Characterization of Compositional Variation and Solidification Condition on Rapid Solidification Behavior of Beta Stabilized Titanium
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Williamson, C. Jacob↗
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Results for “stability characterization”
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Characterization of compositional variation and solidification condition on rapid solidification behavior of beta stabilized titanium
Rapid solidification (RS) is a field of study that has increased in importance due to the rise of additive manufacturing (AM) techniques. The breakdown of equilibrium at the solid-liquid interface results in an inability to use traditional solidification models that have been applied to great success in casting. As such, there is a current need for a high-throughput testing method to screen alloys at rapid solidification conditions without the significant cost for powder atomization. In this work, twin hammer splat quenching (SQ) is utilized and theoretically developed as a technique uniquely placed to test alloy systems for AM applications. Using analytical thermal spray models and numerical heat transfer simulations, the cooling rate and solidification conditions of splat quenching are compared across several parameters to evaluate the key parameters for generating cooling rates relevant to AM process. Once a framework for the cooling rates and relevancy of SQ are developed, SQ was used to process alloy compositions in the Ti5553 alloy space (AMS 7026) to study the formation of detrimental secondary phases occurring upon rapid quenching from the melt. A martensitic phase is found to occur at the lower end of the standard, but the composition listed in the standard were found to be safe. Finally, the rapid solidification behavior of Ti-5553 is evaluated by comparing splat quenching, laser welding, and plasma atomization that offer a wide window of solidification conditions. The segregation and solidification structure are analyzed and compared to models to provide a deeper understanding of the solidification behavior of beta stabilized titanium alloys.
Williamson, Christopher J.↗
Morphological Evolution and Dealloying During Corrosion of Ni20Cr (wt.%) in Molten FLiNaK Salts
The dealloying corrosion behavior of the FCC Ni20Cr (wt%) in molten LiF-NaF-KF (FLiNaK) salts at 600 °C under varying applied potentials was investigated. Using in-operando electrochemical techniques and a multi-modal suite of characterization methods, we connect electrochemical potential, thermodynamic stability, and electro-dissolution kinetics to the corrosion morphologies. Notably, under certain potential regimes, a micron-scale bicontinuous structure, characterized by a network of interconnected pores and ligaments riched with the composition of the more noble (MN) element, becomes prominent. At other potentials both MN and less noble (LN) elements dealloy but at different rates. The dealloying process consists of lattice and grain boundary diffusion of Cr to the metal/salt interface, interphase Cr oxidation, accompanied by surface diffusion of Ni to form interconnected ligaments. At higher potentials, the bicontinuous porous structure undergoes further surface coarsening. Concurrently, Cr(II), Cr(III), and Ni(II) begin to dissolve, with the dissolution of Ni occurring at a significantly slower rate. When solid-state transport of Cr is exceeded by the interfacial rates, dealloying depths are limited.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Indirect Magnetic Measurements on the Aerodynamic Heating Facility (AHF)
The arc jet complex at NASA Ames Research Center (ARC) investigates various thermal protection systems (TPS) and their performance in high enthalpy flow environments to improve heat shields used in atmospheric entry. The arc jet operates by inducing an arc between two electrodes and passing the heated gas through a supersonic nozzle. The arc plasma is typically a partially ionized air mixture at low temperature (< 2 eV) but operates for long periods of time (up to 30 min) at high power (< 60 MW). However, simulations using the in-house ARC Heater Simulator (ARCHeS) code predict that the arc is still unstable to MHD instabilities, primarily the kink instability, which limit the operational envelope of the facility [1]. Consequently, it is important to better characterize these instabilities to improve facility stability and extend operational ranges. Due to the high enthalpy and long timescales (i.e., minutes) arc diagnostics must be non-invasive (i.e., optical or magnetic). This work will cover the development of tri-axial magnetic hall sensors for arc jet instabilities and subsequent 3D characterization of arc motion. The latest results describing the kink instability amplitude, frequency and wavelength will be presented and represent the first measurements of this instability in a NASA arc jet facility. References: [1] Meurisse, J. (2018). 3D Unsteady Model of Arc Heater Plasma Flow Using the ARC Heater Simulator (ARCHeS), APS Gaseous Electronics Conference, 2018: APS.
Sebastian Vicente Colom↗
The stability of numerical methods for second order ordinary differential equations
An important characterization of a numerical method for first order ODE's is the region of absolute stability. If all eigenvalues of the linear problem dy/dt = Ay are inside this region, the numerical method is stable. If the second order system d/dt(dy/dt) = 2Ady/dt - By is solved as a first order system, the same result applies to the eigenvalues of the generalized eigenvalue problem (lambda-squared)I 2(lambda)A + B. No such region exists for general methods for second order equations, but in some cases a region of absolute stability can be defined for methods for the single second order equation d/dt(dy/dt) = 2ady/dt - by. The absence of a region of absolute stability can occur when different members of a system of first order equations are solved by different methods.
Gear, C. W.↗
Operando Freezing Cryogenic Electron Microscopy of Active Battery Materials
Abstract Understanding structural and chemical evolution of battery materials during operation is critical to achieving safe, efficient, and long-lasting energy storage. Cryogenic electron microscopy (cryo-EM) has become a valuable tool in battery characterization, leveraging low temperatures to improve stability of sensitive materials under electron beam irradiation. However, typical cryo-EM sample preparations leave extended time between the electrochemical point of interest and ex situ freezing of samples, during which active structures may relax, degrade, or otherwise evolve. Here, we detail a method for operando freezing cryo-EM to preserve and characterize native electrode and interfacial structures that arise during battery cycling, based on an operando plunge freezer and cold sample removal process. We validate the method on multiple electrode materials and quantify and discuss the freezing rate achieved. Operando freezing cryo-EM can be used to directly visualize transient features that arise at active electrochemical interfaces, to enable deeper understanding of structural evolution and interfacial chemistry in batteries and other electrochemical systems.
25 ENERGY STORAGE↗
Test Results of the Modified Space Shuttle Main Engine at the Marshall Space Flight Center Technology Test Bed Facility
A modified space shuttle main engine (SSME), which primarily includes an enlarged throat main combustion chamber with the acoustic cavities removed and a main injector with the stability control baffles removed, was tested. This one-of-a-kind engine's design changes are being evaluated for potential incorporation in the shuttle flight program in the mid-1990's. Engine testing was initiated on September 15, 1988 and has accumulated 1,915 seconds and 19 starts. Testing is being conducted to characterize the engine system performance, combustion stability with the baffle-less injector, and both low pressure oxidizer turbopump (LPOTP) and high pressure oxidizer turbopump (HPOTP) for suction performance. These test results are summarized and compared with the SSME flight configuration data base. Testing of this new generation SSME is the first product from the technology test bed (TTB). Figure test plans for the TTB include the highly instrumented flight configuration SSME and advanced liquid propulsion technology items.
Cook, J.↗
How machine learning can help select capping layers to suppress perovskite degradation
Environmental stability of perovskite solar cells (PSCs) has been improved by trial-and-error exploration of thin low-dimensional (LD) perovskite deposited on top of the perovskite absorber, called the capping layer. In this study, a machine-learning framework is presented to optimize this layer. We featurize 21 organic halide salts, apply them as capping layers onto methylammonium lead iodide (MAPbI 3 ) films, age them under accelerated conditions, and determine features governing stability using supervised machine learning and Shapley values. We find that organic molecules’ low number of hydrogen-bonding donors and small topological polar surface area correlate with increased MAPbI 3 film stability. The top performing organic halide, phenyltriethylammonium iodide (PTEAI), successfully extends the MAPbI3 stability lifetime by 4 ± 2 times over bare MAPbI 3 and 1.3 ± 0.3 times over state-of-the-art octylammonium bromide (OABr). Through characterization, we find that this capping layer stabilizes the photoactive layer by changing the surface chemistry and suppressing methylammonium loss.
36 MATERIALS SCIENCE↗
Theory of In-Cloud Activation of Aerosols and Microphysical Quasi-Equilibrium in a Deep Updraft
The microphysical quasi-equilibrium in an ascending adiabatic parcel is elucidated by an analytical theory in 0D with drastic simplifications. The theory predicts how in-cloud activation is most likely to be triggered by the onset of precipitation during sufficient ascent, with the ascent only needing to approach almost twice the cloud-base updraft speed aloft. The precipitation and cloud condensate mass fields are coupled in a closed system in a simplified version of the model. The initial state of no precipitation is unstable with respect to a perturbation. In the 2D phase space of both mass fields, there is a neutral line. Unstable growth of precipitation mass drives the system to cross the line into a regime of stability. An attractor is then approached consisting of precipitation mass balanced by accretion of cloud mass and fallout. The cloud-particle number concentration also approaches a stable equilibrium governed by the balance between in-cloud activation aloft from the inexorably increasing supersaturation during vertical acceleration and accretion of cloud droplets by precipitation. Dimensionless numbers characterizing the microphysical equilibria and their stability are derived mathematically, including a condensation–precipitation efficiency and an in-cloud activation efficiency. The theory explains common observations of the orders of magnitude of liquid water content in convective and stratiform clouds. Finally, sensitivity tests of the numerically integrated theoretical equations are documented with respect to variations in cloud condensation nucleus (CCN) aerosols and updraft speed. In conclusion, it is shown that this theory of in-cloud activation, with an increasing supersaturation during ascent, applies to both ice-only and liquid-only cloud.
54 ENVIRONMENTAL SCIENCES↗
An Integrated Deposition and Passivation Strategy for Controlled Crystallization of 2D/3D Halide Perovskite Films
Abstract This work introduces a simplified deposition procedure for multidimensional (2D/3D) perovskite thin films, integrating a phenethylammonium chloride (PEACl)‐treatment into the antisolvent step when forming the 3D perovskite. This simultaneous deposition and passivation strategy reduces the number of synthesis steps while simultaneously stabilizing the halide perovskite film and improving the photovoltaic performance of resulting solar cell devices to 20.8%. Using a combination of multimodal in situ and additional ex situ characterizations, it is demonstrated that the introduction of PEACl during the perovskite film formation slows down the crystal growth process, which leads to a larger average grain size and narrower grain size distribution, thus reducing carrier recombination at grain boundaries and improving the device's performance and stability. The data suggests that during annealing of the wet film, the PEACl diffuses to the surface of the film, forming hydrophobic (quasi‐)2D structures that protect the bulk of the perovskite film from humidity‐induced degradation.
2D/3D perovskites↗
The role of energy transfer and competing bimolecular reactions in characterizing the unimolecular dissociations of allylic radicals
Resonantly stabilized radicals (RSR's) such as allylic radicals typically have bond energies exceeding 45 kcal/mol and are therefore reasonably long-lived up to quite high temperatures. Consequently, kinetics of the unimolecular dissociations and bimolecular reactions of these long-lived RSR's assume significance in high temperature chemically reacting systems such as in flames. Our recent analyses (J. Cho et al., Proc. Comb. Inst., 2022) of the uncertainty propagated by the energy transfer parameters for 1-methylallyl (1MA) dissociation to the laminar flame speed, indicates an intricate coupling between the kinetics of 1MA dissociation (chain propagation) and its reaction with H-atoms (chain-termination). Here, this work extends such analyses to other C 3 – C 5 allylic radicals: allyl, 2-methylallyl, 1,1-dimethylallyl, 1,2-dimethylallyl, and 1,3-dimethylallyl. Theoretical kinetics for the C 3 – C 4 allylic radicals were taken from prior literature studies (J.A. Miller et al., J. Phys. Chem., 2008; J. Cho et al., Proc. Comb. Inst., 2022; R.S. Tranter et al., Proc. Comb. Inst., 2017). Potential energy surfaces were newly computed for the dissociations of the larger C5 allylic radicals and the reactions of these radicals with H-atoms. These PES's were then used to calculate rate constants for the relevant unimolecular and bimolecular reactions. Energy transfer has a crucial role to play in these pressure-dependent reactions and therefore the present kinetics calculations relied on a-priori predictions of collisional energy transfer parameters to best characterize the branching between chain propagating unimolecular dissociations of these allylic radicals and chain terminating bimolecular reactions of these RSR's with H-atoms. Prompt dissociations are now established to be a universal feature of free radical dissociations. Here we have also characterized the propensity for prompt dissociations in these more-stable allylic RSR's and their role in combustion simulations.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Characterizations of a KHz Pulsed Laser Detection System
A KHz Pulsed Laser Detection System was developed employing the concept of charge integration with an electrometer, in the NASA Goddard Space Flight Center, Code 618 Calibration Lab for the purpose of using the pulsed lasers for radiometric calibration. Comparing with traditional trans-impedance (current-voltage conversion) detection systems, the prototype of this system consists of a UV-Enhanced Si detector head, a computer controlled shutter system and a synchronized electrometer. The preliminary characterization work employs light sources running in either CW or pulsed mode. We believe this system is able to overcome the saturation issue when a traditional trans-impedance detection system is used with the pulsed laser light source, especially with high peak-power pulsed lasers operating at kilohertz repetition rates (e.g. Ekspla laser or KHz OPO). The charge integration mechanism is also expected to improve the stability of measurements for a pulsed laser light source overcoming the issue of peak-to-peak stability. We will present the system characterizations including signal-to-noise ratio and uncertainty analysis and compare results against traditional trans-impedance detection systems.
Ding, Leibo↗
Characterizations of a KHz Pulsed Laser Detection System
A KHz Pulsed Laser Detection System was developed employing the concept of charge integration with an electrometer, in the NASA Goddard Space Flight Center, Code 618 Calibration Lab for the purpose of using the pulsed lasers for radiometric calibration. Comparing with traditional trans-impedance (current-voltage conversion) detection systems, the prototype of this system consists of a UV-Enhanced Si detector head, a computer controlled shutter system and a synchronized electrometer. The preliminary characterization work employs light sources running in either CW or pulsed mode. We believe this system is able to overcome the saturation issue when a traditional trans-impedance detection system is used with the pulsed laser light source, especially with high peak-power pulsed lasers operating at kilohertz repetition rates (e.g. Ekspla laser or KHz OPO). The charge integration mechanism is also expected to improve the stability of measurements for a pulsed laser light source overcoming the issue of peak-to-peak stability. We will present the system characterizations including signal-to-noise ratio and uncertainty analysis and compare results against traditional trans-impedance detection systems.
Ding, Leibo↗
A formulation of stability for spacecraft formations
A formulation of stability for a set of spacecraft in formation flight is presented. First, a formation is defined in a precise mathematical form in terms of control interactions. Then, stability is formulated based on input-to-output stability with respect to a partitioning of the formation dynamics. This formulation of stability is shown to be useful in characterizing disturbance propagation in the formation as a function of the partition interconnection topology, and also in analyzing the robustness of sensing, communication, and control topologies. Stability results are presented for hierarchical, cyclic, and disturbance attenuating formations.
formation flyer↗
Aerogeophysical evidence for active volcanism beneath the West Antarctic Ice Sheet
Although it is widely understood that the collapse of the West Antarctic Ice Sheet (WAIS) would cause a global sea-level rise of 6 m, there continues to be considerable debate about the response of this ice sheet to climate change. The stability of the WAIS, which is characterized by a bed grounded well below sea level, may depend on geologically controlled conditions at the base, which are independent of climate. Ice streams moving up to 750 m/yr disperse material from the interior through to the oceans. As these ice streams tend to buffer the reservoir of slow-moving inland ice from exposure to oceanic degradation, understanding the ice-streaming process is important for evaluating WAIS stability. There is strong evidence that ice streams slide on a lubricating layer of water-saturated till. Development of this basal layer requires both water and easily eroded sediments. Active lithospheric extension may elevate regional heat flux, increase basal melting, and trigger ice streaming. If a geologically defined boundary with a sharp contrast in geothermal flux exists beneath the WAIS, ice streams may only be capable of operating as a buffer over a restricted region. Should ocean waters penetrate beyond this boundary, the ice-stream buffer would disappear, possibly triggering a collapse of the inland ice reservoir. Aerogeophysical evidence for active volcanism and elevated heat flux beneath the WAIS near the critical region where ice streaming begins is presented.
Blankenship, Donald D.↗
Material Changes in Electrocatalysis: An In Situ/Operando Focus on the Dynamics of Cobalt‐Based Oxygen Reduction and Evolution Catalysts
Abstract The shift towards cheaper, non‐platinum group metal electrocatalyst materials for clean energy technologies is coupled with challenges in maintaining long‐term performance. For practical purposes, electrocatalytic stability typically focuses on catalyst electrochemical performance over time. However, a deeper understanding of catalyst material property changes during operation is needed to enable material‐specific design strategies for long‐term stabilization. In the last several decades, improvements in material characterization techniques have made it possible to probe the composition, structure, and degradation products of catalysts in situ/operando. Herein we review the current understanding of in situ/operando material stability of Co‐based electrocatalysts for the oxygen evolution (OER) and reduction reactions (ORR) in acidic and alkaline environments. We focus on in situ/operando materials characterization of three categories of Co‐based OER/ORR catalysts: oxides and (oxy)hydroxides, mixed‐metal catalysts, and non‐oxide materials. This review aims to compile and compare the results from multiple studies and techniques to provide insight into the role that the starting material, pH, and applied potential have on the active surface and stability of Co‐based materials. We conclude by highlighting directions that have been underexplored with opportunities for continued research including improving in situ/operando characterization, methods to probe long‐term material changes, and the development of operando studies on full‐scale devices. Using Co‐based materials as a case study, this review shows the vital role that in situ/operando characterization must play in the future of improving electrocatalyst stability.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Reassembly of Peptide Nanofibrils on Live Cell Surfaces Promotes Cell–Cell Interactions
Nature regulates cellular interactions through the cell-surface molecules and plasma membranes. Despite advances in cell-surface engineering with diverse ligands and reactive groups, modulating cell–cell interactions through scaffolds of the cell-binding cues remains a challenging endeavor. Here, we assembled peptide nanofibrils on live cell surfaces to present the ligands that bind to the target cells. Surprisingly, with the same ligands, reducing the thermal stability of the nanofibrils promoted cellular interactions. Characterizations of the system revealed a thermally induced fibril disassembly and reassembly pathway that facilitated the complexation of the fibrils with the cells. Using the nanofibrils of varied stabilities, the cell–cell interaction was promoted to different extents with free-to-bound cell conversion ratios achieved at low (31%), medium (54%), and high (93%) levels. Further, this study expands the toolbox to generate desired cell behaviors for applications in many areas and highlights the merits of thermally less stable nanoassemblies in designing functional materials.
77 NANOSCIENCE AND NANOTECHNOLOGY↗
Simultaneous Enhancement of Efficiency And Operational-Stability of Mesoscopic Perovskite Solar Cells via Interfacial Toughening
The combined effects of compact TiO 2 (c-TiO 2 ) electron-transport layer (ETL) are investigated without and with mesoscopic TiO 2 (m-TiO 2 ) on top, and without and with an iodine-terminated silane self-assembled monolayer (SAM), on the mechanical behavior, opto–electronic properties, photovoltaic (PV) performance, and operational-stability of solar cells based on metal-halide perovskites (MHPs). The interfacial toughness increases almost threefold in going from c-TiO 2 without SAM to m-TiO 2 with SAM. This is attributed to the synergistic effect of the m-TiO 2 /MHP nanocomposite at the interface and the enhanced adhesion afforded by the iodine-terminated silane SAM. The combination of m-TiO 2 and SAM also offers a significant beneficial effect on the photocarriers extraction at the ETL/MHP interface, resulting in perovskite solar cells (PSCs) with power-conversion efficiency (PCE) of over 24% and 20% for 0.1 and 1 cm 2 active areas, respectively. These PSCs also have exceptionally long operational stability lives extrapolated T80 (duration at 80% initial PCE retained) is ≈18 000 and 10 000 h for 0.1 and 1 cm 2 active areas, respectively. In conclusion, postmortem characterization and analyses of the operational-stability-tested PSCs are performed to elucidate the possible mechanisms responsible for the long operational-stability.
14 SOLAR ENERGY↗