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DOE OSTI2022

Intrinsically Chiral Twist‐Bend Nematogens: Interplay of Molecular and Structural Chirality in the N TB Phase

Abstract Non‐symmetric lactate‐based chiral liquid crystal dimers containing an odd‐membered spacer are shown to exhibit a chiral twist‐bend nematic phase which is stable on cooling to room temperature. A comparison of racemic and optically pure materials reveals that the pitch length in the N* TB phase is not influenced by molecular chirality, whereas the nematic‐twist‐bend nematic transition temperature is increased.

Chemistry↗

DOE OSTI2023

Robotic pendant drop: containerless liquid for μs-resolved, AI-executable XPCS

Abstract The dynamics and structure of mixed phases in a complex fluid can significantly impact its material properties, such as viscoelasticity. Small-angle X-ray Photon Correlation Spectroscopy (SA-XPCS) can probe the spontaneous spatial fluctuations of the mixed phases under various in situ environments over wide spatiotemporal ranges (10 −6 –10 3 s /10 −10 –10 −6 m). Tailored material design, however, requires searching through a massive number of sample compositions and experimental parameters, which is beyond the bandwidth of the current coherent X-ray beamline. Using 3.7-μs-resolved XPCS synchronized with the clock frequency at the Advanced Photon Source, we demonstrated the consistency between the Brownian dynamics of ~100 nm diameter colloidal silica nanoparticles measured from an enclosed pendant drop and a sealed capillary. The electronic pipette can also be mounted on a robotic arm to access different stock solutions and create complex fluids with highly-repeatable and precisely controlled composition profiles. This closed-loop, AI-executable protocol is applicable to light scattering techniques regardless of the light wavelength and optical coherence, and is a first step towards high-throughput, autonomous material discovery.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Cation valency in water-in-salt electrolytes alters the short- and long-range structure of the electrical double layer

Highly concentrated aqueous electrolytes (termed water-in-salt electrolytes, WiSEs) at solid-liquid interfaces are ubiquitous in myriad applications including biological signaling, electrosynthesis, and energy storage. This interface, known as the electrical double layer (EDL), has a different structure in WiSEs than in dilute electrolytes. Here, we investigate how divalent salts [zinc bis(trifluoromethylsulfonyl)imide, Zn(TFSI) 2 ], as well as mixtures of mono- and divalent salts [lithium bis(trifluoromethylsulfonyl)imide (LiTFSI) mixed with Zn(TFSI) 2 ], affect the short- and long-range structure of the EDL under confinement using a multimodal combination of scattering, spectroscopy, and surface forces measurements. Raman spectroscopy of bulk electrolytes suggests that the cation is closely associated with the anion regardless of valency. Wide-angle X-ray scattering reveals that all bulk electrolytes form ion clusters; however, the clusters are suppressed with increasing concentration of the divalent ion. To probe the EDL under confinement, we use a Surface Forces Apparatus and demonstrate that the thickness of the adsorbed layer of ions at the interface grows with increasing divalent ion concentration. Multiple interfacial layers form following this adlayer; their thicknesses appear dependent on anion size, rather than cation. Importantly, all electrolytes exhibit very long electrostatic decay lengths that are insensitive to valency. It is likely that in the WiSE regime, electrostatic screening is mediated by the formation of ion clusters rather than individual well-solvated ions. This work contributes to understanding the structure and charge-neutralization mechanism in this class of electrolytes and the interfacial behavior of mixed-electrolyte systems encountered in electrochemistry and biology.

Science & Technology - Other Topics↗

NASA NTRS1999

Cloud-Vegetation Interaction: Use of Normalized Difference Cloud Index for Estimation of Cloud Optical Thickness

A new technique to retrieve cloud optical depth for broken clouds above green vegetation using ground-based zenith radiance measurements is developed. By analogy with the Normalized Difference Vegetation Index NDVI), the Normalized Difference Cloud Index (NDCI) is defined as a ratio between the difference and the sum of two zenith radiances measured for two narrow spectral bands in the visible and near-IR regions. The very different spectral behavior of cloud liquid water drops and green vegetation is the key physics behind the NDCI. It provides extra tools to remove the radiative effects of the 3D cloud structure. Numerical calculations based on fractal clouds and real measurements of NDCI and cloud liquid water path confirm the improvements.

Marshak, A.↗

NASA NTRS2016

Update on Risk Reduction Activities for a Liquid Advanced Booster for NASA's Space Launch System

Dynetics has designed innovative structure assemblies; manufactured them using Friction Stir Welding (FSW) to leverage NASA investments in tools, facilities, and processes; conducted proof and burst testing, demonstrating viability of design/build processes Dynetics/AR has applied state-of-the-art manufacturing and processing techniques to the heritage F-1, reducing risk for engine development Dynetics/AR has also made progress on technology demonstrations for ORSC cycle engine, which offers affordability and performance for both NASA and other launch vehicles Full-scale integrated oxidizer-rich test article. Testing will evaluate performance and combustion stability characteristics. Contributes to technology maturation for ox-rich staged combustion engines.

Crocker, Andy↗

DOE OSTI2021

Preface to the JPCM special issue on intense radiation sources in condensed matter and materials physics

This special issue is designed to honour the contributions of our colleague Neville Greaves who was among the first to apply newly-available synchrotron x-ray techniques to study the synthesis, structures and properties of advanced materials [1, 2]. His wide ranging work on ceramics, glasses and nanomaterials was celebrated in a recent issue of the J. Non-Cryst. Solids [3]. Neville's contributions to synchrotron research, highlighted here, focussed on design and construction of new beamline capabilities and sample environments to probe materials under different physical and chemical conditions, integrating various techniques to obtain complementary data on structure and bonding. The innovative nature of his work is illustrated by his studies of liquids and glasses, where he incorporated aerodynamic levitation into these experimental techniques, using both synchrotron x-ray and neutron beams to probe the structural transformations and dynamics combined with molecular dynamics simulations to study atomic scale organisation. His work has had a major impact on fundamental condensed matter physics and chemistry as well as applied materials science; and in this issue, we present contributions from colleagues using and developing new experimental techniques at current and next-generation synchrotron, neutron and free-electron laser sources and in their own laboratories, that probe the fundamental physics, chemistry and functional properties of novel materials and processes.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

NASA NTRSDate not supplied

Centrifugal Nuclear Thermal Rocket Challenges and Potential

The Centrifugal Nuclear Thermal Rocket (CNTR) is a liquid fueled fission propulsion concept designed to heat propellant to 5000 K prior to expansion through a nozzle. A specific impulse up to 1800 s may be achieved using hydrogen propellant, and a specific impulse up to 1000 s may be achieved using more storable propellants such as methane, ammonia, or propane. The high uranium density of the liquid metallic uranium or liquid uranium carbide fuel will help enable compact engines suitable for missions such as fast (<15 month) round trip human Mars missions or high delta-V missions in cislunar space. Long term applications of the CNTR could include the advanced exploration and utilization of the solar system through direct use of in-situ volatiles as propellant. Challenges associated with the CNTR are numerous. Centrifugal force is used to retain the liquid fuel in rotating fuel cylinders, and rotational velocities up to 5000 rpm may be required. Propellant flow must be directed such that all structures and moderators in the core are adequately cooled prior to the propellant entering the liquid fuel and being heated to 5000 K. The rotating fuel cylinder wall (RFCW) must have an inner surface designed to be compatible with liquid uranium metal or uranium carbide fuel up to at least 1500 K, and that inner surface may also need to be textured to help maintain acceptable wall temperatures. Propellant must flow radially inward through the RFCW while fuel is simultaneously contained. The RFCW should ideal-ly be made from a material with low neutron absorption to help minimize engine mass and facilitate the use of High Assay Low Enriched Uranium (HALEU) fuel in the system. The drive system for the rotating fuel cylinders must support all phases of operation. This paper will discuss computational and experimental research being conducted to address some of the challenges associated with the CNTR, and will also note potential mission benefits from the CNTR.

Michael G. Houts↗

NASA NTRS1972

Radiation heating in selected NERVA engine components

The role of heating from nuclear radiation in design of the NERVA engine is treated. Some components are subjected to very high gamma heating rates in excess of 0.5 Btu/cubic inch/sec in steel in the primary nozzle or 0.25 Btu/cubic inch/sec in aluminum in the pressure vessel. These components must be cooled by a fraction of the liquid hydrogen propellant before it is passed through the core, heated, and expanded out the nozzle as a gas. Other components that are subjected to lower heating rates such as the thrust structure and the disk shield are designed so that they would not require liquid hydrogen cooling. Typical gamma and neutron heating rates, resulting temperatures, and their design consequences are discussed. Calculational techniques used in the nuclear and thermal analyses of the NERVA engine are briefly treated.

Courtney, J. C.↗

NASA NTRS2000

Quantitative Measurements of Nitric Oxide Concentration in High-Pressure, Swirl-Stabilized Spray Flames

Lean direct-injection (LDI) spray flames offer the possibility of reducing NO(sub x) emissions from gas turbines by rapid mixing of the liquid fuel and air so as to drive the flame structure toward partially-premixed conditions. We consider the technical approaches required to utilize laser-induced fluorescence methods for quantitatively measuring NO concentrations in high-pressure LDI spray flames. In the progression from atmospheric to high-pressure measurements, the LIF method requires a shift from the saturated to the linear regime of fluorescence measurements. As such, we discuss quantitative, spatially resolved laser-saturated fluorescence (LSF), linear laser-induced fluorescence (LIF), and planar laser-induced fluorescence (PLIF) measurements of NO concentration in LDI spray flames. Spatially-resolved LIF measurements of NO concentration (ppm) are reported for preheated, LDI spray flames at pressures of two to five atmospheres. The spray is produced by a hollow-cone, pressure-atomized nozzle supplied with liquid heptane. NO is excited via the Q(sub 2)(26.5) transition of the gamma(0,0) band. Detection is performed in a two nanometer region centered on the gamma(0,1) band. A complete scheme is developed by which quantitative NO concentrations in high-pressure LDI spray flames can be measured by applying linear LIF. NO is doped into the reactants and convected through the flame with no apparent destruction, thus allowing a NO fluorescence calibration to be taken inside the flame environment. The in-situ calibration scheme is validated by comparisons to a reference flame. Quantitative NO profiles are presented and analyzed so as to better understand the operation of lean-direct injectors for gas turbine combustors. Moreover, parametric studies are provided for variations in pressure, air-preheat temperature, and equivalence ratio. Similar parametric studies are performed for lean, premixed-prevaporized flames to permit comparisons to those for LDI flames. Finally, PLIF is expanded to high pressure in an effort to quantify the detected fluorescence image for LDI flames. Success is achieved by correcting the PLIF calibration via a single-point LIF measurement. This procedure removes the influence of any preferential background that occurs in the PLIF detection window. In general, both the LIF and PLIF measurements verify that the LDI strategy could be used to reduce NO(sub x) emissions in future gas turbine combustors.

Cooper, Clayton S.↗

NASA NTRS2011

A Variational Method to Retrieve the Extinction Profile in Liquid Clouds Using Multiple Field-of-View Lidar

While liquid clouds playa very important role in the global radiation budget, it's been very difficult to remotely determine their internal cloud structure. Ordinary lidar instruments (similar to radars but using visible light pulses) receive strong signals from such clouds, but the information is limited to a thin layer near the cloud boundary. Multiple field-of-view (FOV) lidars offer some new hope as they are able to isolate photons that were scattered many times by cloud droplets and penetrated deep into a cloud before returning to the instrument. Their data contains new information on cloud structure, although the lack of fast simulation methods made it challenging to interpret the observations. This paper describes a fast new technique that can simulate multiple-FOV lidar signals and can even estimate the way the signals would change in response to changes in cloud properties-an ability that allows quick refinements in our initial guesses of cloud structure. Results for a hypothetical airborne three-FOV lidar suggest that this approach can help determine cloud structure for a deeper layer in clouds, and can reliably determine the optical thickness of even fairly thick liquid clouds. The algorithm is also applied to stratocumulus observations by the 8-FOV airborne "THOR" lidar. These tests demonstrate that the new method can determine the depth to which a lidar provides useful information on vertical cloud structure. This work opens the way to exploit data from spaceborne lidar and radar more rigorously than has been possible up to now.

Pounder, Nicola L.↗

NASA NTRS1993

Study on solidification of immisible alloys (M-10)

Alloying of immiscible alloys under microgravity is of interest in metallurgical processes. Several experiments investigating the alloying of immiscible alloys, such as Al-In, Al-Bi, Zn-Bi, and Zn-Pb, were done in space. Homogeneous distribution of small L2 particles in the matrix, such as an emulsion structure, was expected in the space-solidifed alloys. However, the alloys demonstrated an extremely segregated structure. To date insufficient information was obtained to explain these unexpected results. Our experiment was proposed to clarify the solidification manner of immiscible alloys and to obtain fundamental information concerning structural control of the alloys. In space, density differences between the two liquids separated in immiscible regions can be neglected, so that no sedimentation of L(sub 2) phase will take place. When the growth of the alloys is interrupted and this status is frozen by an adequate rapid cooling procedure, it will provide much information concerning decomposing homogeneous liquid and the interaction between the monotectic growth front morphology and the distribution of L(sub 2) phase. It is anticipated that the results will be useful for elucidating the monotectic solidification manner and it will be instructive to explain the segregated structures obtained in the past space experiments.

Kamio, Akihiko↗

NASA NTRS1999

Containerless, Low-Gravity Undercooling of Ti-Ce Alloys in the MSFC Drop Tube

Previous tests of the classical nucleation theory as applied to liquid-liquid gap miscibility systems found a discrepancy between experiment and theory in the ability to undercool one of the liquids before the L1-L2 separation occurs. To model the initial separation process in a two-phase liquid mixture, different theoretical approaches, such as free-energy gradient and density gradient theories, have been put forth. If there is a large enough interaction between the critical liquid and the crucible, both models predict a wetting temperature (T(sub w)) above which the minority liquid perfectly wets and layers the crucible interface, but only on one side of the immiscibility dome. Materials with compositions on the other side of the dome will have simple surface adsorption by the minority liquid before bulk separation occurs when the coexistence (i.e., binoidal) line in reached. If the interaction between the critical liquid and the crucible were to decrease, T(sub w) would increase, eventually approaching the critical consolute temperature (T(sub cc)). If this situation occurs, then there could be large regions of the miscibility gap where non-perfect wetting conditions prevail resulting in droplets of L1 liquid at the surface having a non-zero contact angle. The resulting bulk structure will then depend on what happens on the surface and the subsequent processing conditions. In the past several decades, many experiments in space have been performed on liquid metal binary immiscible systems for the purpose of determining the effects that different crucibles may have on the wetting and separation process of the liquids. Potard performed experiments that showed different crucible materials could cause the majority phase to preferentially wet the container and thus produce a dispersed microstructure of the minority phase. Several other studies have been performed on immiscibles in a semi-container environment using an emulsion technique. Only one previous study was performed using completely containerless processing of immiscible metals and the results of that investigation are similar to some of the emulsion studies. In all the studies, surface wetting was attributed as the cause for the similar microstructures or the asymmetry in the ability to undercool the liquid below the binoidal on one side of the immiscibility dome. By removing the container completely from the separation process, it was proposed that the loss of the crucible/liquid interaction would produce a large shift in T(sub w) and thus change the wetting characteristics at the surface. By investigating various compositions across the miscibility gap, a change in the type and amount of liquid wetting at the surface of a containerless droplet should change the surface nucleating behavior of the droplet - whether it be the liquid-liquid wetting or the liquid-to-solid transition. Undercooling of the liquid into the metastable region should produce significant differences in the separation process and the microstructure upon solidification. In this study, we attempt to measure these transitions by monitoring the temperature of the sample by optical pyrometry. Microstructural analysis will be made to correlate with the degree of undercooling and the separation mechanisms involved.

Robinson, M. B.↗

NASA NTRS2002

Galvanic Liquid Applied Coating System For Protection of Embedded Steel Surfaces from Corrosion

Corrosion of reinforcing steel in concrete is an insidious problem facing Kennedy Space Center (KSC), other Government Agencies, and the general public. These problems include KSC launch support structures, highway bridge infrastructure, and building structures such as condominium balconies. Due to these problems, the development of a Galvanic Liquid Applied Coating System would be a breakthrough technology having great commercial value for the following industries: Transportation, Infrastructure, Marine Infrastructure, Civil Engineering, and the Construction Industry. This sacrificial coating system consists of a paint matrix that may include metallic components, conducting agents, and moisture attractors. Similar systems have been used in the past with varying degrees of success. These systems have no proven history of effectiveness over the long term. In addition, these types of systems have had limited success overcoming the initial resistance between the concrete/coating interface. The coating developed at KSC incorporates methods proven to overcome the barriers that previous systems could not achieve. Successful development and continued optimization of this breakthrough system would produce great interest in NASA/KSC for corrosion engineering technology and problem solutions. Commercial patents on this technology would enhance KSC's ability to attract industry partners for similar corrosion control applications.

Curran, Joseph↗

DOE OSTI2021

Direct Observation of Ultrafast Hydrogen Bond Strengthening in Liquid Water

Water is one of the most important, yet least understood, liquids in nature. Many anomalous properties of liquid water originate from its well-connected hydrogen bond network, including unusually efficient vibrational energy redistribution and relaxation. An accurate description of the ultrafast vibrational motion of water molecules is essential for understanding the nature of hydrogen bonds and many solution-phase chemical reactions. Most existing knowledge of vibrational relaxation in water is built upon ultrafast spectroscopy experiments. However, these experiments cannot directly resolve the motion of the atomic positions and require difficult translation of spectral dynamics into hydrogen bond dynamics. Here we measured the ultrafast structural response to the excitation of the OH stretching vibration in liquid water with femtosecond temporal and atomic spatial resolution using liquid ultrafast electron scattering. We observed a transient hydrogen bond contraction of roughly 0.04 Å on a timescale of 80 femtoseconds, followed by a thermalization on a timescale of ~1 picosecond. Molecular dynamics simulations reveal the need to treat the distribution of the shared proton in the hydrogen bond quantum mechanically to capture the structural dynamics on the femtosecond timescales. Our experiment and simulations unveiled the intermolecular character of the water vibration preceding the relaxation of the OH stretch.

36 MATERIALS SCIENCE↗

DOE OSTI2025

FLAMES─Fast, Low-Storage, Accurate, and Memory-Efficient Adaptive Sampling─Approach to Resolve Spatially Dependent Dynamics of Molecular Liquids

Many critical phenomena in soft matter occur at large length scales, necessitating the resolution of their structure and dynamics at low wavenumbers. However, resolving wavenumber-dependent dynamics computationally via molecular dynamics simulations presents significant challenges, as these phenomena span several orders of magnitude in both time and length scales, resulting in high computational costs and memory demands. Here, this work highlights the computational and memory challenges associated with analyzing molecular trajectories in reciprocal space and demonstrates a method to address them. We introduce FLAMESFast, Low-storage, Accurate, and Memory-Efficient adaptive Sampling, which is a direct method for calculation of structure factors, allowing us to select only the required number of wavevectors for binning. We also use wavenumber-dependent time steps to extract dynamics. Our FLAMES approach effectively mitigates computational and memory/storage bottlenecks. We demonstrate the method using simulations of a model system, liquid octane, at various temperatures. Comparisons with experimental data and real space computation show that the FLAMES technique achieves high accuracy in resolving temperature- and spatially dependent dynamics while being significantly more computationally efficient and requiring less memory and storage than methods based on a uniform wavevector grid and fixed temporal spacing.

Chen, Guang [Argonne National Laboratory (ANL), Ar↗

NASA NTRS1998

Semiconductor apparatus utilizing gradient freeze and liquid-solid techniques

Transition metals of Group VIII (Co, Rh and Ir) have been prepared as semiconductor compounds with the general formula TSb.sub.3. The skutterudite-type crystal lattice structure of these semiconductor compounds and their enhanced thermoelectric properties results in semiconductor materials which may be used in the fabrication of thermoelectric elements to substantially improve the efficiency of the resulting thermoelectric device. Semiconductor materials having the desired skutterudite-type crystal lattice structure may be prepared in accordance with the present invention by using vertical gradient freezing techniques and/or liquid phase sintering techniques. Measurements of electrical and thermal transport properties of selected semiconductor materials prepared in accordance with the present invention, demonstrated high Hall mobilities (up to 1200 cm.sup.2.V.sup.-1.s.sup.-1) and good Seebeck coefficients (up to 150 .mu.VK.sup.-1 between 300.degree. C. and 700.degree. C.). Optimizing the transport properties of semiconductor materials prepared from elemental mixtures Co, Rh, Ir and Sb resulted in a substantial increase in the thermoelectric figure of merit (ZT) at temperatures as high as 400.degree. C. for thermoelectric elements fabricated from such semiconductor materials.

Fleurial, Jean-Pierre↗

DOE OSTI2020

Ultrafast solid-liquid intercalation enabled by targeted microwave energy delivery

In chemical reactions, the breaking and formation of chemical bonds usually need external energy to overcome the activation barriers. Conventional energy delivery transfers energy from heating sources via various media, hence losing efficiency and inducing side reactions. In contrast, microwave (MW) heating is known to be highly energy efficient through dipole interaction with polar media, but how exactly it transmits energy to initiate chemical reactions has been unknown. Here, we report a rigorous determination of energy delivery mechanisms underlying MW-enabled rapid hydrothermal synthesis, by monitoring the structure and temperature of all the involved components as solid-liquid intercalation reaction occurs using in situ synchrotron techniques. We reveal a hitherto unknown direct energy transmission between MW irradiation source and the targeted reactants, leading to greatly reduced energy waste, and so the ultrafast kinetics at low temperature. These findings open up new horizons for designing material synthesis reactions of high efficiency and precision.

36 MATERIALS SCIENCE↗

NASA NTRS1994

Influence of Two-Phase Thermocapillary Flow on Cryogenic Liquid Retention in Microscopic Pores

Previous experiments indicate that the bubble point pressure of spacecraft liquid hydrogen acquisition devices is reduced substantially when the ullage is pressurized with heated hydrogen vapor. The objective is to determine whether the two-phase thermocapillary convection arising from thermodynamic non-equilibrium along the porous surfaces of such devices could lead to this observed degradation in retention performance. We also examine why retention capability appears to be unaffected by pressurization with heated helium or direct heating through the porous structure. Computational assessments based on coupled solution of the flowfield and liquid free surface indicate that for highly wetting fluids in small pores, dynamic pressure and vapor recoil dictate surface morphology and drive meniscus deformation. With superheating, the two terms exert the same influence on curvature and promote mechanical equilibrium, but with subcooling, the pressure distribution produces a suction about the pore center-line that degrades retention. This result points to thermocapillary-induced deformation arising from condensation as the cause for retention loss. It also indicates that increasing the level of non-equilibrium by reducing accommodation coefficient restricts deformation and explains why retention failure does not occur with direct screen heating or helium pressurization.

Schmidt, G. R.↗