formation in LMAs with irregular morphology, even at low current density, during discharge results in an unstable, high-impedance interface. Understanding and addressing this inherent anode instability is essential for increasing the power densities in SSBs. Herein, we suggest that the morphology of the stripped electrode is related to dislocations in the LMA. To investigate the influence of dislocations, symmetric cells, Li|Li 6.25 Al 0.25 La 3 Zr 2 O 12 (LLZO)|X-Li, are studied, where X-Li represents the microstructurally controlled LMA obtained via suitable thermomechanical processing. Operando impedance measurements are corroborated with SEM, confocal microscopy, and AFM data. Based on the experimental observations, a mechanism for pore formation is proposed. Here we show that the stack pressure required to maintain a stable interface is governed by the lithium microstructure and its thermomechanical processing history.

25 ENERGY STORAGE↗

DOE OSTI2023

Guided anisotropic oxygen transport in vacancy ordered oxides

Abstract Anisotropic and efficient transport of ions under external stimuli governs the operation and failure mechanisms of energy-conversion systems and microelectronics devices. However, fundamental understanding of ion hopping processes is impeded by the lack of atomically precise materials and probes that allow for the monitoring and control at the appropriate time- and length- scales. In this work, using in-situ transmission electron microscopy, we directly show that oxygen ion migration in vacancy ordered, semiconducting SrFeO 2.5 epitaxial thin films can be guided to proceed through two distinctly different diffusion pathways, each resulting in different polymorphs of SrFeO 2.75 with different ground electronic properties before reaching a fully oxidized, metallic SrFeO 3 phase. The diffusion steps and reaction intermediates are revealed by means of ab-initio calculations. The principles of controlling oxygen diffusion pathways and reaction intermediates demonstrated here may advance the rational design of structurally ordered oxides for tailored applications and provide insights for developing devices with multiple states of regulation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

High-performance Ruddlesden–Popper perovskite oxide with in situ exsolved nanoparticles for direct CO 2 electrolysis

Carbon dioxide (CO 2 ) is one of the principal greenhouse gases accountable for global warming and extreme climate changes. Electrochemically converting CO 2 into carbon monoxide (CO) is a promising approach for CO 2 utilization in achieving industrial decarbonization. High-temperature CO 2 electrolysis via solid oxide electrolysis cells (SOECs) has great potential, including high-energy efficiency, fast electrode kinetics, and competitive cost; however, this technology still has challenges associated with developing highly active, robust CO 2 electrodes for SOECs. We report novel Ruddlesden–Popper structured Pr 1.2 Sr 0.8 Mn 0.4 Fe 0.6 O 4–δ (RP-PSMF) with in situ exsolved Fe nanoparticles as the CO 2 electrode in SOECs for direct CO 2 conversion to CO. The mechanism of CO 2 electrolysis is studied by using the distribution of relaxation times method from electrochemical impedance spectroscopy. La 0.8 Sr 0.2 Ga 0.8 Mg 0.2 O 3–δ (LSGM)-electrolyte supported SOECs with the RP-PSMF cathode have achieved exceptionally high current densities of 2.90, 1.61, 0.91, and 0.48 A·cm –2 at an applied voltage of 1.5 V at 800, 750, 700, and 650 °C, respectively. Moreover, SOECs with the RP-PSMF cathode have exhibited a stable electrolysis performance for 100 h under a current cycling operation. Here, these results suggest that RP-PSMF with exsolved Fe nanoparticles is a highly promising cathode for high-temperature direct CO 2 electrolysis cells.

03 NATURAL GAS↗

DOE OSTI2021

Simulations of Nb$_3$Sn Layer RF Field Limits Due to Thermal Impedance

Nb3Sn performance in RF fields is limited to fields far below its superheating critical field. Poor thermal conductivity of Nb3Sn has been speculated to be the reason behind this limit. In order to better understand the contribution of Nb3Sn thermal conductivity to its RF performance, we simulated numerically with Matlab program*(based on SRIMP and HEAT codes) thelimiting fields under different realistic conditions. Our simulations indicate that limiting fields observed presently in the experiments with RF fields cannot be explained by the thermal impedance of Nb3Sn alone. The results change significantly in the presence of higher losses due to extrinsic mechanisms.

43 PARTICLE ACCELERATORS↗

NASA NTRS1974

High-efficiency, low-temperature cesium diodes with lanthanum-hexaboride electrodes

Lanthanum hexaboride electrodes in 1700 K cesium diodes may triple power outputs compared with those demonstrated for nuclear thermionic space applications. Still greater relative gains seem possible for emitters below 1700 K. Further improvements in cesium diode performance should result from the lower collector temperatures allowed for earth and low power space duties. Decreased temperatures will lessen thermal transport losses that attend thermionic conversion mechanisms. Such advantages will add to those from collector Carnot and electrode effects. If plasma ignition difficulties impede diode temperature reductions, recycling small fractions of the output power could provide ionization. So high efficiency, low temperature cesium diodes with lanthanum hexaboride electrodes appear feasible.

Morris, J. F.↗

NASA NTRS1984

Analysis of an infinite array of rectangular microstrip patches with idealized probe feeds

A solution is presented to the problem of an infinite array of microstrip patches fed by idealized current probes. The input reflection coefficient is calculated versus scan angle in an arbitrary scan plane, and the effects of substrate parameters and grid spacing are considered. It is pointed out that even when a Galerkin method is used the impedance matrix is not symmetric due to phasing through a unit cell, as required for scanning. The mechanism by which scan blindness can occur is discussed. Measurement results are presented for the reflection coefficient magnitude variation with angle for E-plane, H-plane, and D-plane scans, for various substrate parameters. Measured results from waveguide simulators are also presented, and the scan blindness phenomenon is observed and discussed in terms of forced surface waves and a modified grating lobe diagram.

Pozar, D. M.↗

NASA NTRS2015

Random Vibration Testing of Advanced Wet Tantalum Capacitors

Advanced wet tantalum capacitors allow for improved performance of power supply systems along with substantial reduction of size and weight of the systems that is especially beneficial for space electronics. Due to launch-related stresses, acceptance testing of all space systems includes random vibration test (RVT). However, many types of advanced wet tantalum capacitors cannot pass consistently RVT at conditions specified in MIL-PRF-39006, which impedes their use in space projects. This requires a closer look at the existing requirements, modes and mechanisms of failures, specifics of test conditions, and acceptance criteria. In this work, different lots of advanced wet tantalum capacitors from four manufacturers have been tested at step stress random vibration conditions while their currents were monitored before, during, and after the testing. It has been shown that the robustness of the parts and their reliability are mostly due to effective self-healing processes and limited current spiking or minor scintillations caused by RVT do not increase the risk of failures during operation. A simple model for scintillations events has been used to simulate current spiking during RVT and optimize test conditions. The significance of scintillations and possible effects of gas generation have been discussed and test acceptance criteria for limited current spiking have been suggested.

cracking↗

NASA NTRS2015

Random Vibration Testing of Advanced Wet Tantalum Capacitors

cracking↗

NASA NTRS2015

Random Vibration Testing of Advanced Wet Tantalum Capacitors

wet tantalum capacitors↗

NASA NTRS2023

Molecular Dynamics Simulations of Austenite-Martensite Interfaces in NiTi Shape Memory Alloys

The unique properties of shape memory alloys (SMAs) arise from a reversible martensitic transformation. The nucleation and migration of austenite-martensite interfaces are the key to understanding the SMA properties. Molecular dynamics (MD) simulations can provide important atomic-scale information about these aspects of the transformation, but their time scales prevent the interface formation under near-equilibrium conditions relevant to experiment. We present a new MD methodology which allows for the natural formation of energetically preferred austenite-martensite interfaces under near-equilibrium conditions. Our simulation demonstrates that the interfaces in NiTi are semi-coherent, composed of a series of terrace planes and structural disconnections, and they migrate rapidly through single crystals with only a small thermodynamic driving force. In bi-crystals and polycrystals, the migration of these same interfaces is significantly impeded by grain boundaries and stored elastic energy. This behavior can result in SMA hysteresis via several mechanisms associated with nucleation and non-elastic strain accommodation.

Gabriel Plummer↗

NASA NTRS2013

Properties and Performance Attributes of Novel Co-extruded Polyolefin Battery Separator Materials: Electrical Properties - Part 2

As NASA prepares for its next era of manned spaceflight missions, advanced energy storage technologies are being developed and evaluated to address and enhance future mission needs and technical requirements. Cell-level components for advanced lithium-ion batteries possessing higher energy, more reliable performance and enhanced, inherent safety characteristics have been under development within the NASA infrastructure. A key component for safe and reliable cell performance is the cell separator, which separates the two energetic electrodes and functions to inhibit the occurrence of an internal short circuit but preserves an ionic current. Recently, a new generation of co-extruded separator films has been developed by ExxonMobil Chemical and introduced into their battery separator product portfolio. Several grades of this new separator material were evaluated with respect to dynamic mechanical properties and safety-related performance attributes, and the results of these evaluations were previously reported in "Part 1: Mechanical Properties" of this publication. This current paper presents safety-related performance results for these novel materials obtained by employing a complementary experimental methodology, which involved the analysis of separator impedance characteristics as a function of temperature. The experimental results from this study are discussed with respect to potential cell safety enhancement for future aerospace as well as for terrestrial energy storage needs, and they are compared with pertinent mechanical properties of these materials, as well as with current state-of-the practice separator materials.

Baldwin, Richard S.↗

DOE OSTI2024

Electrolyte and Cutoff Potential Effects on Cycle Life of Li4Ti5O12/LiNi0.9Mn0.1O2 Batteries for Behind-the-Meter Storage Applications

Behind-the-Meter Storage (BTMS) is a stationary battery energy storage system that is connected to the electrical distribution system on the customer's side of the utility's service meter. BTMS systems are used to store electrical energy from the grid as well as inconstant, renewable energy, such as local solar and wind generation. A successful BTMS system will allow the customer to pair their energy generation and storage to optimize electrical consumption from the grid, improving reliability and minimizing cost. For BTMS applications, batteries must be designed and optimized with different set of criteria from other leading segments of the Li-ion battery market, like transportation, due the system being stationary and proximal to the residential or commercial building it's benefitting. BTMS applications prioritize safety, cost (low/no-critical materials), reliability (20-year calendar life), and durability (10,000 cycle life), while having the ability to (minimally) compromise energy density and rate capability. Lithium titanate (Li4Ti5O12-, LTO) is a promising anode candidate for BTMS applications due to its high safety and capacity retention, while maintaining a reasonable 160 mAhg-1 reversable capacity and composition of relatively abundant materials. (1) Specifically, LTO has a high working voltage which helps to prevent Li dendrite formation, improving safety. Furthermore, LTO also has negligible lithiation-based volume change, leading to less mechanical pulverization, or loss of active material, upon cycling. For the cathode, materials with little or no Co are of high interest due to the high cost and low abundance of Co. LiMn2O4 (LMO) has been paired with LTO for BTMS applications in the past due to its safety, low cost (abundancy), and reasonably high operating voltage. (2-4) However, the low capacity of LMO limits energy density and specific energy. While not the highest priority for BTMS applications, increasing energy density will enable deployment in space constrained BTMS applications and decrease total cost. LiNi0.9Mn0.1O2 (LN-MO) is a recently developed material with promise due to its high operating voltage and relatively low price. (5) However, Ni-rich layered oxides, including LNMO, tend to struggle with capacity retention during high-voltage cycling due to mechanical pulverization, irreversible phase transitions, and unstable solid-electrolyte interphase. The study presented here focuses on building an understanding of how electrolyte solvent and varied cutoff potentials will impact the cycle life of LTO/LN-MO cells. Specifically, a comparison is provided between ethylene carbonate (EC), ethyl methyl carbonate (EMC), fluoroethylene carbonate (FEC), and Gen2 electrolyte solvents with 1M Lithium hexafluorophosphate (LiPF6) salt, cycling to two upper termination potentials, 2.6V and 2.7V. Electrochemical testing and diagnostics (e.g., differential capacity analysis, area specific impedance, constant voltage hold, and rate capability) and post-mortem characterization will be used to understand the aging behavior and failure mechanisms of the 8 cell combinations (four electrolytes and two voltage cutoffs). Cells with FEC electrolyte showed a lower initial capacity compared to cells with Gen2, EMC, and EC cycling at both voltages; however, the cells with FEC showed consistent trends in capacity retention with 2.6V and 2.7V termination potentials, while the cells with the other electrolytes showed much higher rates of capacity loss when cycling to the higher voltage. These results indicate that FEC may play a role in improving durability of high-voltage, Ni-rich electrode systems for use in high-cycle applications, such as BTMS.

electrolyte↗

NASA NTRS1982

Nondestructive evaluation techniques for nickel-cadmium aerospace battery cells

The ac impedance characteristics of Ni-Cd cells as an in-situ, nondestructive means of determining cell lifetime, particularly with respect to the probability of premature failure were evaluated. Emphasis was on evaluating Ni-Cd cell impedance over a wide frequency range (10,000 to 0.0004 Hz) as the cells were subjected to charge/discharge cycle testing. The results indicate that cell degradation is reflected in the low frequency (Warburg) impedance characteristics associated with diffusion processes. The Warburg slope (W) was found to steadily increase as a function of cell aging for completely discharged cells. In addition, based on data for two cells, a high or rapidly increasing value for W signals imminent cell failure by one mechanism. Degradation by another mechanism is apparently reflected in a fall-off (roll-over) of W at lower frequencies. As a secondary result, the frequency dependence of the absolute cell impedance at low frequencies (5 - 500 mHz) was found to be a good indication of the cell state-of-charge.

Haak, R.↗

NASA NTRS1994

Acoustic properties and durability of liner materials at non-standard atmospheric conditions

This report documents the results of an experimental study on how acoustic properties of certain absorbing liner materials are affected by nonstandard atmospheric conditions. This study was motivated by the need to assess risks associated with incorporating acoustic testing capability in wind tunnels with semicryogenic high Reynolds number aerodynamic and/or low pressure capabilities. The study consisted of three phases: 1) measurement of acoustic properties of selected liner materials at subatmospheric pressure conditions, 2) periodic cold soak and high pressure exposure of liner materials for 250 cycles, and 3) determination of the effect of periodic cold soak on the acoustic properties of the liner materials at subatmospheric conditions and the effect on mechanical resiliency. The selected liner materials were Pyrell foam, Fiberglass, and Kevlar. A vacuum facility was used to create the subatmospheric environment in which an impedance tube was placed to measure acoustic properties of the test materials. An automated cryogenic cooling system was used to simulate periodic cold soak and high pressure exposure. It was found that lower ambient pressure reduced the absorption effectiveness of the liner materials to varying degrees. Also no significant change in the acoustic properties occurred after the periodic cold soak. Furthermore, mechanical resiliency tests indicated no noticeable change.

Ahuja, K. K.↗

DOE OSTI2024

Distinct Mechanism of Anti-Corrosion and Swelling-Adhesion Modeling of Low-Dimensional Nylon-Fluoropolymer Composite Coatings

Compared to other polymers, composite coatings with fluoropolymers as the matrix have attracted considerable interest due to their mechanical performance, chemical stability, and low surface energy. Herein, we present an anticorrosion mechanism of fluoropolymer composite coatings achieved by dispersing varying amounts of polyamide 12 (PA-12) particles over a poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-HFP) matrix. The choice of PVDF-HFP as a coating matrix was driven by its superior processability and mechanical properties over Teflon, while PA-12 afforded swelling capacity, preventing electrolyte permeation, and inhibiting matrix stress crack propagation. The corrosion resistance of the coatings was assessed mainly by potentiodynamic polarization and impedance measurements while being immersed in a NaCl solution. Our electrochemical measurement findings showed that 0.75% w/w PA-12 in the PVDF-HFP matrix significantly enhanced corrosion protection even after 21 days of immersion. Microscopy, dielectric spectroscopy, surface analysis, and mechanical testing (American Society for Testing and Materials standards) corroborated the results. PVDF-HFP coatings containing a minimum percolation threshold of 0.75 wt % PA-12 with 1 mil thickness on mild steel exhibited a remarkable increase in resistance and film adhesion, and a notable corrosion rate decrease. Finite element analysis simulation with a bilinear traction-separation law confirmed the swelling mechanism and adhesion behavior. Finally, this study highlights the potential of nylon particle dispersion in PVDF-HFP matrices as a practical approach to developing advanced anticorrosion coatings with promising practical applications in various industries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Tailoring Electrochemical CO 2 Reduction on Copper by Reactive Ionic Liquid and Native Hydrogen Bond Donors

Abstract Electrochemical CO 2 reduction (CO 2 RR) on copper (Cu) shows promise for higher‐value products beyond CO. However, challenges such as the limited CO 2 solubility, high overpotentials, and the competing hydrogen evolution reaction (HER) in aqueous electrolytes hinder the practical realization. We propose a functionalized ionic liquid (IL) which generates ion‐CO 2 adducts and a hydrogen bond donor (HBD) upon CO 2 absorption to modulate CO 2 RR on Cu in a non‐aqueous electrolyte. As revealed by transient voltammetry, electrochemical impedance spectroscopy (EIS), and in situ surface‐enhanced Raman spectroscopy (SERS) complemented with image charge augmented quantum‐mechanical/molecular mechanics (IC‐QM/MM) computations, a unique microenvironment is constructed. In this microenvironment, the catalytic activity is primarily governed by the IL and HBD concentrations; former controlling the double layer thickness and the latter modulating the local proton availability. This translates to ample CO 2 availability, reduced overpotential, and suppressed HER where C 4 products are obtained. This study deepens the understanding of electrolyte effects in CO 2 RR and the role of IL ions towards electrocatalytic microenvironment design.

Coskun, Oguz Kagan↗