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DOE OSTI2025

Direct Measurements of Dimethyl Sulfide Oxidation Chemistry: Uncovering the Primary Pathways from Gas Phase to Sulfate Aerosols

We report experimental measurements of dimethyl sulfide oxidation, focusing on a major chemical intermediate, hydroperoxymethyl thioformate (HPMTF). The (photo)chemistry and transport properties of HPMTF, which are critical to accurate modeling of tropospheric sulfur, are not known, partly because current analytical methods are not optimized for elusive chemical intermediates. We investigated dimethyl sulfide oxidation using a custom time-resolved photoionization mass spectrometer, interfaced with pulsed laser photolysis, continuous photolysis, and liquid droplet reactors. We detected and characterized HPMTF (along with other reaction intermediates), quantified its yield, and measured its formation rate coefficient. We also developed a clean, intense, online HPMTF source, suitable for further experimental investigations. Lastly, we measured the mass accommodation coefficient of HPMTF on water droplets – a critical quantity for modeling its atmospheric partitioning between the gas and condensed phases. The experimental platform we developed here enables the exploration of other critical elusive reaction intermediates.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Hydrodynamic instabilities and heat transfer characteristics in the duct flow of a fluid in the supercritical thermodynamic regime

The behavior of fluids at supercritical thermodynamic conditions is inherently complex due to large variations in thermodynamic and transport properties. Recent numerical and experimental investigations illustrate ongoing interest for these fluids, especially supercritical CO 2 and supercritical water, for a variety of applications. For example, supercritical water reactors (SCWR) operate in this extreme condition of high-pressure and temperature, resulting in highly dynamic flow fields and unexpected heat transfer regimes. The potential heat transfer benefits in this regime are directly associated with the extreme variations in thermodynamic and transport properties, which occur at, and above, the critical point. This work characterizes the hydrodynamic instabilities that arise for fluids at supercritical thermodynamic conditions when buoyancy forces are significant. Two specific configurations are considered, a natural convection cavity flow, and a mixed convection, heated, horizontal channel flow. Natural convection flow in a cavity is a classical configuration with expected behavior below the critical point. This configuration aids in characterizing the effect of the variable properties in the supercritical thermodynamic regime. Further, limited studies in the existing literature have been conducted for low-Reynolds and intermediate-Rayleigh numbers, mixed-convection channel flows for supercritical water, which is the focus of the channel flow configuration. To investigate the thermally driven hydrodynamic instabilities in this regime, a high-order fully-implicit numerical method is used. Such strong variations in thermophysical properties (in particular, density) are difficult to simulate and an altogether compressible framework is needed. Therefore, the compressible Navier-Stokes equations are solved without any additional assumptions. The fully implicit, high-order in space and time, reconstructed discontinuous Galerkin method as implemented within the multi-physics code called ALE3D (Arbitrary Lagrangian and Eulerian in 2D and 3D), developed at Lawrence Livermore National Laboratory (LLNL), is used. This fully implicit, L-stable method accurately captures the compressible nature of the ow in the limit of very low Mach number. It has been widely accepted that above the critical point, only one phase is observed. However, recent research has indicated the existence of the distinct gas-like and liquid-like regions separated by the Widom line, the locus of the maxima of the specific heat. Along the Widom line, density decreases 6-fold, viscosity drops by a factor of 2, while specific heat spikes by an order of magnitude. These variations, specifically in density and viscosity, produce a thick pseudo-interface and flow dynamics behavior akin to film boiling. A pseudo-film at the heated wall of the cavity and the horizontal channel is observed where buoyancy forces induce mixing through the specific configurations. Further the local Rayleigh and Richardson numbers provide maps of the flow field and the buoyancy forces driving the microscopic mixing. In the first chapter, I describe a background of supercritical fluid and the various applications. The second chapter focuses on the mathematical model and numerical method used for simulations, where a description of the equation of state for supercritical water is described. The third chapter focuses on the natural convection cavity with a heated bottom wall. In this cavity a gas-like and a liquid-like flow within the supercritical thermodynamic regime are observed. The fourth chapter focuses on a forced convection, horizontal channel, distinguishing between the gas-like, liquid-like, and mixed flow regimes. Mixed convection flow, with the addition of gravitational forces in the horizontal channel show the influence of variable properties on the hydrodynamic development, heat transfer, and rising instabilities. The last chapter of this research focuses on characterizing the unstable hydrodynamics through time-averaging processes and analysis of the movement of energy through the developing plumes.

42 ENGINEERING↗

DOE OSTI2022

Self-organized patterns at the plasma–liquid anode interface in a helium glow discharge: temporal development and mechanisms

Self-organization at the plasma–liquid anode interface is a commonly observed phenomenon for atmospheric pressure glow plasmas, resulting in patterns with distinctive shapes such as circular ring, star-shaped, and gear-like structures, depending primarily on the discharge current and solution conductivity. Recent studies have shown that the electrode gap distance, solute used for liquid anode solution, and gas composition can also significantly impact pattern formation. Nonetheless, an overarching model or explanation of the key underlying mechanisms consistent with all experimentally observed trends is not yet reported. We propose a key underlying mechanism enabling pattern formation motivated by a detailed parametric study of pattern formation complemented by the temporal development of patterns and consistent with all observed trends. Pattern formation was observed to be on a time scale of 100 μs, similar to the time scales of gas heating and evaporation. It was found that a minimum water evaporation rate of (3.5 ± 0.5) × 10 –6 kg s –1 and reduced electric field in the positive column of 16.6 ± 0.4 Td is required for pattern formation in the investigated cases irrespective of solution conductivity and gas composition for NaCl solutions. Nonetheless, the presence of cations for which the corresponding metal atom has a low ionization energy was identified as a necessary condition for pattern formation. Furthermore, the reported results suggest that the presence of a small amount of metal atoms in the gas phase with low ionization energy enhances the overall ionization rate in the near anode region which triggers pattern formation.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS1991

Full-size solar dynamic heat receiver thermal-vacuum tests

The testing of a full-size, 120 kW, solar dynamic heat receiver utilizing high-temperature thermal energy storage is described. The purpose of the test program was to quantify receiver thermodynamic performance, operating temperatures, and thermal response to changes in environmental and power module interface boundary conditions. The heat receiver was tested in a vacuum chamber with liquid nitrogen cold shrouds and an aperture cold plate to partly simulate a low-Earth-orbit environment. The cavity of the receiver was heated by an infrared quartz lamp heater with 30 independently controllable zones to allow axially and circumferentially varied flux distributions. A closed-Brayton cycle engine simulator conditioned a helium-xenon gas mixture to specific interface conditions to simulate the various operational modes of the solar dynamic power module on the Space Station Freedom. Inlet gas temperature, pressure, and flow rate were independently varied. A total of 58 simulated orbital cycles, each 94 minutes in duration, was completed during the test conduct period.

Sedgwick, L. M.↗

NASA NTRS1991

Full-size solar dynamic heat receiver thermal-vacuum tests

The testing of a full-size, 102 kW, solar dynamic heat receiver utilizing high-temperature thermal energy storage is described. The purpose of the test program was to quantify receiver thermodynamic performance, operating temperatures, and thermal response to changes in environmental and power module interface boundary conditions. The heat receiver was tested in a vacuum chamber with liquid nitrogen cold shrouds and an aperture cold plate to partly simulate a low-Earth-orbit environment. The cavity of the receiver was heated by an infrared quartz lamp heater with 30 independently controllable zones to allow axially and circumferentially varied flux distributions. A closed-Brayton cycle engine simulator conditioned a helium-xenon gas mixture to specific interface conditions to simulate the various operational modes of the solar dynamic power module on the Space Station Freedom. Inlet gas temperature, pressure, and flow rate were independently varied. A total of 58 simulated orbital cycles, each 94 minutes in duration, was completed during the test period.

Sedgwick, L. M.↗

NASA NTRS1987

Total immersion crystal growth

Crystals of wide band gap materials are produced by positioning a holder receiving a seed crystal at the interface between a body of molten wide band gap material and an overlying layer of temperature-controlled, encapsulating liquid. The temperature of the layer decreases from the crystallization temperature of the crystal at the interface with the melt to a substantially lower temperature at which formation of crystal defects does not occur, suitably a temperature of 200 to 600 C. After initiation of crystal growth, the leading edge of the crystal is pulled through the layer until the leading edge of the crystal enters the ambient gas headspace which may also be temperature controlled. The length of the column of liquid encapsulant may exceed the length of the crystal such that the leading edge and trailing edge of the crystal are both simultaneously with the column of the crystal. The crystal can be pulled vertically by means of a pulling-rotation assembly or horizontally by means of a low-angle withdrawal mechanism.

Morrison, Andrew D.↗

DOE OSTI2022

Avoiding CO 2 Improves Thermal Stability at the Interface of Li 7 La 3 Zr 2 O 12 Electrolyte with Layered Oxide Cathodes

Abstract Solid‐state batteries promise higher energy densities and better safety than Li‐ion batteries with liquid electrolytes. However, the interface between solid electrolyte and cathode is unstable at the elevated temperatures that are needed while sintering to achieve good bonding between ceramic components. Here, the hypothesis is that, the gas environment, especially the presence of CO 2, is critical in determining the stability of the solid electrolyte–cathode interface. The effect of gas species on the interface is systematically probed, by a using Li 7 La 3 Zr 2 O 12 (LLZO) solid electrolyte with a thin film LiNi 0.6 Mn 0.2 Co 0.2 O 2 cathode as a model system to enable interface sensitivity. Detrimental phases formed at the interface and their onset conditions are identified by X‐ray absorption spectroscopy, X‐ray diffraction, and Gibbs free energy analysis. As a result, removing CO 2 and minimizing H 2 O(g) during sintering is necessary to obtain good contact at the LLZO|cathode interface without forming secondary phases. Sintering in O 2 is ideal, yielding excellent chemical stability and low interfacial resistance. Secondary phases also do not form in N 2, but oxygen loss occurs at elevated temperatures. The interfacial resistance obtained upon sintering in pure O 2 is comparable to the lowest values at LLZO interfaces with protective coatings, but here without the need for interface coatings.

25 ENERGY STORAGE↗

DOE OSTI2024

Cryogenic aspects of a 20 MW class low-temperature superconducting generator for the renewables industry

In this paper we give a progress update on the cryogenic design for cooling a 20 MW class, partially superconducting generator with stationary field coils for offshore wind renewables industry [1-2]. This is a continuation of an earlier program on a 10 MW system dating back ten years. Whereas this new power rating increase leads to a radial diameter expansion of the superconducting field coils from 4 to > 9.5 m, it maintains the axial length. We show the design based on this scaled up with enlarged diameter. The field coil size increase asks for higher cooling power that leads to a bigger cold box size to accommodate the cryocoolers. In the design, as many as 8 cryocoolers can be accessed and serviced from the nacelle that houses the main cryogenic components. A typical thermal load balance sheet with all components is given and compared against the available cryocooler cooling power at different operating conditions. Due to the cryocoolers’ local point of contact cooling within the nacelle, the temperature gradient of the thermal shield that fully encloses the cold mass with its embedded field coils needs to be balanced out to minimize the heat burden on the field coils. This requires additional analytical efforts and implementation of further design features. The extended nacelle houses the cold box with its cryogenic infrastructure. The interface for the envisaged cryogenic pushbutton closed-loop circulating system remains invisible, requires no handling of cryogenic liquids and is hermetically closed. The field coil diameter increase also leads to a greater initial helium gas storage volume. In addition, it requires higher initial room temperature fill pressure within the toroidal helium vapor storage tanks and in cooling tubes connecting to the cryocoolers. The toroidal helium gas tanks are thermally coupled with the thermal shield so that helium convection inside the storage tank can improve heat transfer and reduce the temperature gradient of the thermal shield. Besides those heat transfer challenges, additional mechanical strain within this large structure is exerted on the torque tubes during initial cooldown and when energizing field coils. Some of those design challenges are quite unexpected, leading to novel workarounds in order to maintain the chosen cooling strategy. Finally, we assess those design limitations in view of further cryogenic scalability with emphasis on manufacturability and assembly.

cryogenics↗

NASA NTRS1999

Buoyancy Driven Shear Flows of Bubble Suspensions

In this work the gas volume fraction and the root-mean-squared fluid velocity are measured in buoyancy driven shear flows of bubble suspensions in a tall, inclined, rectangular channel. The experiments are performed under conditions where We << 1a nd Re >> 1, for which comparisons are made with kinetic theory and numerical simulations. Here Re = gamma(a(exp 2)/nu is the Reynolds number and We = rho(gamma(exp 2))a(exp 3)/sigma is the Weber number; gamma is the shear rate, a is the bubble radius, nu is the kinematic viscosity of the liquid, rho is the density of the liquid, and sigma is the surface tension of the gas/liquid interface. Kang et al. calculated the bubble phase pressure and velocity variance of sheared bubble suspensions under conditions where the bubbles are spherical and the liquid phase velocity field can be approximated using potential flow theory, i.e. We= 0 and Re >> 1. Such conditions can be achieved in an experiment using gas bubbles, with a radius of O(0.5mm), in water. The theory requires that there be no average relative motion of the gas and liquid phases, hence the motivation for an experimental program in microgravity. The necessity of performing preliminary, Earth based experiments, however, requires performing experiments where the gas phase rises in the liquid, which significantly complicates the comparison of experiments with theory. Rather than comparing experimental results with theory for a uniform, homogeneous shear flow, experiments can be compared directly with solutions of the averaged equations of motion for bubble suspensions. This requires accounting for the significant lift force acting on the gas phase when the bubbles rise parallel to the average velocity of the sheared suspension. Shear flows can be produced in which the bubble phase pressure gradient, arising from shear induced collisions amongst the bubbles, balances a body force (centrifugal or gravitational) on the gas phase. A steady, non-uniform gas volume fraction can be measured, from which the bubble phase pressure gradient can be obtained and compared to theory and numerical simulations. The presence of bounding walls further complicates the experiments, since the detailed interactions of the bubbles with bounding walls is not well understood, especially in the presence of gravity, where the momentum and energy exchange depends on the inclination of the wall.

Koch, D. L.↗

DOE OSTI2021

Multichannel gas-uptake/evolution reactor for monitoring liquid-phase chemical reactions

The design of a headspace pressure-monitoring reactor for measuring the uptake/evolution of gas in gas–liquid chemical transformations is described. The reactor features a parallel setup with ten-reactor cells, each featuring a low working volume of 0.2–2 ml, a pressure capacity from 0 to 150 PSIa, and a high sensitivity pressure transducer. The reactor cells are composed of commercially available disposable thickwalled glassware and compact monolithic weld assemblies. The software interface controls the reactor temperature while monitoring pressure in each of the parallel reactor cells. Reactions are easy to set up and yield high-density gas uptake/evolution data. This instrument is especially well suited to acquire quantitative time-course data for reactions with small quantities of gas consumed or produced.

47 OTHER INSTRUMENTATION↗

DOE OSTI2025

Insight into pseudo-film-boiling in supercritical water under simplified interfacial conditions

The focus of this paper is the physics of supercritical water film boiling through the simulation of natural convection of supercritical water in a rectangular cavity. It has been widely believed that above a fluid's critical point, only one phase exists. However, recent research has indicated the existence of distinct gas-like and liquid-like regions separated by the Widom line, which is the locus of the maxima of the specific heat. Along the Widom line, density decreases sixfold, viscosity drops by a factor of two, while specific heat spikes by an order of magnitude. These variations, specifically in density and viscosity, produce a thick pseudo-interface and flow dynamics behavior akin to film-boiling, denoted here as pseudo-two-phase flow dynamics. When the cavity is heated from the bottom, a pseudo-film of gas-like fluid is formed at the heated wall, and the flow complexity evolves, characterized by the formation of multiple vortices. Results demonstrate the ability of modern conjugate heat transfer computational fluid dynamics to capture the pseudo two-phase regime, with the formation of a pseudo-film at the heated wall. Further, the boiling curve is studied, showing an increase in heat flux with an increase in the temperature differential between the wall and the pseudo-critical temperature. Furthermore, results also show a previously uncharacterized instability, where the convection cells in the cavity oscillate and can flip directions under certain conditions.

Computational fluid dynamics↗

NASA NTRSDate not supplied

Validation of Two-Phase Flow Modeling Techniques in Loci-Stream Using Axial Jet Pressure Control and Autogenous Pressurization Experiments

Improvements to computational fluid dynamics modeling of cryogenic fluid management operations are presented with experimental validations. Modeling improvements includes utilizing improved delayed detaches eddy simulation to more effectively model turbulence compared to the Reynolds-averaged Navier Stokes modeling, modeling temperature dependent tank solid properties to capture large variation in thermodynamic properties at cryogenic conditions, modeling real gas equation of state for hydrogen instead of ideal gas behavior, and an on-going effort to improve interface turbulence transport for the volume of fluid method. Two flight-scale ground tests, five K-site tank axial jet pressure control experiments and an Engineering Design Unit tank autogenous pressurization experiment are validated and show the effectiveness of the improved modeling techniques. The successful validation establishes further trust in these models for flight project support and provides a pathway for maturation of in-development interface turbulence damping model for the volume of fluid method for more generalized applications.

CFD↗

DOE OSTI2019

Numerical Simulation and Experimental Investigation of Nitrogen Transfer Mechanism from Gas to Liquid Steel During Pressurized Electroslag Remelting Process

Since the gas–slag–metal three-phase transfer mechanism of nitrogen is not suitable to account for the nitrogen pickup during pressurized electroslag remelting process, the laboratory experiments have been carried out to study the transfer mechanism of nitrogen using different nitrogen partial pressures and electrode immersion depths. Then, two possible transfer mechanisms of nitrogen have been proposed, and a 2D transient numerical model has been developed to investigate the behavior of nitrogen based on the new proposed mechanisms. The simulated results are compared with the experiment to validate the feasibility of new proposed mechanism. The results show that the nitrogen content in ingot increases with the increasing nitrogen partial pressure and decreasing electrode immersion depth. At the current experimental condition, the electrode immersion depth seems to play a more important role in the nitrogen pickup than the nitrogen partial pressure. Due to the limits of thermodynamic and kinetic conditions, the nitrogen pickup is negligible via the transfer from gas to liquid metal through molten slag whether nitrogen chemically or physically dissolves into slag. The mechanism that nitrogen directly reacts with the partially exposed liquid metal film under the electrode tip due to the fluctuation of gas/slag interface could reasonably account for the experimental results. Furthermore, based on the mechanism, the predicted variation tendency of nitrogen content in ingot is in agreement with the experiment.

36 MATERIALS SCIENCE↗

NASA NTRSDate not supplied

Validation of Two-phase Flow Modeling Techniques in Loci-Stream using Axial Jet Pressure Control and Autogenous Pressurization Experiment

CFD↗

NASA NTRS2003

Pore Formation and Mobility Investigation (PPMI): Description and Initial Analysis of Experiments Conducted aboard the International Space Station

Flow visualization experiments during the controlled directional melt back and re-solidification of succinonitrile (SCN) and SCN-water mixtures were conducted using the Pore Formation and Mobility Investigation (PFMI) apparatus in the glovebox facility (GBX) aboard the International Space Station. The study samples were initially 'cast' on earth under 450 millibar of nitrogen into 1 cm ID glass sample tubes approximately 30 cm in length, containing 6 in situ thermocouples. During the Space experiments, the processing parameters and flow visualization settings are remotely monitored and manipulated from the ground Telescience Center (TSC). The ground solidified sample is first subjected to a unidirectional melt back, generally at 10 microns per second, with a constant temperature gradient ahead of the melting interface. Bubbles of different sizes are seen to initiate at the melt interface and, upon release from the melting solid, translate at different speeds in the temperature field ahead of them before coming to rest. Over a period of time these bubbles dissolve into the melt. The gas-laden liquid is then directionally solidified in a controlled manner, generally starting at a rate of 1 micron /sec. Observation and preliminary analysis of bubble formation and mobility in pure SCN samples during melt back and the subsequent structure resulting during gas generation upon re-solidification are presented and discussed.

Grugel, R. N.↗

NASA NTRS2002

Pore Formation and Mobility Investigation (PFMI): Description and Initial Analysis of Experiments Conducted aboard the International Space Station

Flow visualization experiments during the controlled directional melt back and re-solidification of succinonitrile (SCN) and SCN-water mixtures were conducted using the Pore Formation and Mobility Investigation (PFMI) apparatus in the glovebox facility (GBX) aboard the International Space Station. The study samples were initially "cast" on earth under 450 millibar of nitrogen into 1 cm ID glass sample tubes approximately 30 cm in length, containing 6 in situ thermocouples. During the Space experiments, the processing parameters and flow visualization settings are remotely monitored and manipulated from the ground Telescience Center (TSC). The ground solidified sample is first subjected to a unidirectional melt back, generally at 10 microns per second, with a constant temperature gradient ahead of the melting interface. Bubbles of different sizes are seen to initiate at the melt interface and, upon release from the melting solid, translate at different speeds in the temperature field ahead of them before coming to rest. Over a period of time these bubbles dissolve into the melt. The gas-laden liquid is then directionally solidified in a controlled manner, generally starting at a rate of 1 micron /sec. Observation and preliminary analysis of bubble formation and mobility in pure SCN samples during melt back and the subsequent structure resulting during gas generation upon re-solidification are presented and discussed.

Grugel, R. N.↗

NASA NTRS2010

A History of Collapse Factor Modeling and Empirical Data for Cryogenic Propellant Tanks

One of the major technical problems associated with cryogenic liquid propellant systems used to supply rocket engines and their subassemblies and components is the phenomenon of propellant tank pressurant and ullage gas collapse. This collapse is mainly caused by heat transfer from ullage gas to tank walls and interfacing propellant, which are both at temperatures well below those of this gas. Mass transfer between ullage gas and cryogenic propellant can also occur and have minor to significant secondary effects that can increase or decrease ullage gas collapse. Pressurant gas is supplied into cryogenic propellant tanks in order to initially pressurize these tanks and then maintain required pressures as propellant is expelled from these tanks. The net effect of pressurant and ullage gas collapse is increased total mass and mass flow rate requirements of pressurant gases. For flight vehicles this leads to significant and undesirable weight penalties. For rocket engine component and subassembly ground test facilities this results in significantly increased facility hardware, construction, and operational costs. "Collapse Factor" is a parameter used to quantify the pressurant and ullage gas collapse. Accurate prediction of collapse factors, through analytical methods and modeling tools, and collection and evaluation of collapse factor data has evolved over the years since the start of space exploration programs in the 1950 s. Through the years, numerous documents have been published to preserve results of studies associated with the collapse factor phenomenon. This paper presents a summary and selected details of prior literature that document the aforementioned studies. Additionally other literature that present studies and results of heat and mass transfer processes, related to or providing important insights or analytical methods for the studies of collapse factor, are presented.

deQuay, Laurence↗

NASA NTRSDate not supplied

Axisymmetric Two-Dimensional Modeling of No Vent Filling of a Cryogenic Tank using Generalized Fluid System Simulation Program

This paper presents preliminary analysis using a finite volume based computational method for network flow analysis for the simulation of chill and fill of a cryogenic tank. An axisymmetric two-dimensional model of a spherical tank was developed using a nodal approach. No Vent Filling (NVF) was accomplished using a Thermodynamic Vent System assisted injector where the injector was cooled by the cold gas generated by Joule-Thompson expansion of the liquid propellant. The numerical model accounts for a) different regimes of pool boiling heat transfer, b) condensation of vapor around spray droplets, and c) condensation of vapor at the interface of the cooled injector and ullage. The numerical predictions of tank pressure, filling rate, and wall temperatures were compared with the test data and one-dimensional (1D) model predictions. It was demonstrated that the axisymmetric 2D model provided a more realistic prediction than the 1D model.

Cryogenics↗