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All sources NASA NTRS DOE OSTI

DOE OSTI2023

Machine learning-based ethylene and carbon monoxide estimation, real-time optimization, and multivariable feedback control of an experimental electrochemical reactor

Electrochemical reduction of CO 2 gas is a novel CO 2 utilization technique that has the potential to mitigate the global climate crisis caused by anthropogenic CO 2 emissions, and enable the large-scale storage of energy generated from renewable sources in the form of carbon-based chemicals and fuels. However, due to the complexity of the electrochemical reactions, the explicit first-principles models for CO2 reduction are not available yet, and there has been a limited effort to develop process modeling, optimization and control of CO 2 electrochemical reactors. To this end, a rotating cylinder electrode (RCE) reactor has been constructed at UCLA to understand the mass transfer and reaction kinetics effects separately on the productivity. In the RCE reactor, the applied potential strongly influences the reaction energetics and the electrode rotation speed affects the hydrodynamic boundary layer and modifies the film mass transfer coefficient, which involves convective and diffusive transport. Further, the present work aims to develop a multi-input multi-output (MIMO) control scheme for the RCE reactor that integrates techniques from artificial and recurrent neural network modeling, nonlinear optimization, and process controller design. Specifically, production rates of two products from the experimental reactor, ethylene and carbon monoxide, are controlled by manipulating two inputs, applied potential and catalyst rotation speed. Process dynamics and controllability are analyzed, a feedback control strategy is designed and the controllers are tuned accordingly. The experimental electrochemical cell is employed to gather data for process modeling and implement the multivariable control system. Finally, the experimental results are presented which demonstrate excellent closed-loop performance by the control system and regulation of the outputs at three different set-points including an economically-optimal set-point.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Hydrogen embrittlement of Zircaloy-4 fabricated by ultrasonic additive manufacturing

Ultrasonic additive manufacturing (UAM) was successfully applied to the zirconium material system to create a planar geometry. Following fabrication, SS-J3 type tensile specimens of the UAM and wrought Zircaloy-4 with a nominal gage section of 5×1.2×0.75 mm were machined for hydriding studies and mechanical testing. The SS-J3 type tensile specimens were gas-charged with hydrogen using a custom system that precisely controls hydrogen gas flow rate, hydrogen partial pressure, and temperature. To avoid altering the UAM material, the maximum process temperature was limited to 550°C. Using different initial hydrogen gas pressures and flow rates, various hydrogen contents (70–1755 wppm) were achieved for Zircaloy-4 specimens. Tensile testing shows that, regardless of hydrogen content, all UAM specimens measured yield strengths in the range of 557±16 MPa and ultimate tensile strengths of 660±4MPa. However, total elongation clearly decreased as a function of increasing hydrogen content. Further, at the lowest hydrogen content, the total plastic elongation measured 21.5%, and this value decreased to less than 2% when the hydrogen content was increased to 1000 wppm. Cross-sectional optical microscopy images revealed that the hydride distributions are randomly oriented. For the low hydrogen content specimen, these randomly distributed hydrides are isolated from each other. A sandwiched structure, consisting of high-density and low-density layers, was also observed for the specimens with hydrogen content between 200 and 400 wppm. As the hydrogen content increases, the hydrides diffuse into the low-density hydride layers to form a network across the whole specimen. Although the tensile properties of UAM and wrought Zircaloy-4 exhibit the same behavior with increasing hydrogen content, the distinctions in grain orientations led to differences in the hydride orientations at low and intermediate hydrogen concentrations.

36 MATERIALS SCIENCE↗

NASA NTRS1997

An Ecosystem Simulation Model for Methane Production and Emission from Wetlands

Previous experimental studies suggest that methane emission from wetland is influenced by multiple interactive pathways of gas production and transport through soil and sediment layers to the atmosphere. The objective of this study is to evaluate a new simulation model of methane production and emission in wetland soils that was developed initially to help identify key processes that regulate methanogenesis and net flux of CH4 to the air, but which is designed ultimately for regional simulation using remotely sensed inputs for land cover characteristics. The foundation for these computer simulations is based on a well-documented model (CASA) of ecosystem production and carbon cycling in the terrestrial blaspheme. Modifications to represent flooded wetland soils and anaerobic decomposition include three new sub-models for: (1) layered soil temperature and water table depth (WTD) as a function of daily climate drivers, (2) CH4 production within the anoxic soil layer as a function of WTD and CO2 production under poorly drained conditions, and (3) CH4 gaseous transport pathways (molecular diffusion, ebullition, and plant vascular transport) as a function of WTD and ecosystem type. The model was applied and tested using climate and ecological data to characterize tundra wetland sites near Fairbanks, Alaska studied previously by Whalen and Reeburgh. Comparison of model predictions to measurements of soil temperature and thaw depth, water-table depth, and CH4 emissions over a two year period suggest that inter-site differences in soil physical conditions and methane fluxes could be reproduced accurately for selected periods. Day-to-day comparison of predicted emissions to measured CH4 flux rates reveals good agreement during the early part of the thaw season, but the model tends to underestimate production of CH4 during the months of July and August in both test years. Important seasonal effects, including that of falling WTD during these periods, are apparently overlooked in the model formulation. Nevertheless, reasonably close agreement was achieved between the model's mean daily and seasonal estimates of CH4 flux and observed emission rates for northern wetland ecosystems. Several features of the model are identified as crucial to more accurate prediction of wetland methane emission, including the capacity to incorporate influences of localized topographic and hydrologic features on site-specific soil temperature and WTD dynamics, and mechanistic simulation of methane emission transport pathways from within the soil profile.

Potter, C. S.↗

DOE OSTI2020

Surface effects on deuterium permeation through vanadium membranes

Dense vanadium-based membranes offer high permeability and perfect selectivity to hydrogen isotopes, maintain favorable neutronic properties, and are compatible with liquid metals such as PbLi. These properties make vanadium membranes a promising fusion fuel cycle technology for processes such as tritium extraction from PbLi and exhaust processing. Surface contamination has a deleterious effect on the gas-phase hydrogen permeation through vanadium, and the reported permeabilities range from 10 -14 to 10 -7 mol m -1 s -1 Pa -0.5 . Thin dense films of palladium applied to clean vanadium surfaces enable a consistently high hydrogen permeability. In this study, uncoated vanadium resulted in deuterium permeabilities ranging from 2.8 × 10 -11 to 6.4 × 10 -9 mol m -1 s -1 Pa -0.5 at 300 °C–700 °C, respectively. Post-test analysis revealed a VO x surface layer and VC x subsurface layer formed on the feed side, while the as-received surface oxide dissolved leaving a submonolayer oxide on the permeate surface. Furthermore, the Pd-coated V resulted in a maximum deuterium permeability of 2.1 × 10 -7 m -1 s -1 Pa -0.5 at 375 °C upon activation of the Pd surface by oxidation and reduction. The deuterium permeation declined upon heating to 500 °C due to intermetallic diffusion between the Pd and V. The Mo 2 C-coated V resulted in deuterium permeabilities ranging from 2.7 × 10 -10 to 1.8 × 10-9 at 500 °C–700 °C, respectively, and a post-test analysis found the carbon in the Mo 2 C layer had dissolved into the V near the interface.

13 HYDRO ENERGY↗

DOE OSTI2024

DNS of ignition and flame stabilization in a simplified gas turbine premixer

With the increasing need for fuel flexibility, mitigation of auto-ignition (AI) inside gas turbine (GT) premixers becomes crucial. They must be designed to yield a sufficiently homogeneous fuel-air mixture to achieve low emissions while at the same time avoiding the occurrence of AI and subsequent flame stabilization. This challenge requires a detailed understanding of turbulent mixing and chemistry interactions. In the present work, a direct numerical simulation (DNS) of an array of jets in crossflow (JICF), representative of an industrial GT premixer, is reported to shed light on these complex phenomena. It is found that AI kernels form in the aft part of the premixer and coalesce into a flame front that then propagates upstream, mainly through the boundary layer, and successively engulfs the jets. This, therefore, suggests a significant role of the jet array pattern on the flame stabilization. It is noted that AI kernels continue to form independently during the whole time of the simulation. To clarify the contribution of AI and diffusion in the ignition kernels and the main flame, chemical explosive mode analysis (CEMA) is employed jointly with a kernel tracking algorithm. It is found that during the initial formation of the flame, many ignition kernels form in mixtures with low scalar dissipation rate and large contribution from AI mode. As they quickly grow, they merge into a single flame front that becomes increasingly more diffusion-assisted over time, balancing the AI mode. Turbulence is shown to have a significant enhancing effect in lean premixed flames, but further analysis is required to fully characterize it. These findings are relevant for the industrial premixer studied, and also for novel micromix concepts that may be used in the next generation of GT combustion systems.

ADVANCED PROPULSION SYSTEMS↗

NASA NTRS2018

PIV and Rotational Raman-Based Temperature Measurements for CFD Validation in a Single Injector Cooling Flow

NASA's Turbulent Heat Flux (THX) task under the Transformational Tools & Technologies project is focused on acquiring benchmark temperature and velocity data in turbulent shear layers for validation of computational fluid dynamics (CFD) codes. Standard CFD turbulence models lack the ability to accurately calculate a number of fundamental flow phenomena, including the turbulent transport of heat. In nearly all production class Reynolds-averaged Navier-Stokes (RANS) CFD codes, a gradient-diffusion approximation is used whereby a constant turbulent Prantdl number, Prt, is used to relate an eddy viscosity calculated for the momentum terms, to the turbulent heat flux terms. The default in most CFD codes is Prt = 0.9, however this is not representative of all flows. As discussed in Yoder et al. (2015) and Reynolds (1974), Prt = 0.7 is felt to be more appropriate for jets. Recent work, as discussed in Yoder (2016a), has explored more complex formulations including variable turbulent Prantdl number models. PARTICLE IMAGE VELOCIMETRY; TEMPERATURE MEASURING INSTRUMENTS; FILM COOLING; HIGH TEMPERATURE GASES; COMPUTATIONAL FLUID DYNAMICS; PREDICTION ANALYSIS TECHNIQUES; TURBULENCE MODELS; RAMAN SPECTRA; VELOCITY; MACH NUMBER; GAS TURBINE ENGINES; NOZZLE FLOW; THERMOCOUPLES; LASER INDUCED FLUORESCENCE; COOLING FLOWS (ASTROPHYSICS); RAMAN SPECTROSCOPY; HEAT FLUX

Wernet, Mark P.↗

DOE OSTI2022

Demonstrate Improved Ag Diffusion and Describe the Basis for Pd Penetration Modeling in SiC

In past work, an effective diffusivity coefficient was determined for Ag transport through the silicon carbide layer of a tristructural isotropic fuel particle. The effective diffusivity coefficient accounts for the microstructure of the silicon carbide and includes both bulk diffusion and grain boundary diffusion of Ag. In this report, the model has been improved by accounting for the enhanced concentration of vacancies in the bulk due to irradiation, which substantially influence bulk diffusivity at low temperatures. To improve the BISON model and make it fission rate dependent, effective diffusivity calculations have been performed that incorporate the radiation modified bulk diffusivity. The microstructure and irradiation-dependent effective diffusivity has also been implemented into BISON, and its predictions for Ag release from tristructural isotropic fuel have been successfully compared to AGR-1 post irradiation measurements. Moreover, a new feature has been developed in the Multiphysics Object-Oriented Simulation Environment (MOOSE) to account for different grain boundary types. The Ag diffusivity in 5 (210)/[001] grain boundaries has been computed and was found to be greater than in random high-angle grain boundaries. The presence of the fission product Pd can also have an important effect on the properties of the silicon carbide layer in tristructural isotropic particles. The penetration of Pd into the silicon carbide layer causes a corrosion reaction that can lead to the failure of the silicon carbide layer; however, this corrosion reaction is not well understood. To enable an improved understanding of the mechanism, ab-initio molecular dynamics simulations of Pd interaction with bulk silicon carbide have been performed. The improved understanding of the reaction will form a basis for future improvements to the BISON’s Pd penetration failure model

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Automated Segmentation of Twin Boundaries in TRISO Silicon Carbide Using Deep Neural Networks

Coated particle fuels, such as the tristructural isotropic (TRISO) fuel particle, are essential for high-temperature gas reactor (HTGR) applications due to their efficiency and stability under normal and off-normal conditions. However, widespread commercialization and deployment of this technology for next-generation nuclear applications require robust quality assurance and quality control (QA/QC) methods linking fabrication, properties, and performance. Of the many important metrics for TRISO QA/QC, quantification of the silicon carbide (SiC) microstructure is critical because it correlates with fission product retention during irradiation. Previous work has shown extensive twinning of the SiC microstructure, which strongly affects microstructural metrics; however, twin grain boundaries are not expected play a significant role in fission product diffusion. This report summarizes the initial development, training, and testing of a machine learning image processing algorithm to detect twin grain boundaries in a backscattered electron image, which can be removed so that microstructural metrics can be recalculated for legacy data. Further development and deployment of this model will provide automated, scalable improvement of potential QA/QC methods for the SiC layer of TRISO particles.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS2005

Numerical Analysis of Flow Evolution in a Helium Jet Injected into Ambient Air

A computational model to study the stability characteristics of an evolving buoyant helium gas jet in ambient air environment is presented. Numerical formulation incorporates a segregated approach to solve for the transport equations of helium mass fraction coupled with the conservation equations of mixture mass and momentum using a staggered grid method. The operating parameters correspond to the Reynolds number varying from 30 to 300 to demarcate the flow dynamics in oscillating and non-oscillating regimes. Computed velocity and concentration fields were used to analyze the flow structure in the evolving jet. For Re=300 case, results showed that an instability mode that sets in during the evolution process in Earth gravity is absent in zero gravity, signifying the importance of buoyancy. Though buoyancy initiates the instability, below a certain jet exit velocity, diffusion dominates the entrainment process to make the jet non-oscillatory as observed for the Re=30 case. Initiation of the instability was found to be dependent on the interaction of buoyancy and momentum forces along the jet shear layer.

Satti, Rajani P.↗

NASA NTRS1994

Dirbe evidence for a wrap in the interstellar dust layer and stellar disk of the galaxy

The Diffuse Infrared Background Experiment (DIRBE) of the Cosmic Background Explorer (COBE) has mapped the surface brightness distributions of the Galactic plane at wavelengths from 1.25 to 240 micrometers. In these maps the latitude of peak brightness, as a function of longitude, traces a roughly sinusoidal curve of period approximately 360 deg. In the far-infrared, where emission by interstellar dust dominates the surface brightness, this curve agrees well with that derived from maps of the velocity-integrated H 1, suggesting that the layers of dust and neutral atomic hydrogen are similarly displaced from the Galactic plane. In the near-infrared (lambda less than 5 micrometers), where old disk stars dominate the emission, the brightness crest exhibits the same phase but roughly half the amplitude. The reduced amplitude of the warp in stellar light could result from a lesser warping of the stellar disk, or from a more rapid falloff of the density of stars relative to the density of gas, possibly due to a radial truncation of the disk.

Freudenreich, H. T.↗

NASA NTRS2000

Effect of Film-Hole Shape on Turbine Blade Film Cooling Performance

The detailed heat transfer coefficient and film cooling effectiveness distributions as well as tile detailed coolant jet temperature profiles on the suction side of a gas turbine blade A,ere measured using a transient liquid crystal image method and a traversing cold wire and a traversing thermocouple probe, respectively. The blade has only one row of film holes near the gill hole portion on the suction side of the blade. The hole geometries studied include standard cylindrical holes and holes with diffuser shaped exit portion (i.e. fanshaped holes and laidback fanshaped holes). Tests were performed on a five-blade linear cascade in a low-speed wind tunnel. The mainstream Reynolds number based on cascade exit velocity was 5.3 x 10(exp 5). Upstream unsteady wakes were simulated using a spoke-wheel type wake generator. The wake Strouhal number was kept at 0 or 0.1. Coolant blowing ratio was varied from 0.4 to 1.2. Results show that both expanded holes have significantly improved thermal protection over the surface downstream of the ejection location, particularly at high blowing ratios. However, the expanded hole injections induce earlier boundary layer transition to turbulence and enhance heat transfer coefficients at the latter part of the blade suction surface. In general, the unsteady wake tends to reduce film cooling effectiveness.

Han, J. C.↗

NASA NTRS1986

Assessment of a parabolic analysis for axisymmetric internal flows in rocket and turbomachinery ducts

The flow paths in gas turbine passages encompass a wide range of flow properties such as Reynolds number and Mach number as well as many other variable flow conditions such as swirl, free-stream turbulence, and laminar/turbulent transition. An existing computer program, the Axisymmetric Diffuser Duct (ADD) code, which calculates compressible, turbulent, swirling flow through axisymmetric ducts has been modified to include the effects of free-stream turbulence and laminar/turbulent transition. The program has been evaluated on a matrix of test cases to determine its accuracy, robustness, and limits of applicability. This improved version of the ADD code calculates solutions which compare well with available data and can now be applied to a wider range of problems than previously possible. In addition a concept called local enhancement was developed and tested on a simple two-dimensional geometry in order to demonstrate a method to reduce computer time. In this concept the pressure distribution is calculated on a coarse grid using the ADD code and the viscous layer is locally enhanced using a boundary layer analysis. By applying this concept, an order of magnitude reduction in computer time was possible without any loss in accuracy.

Power, G. D.↗

DOE OSTI2020

Axial magnetic flux amplification in Hall-magnetohydrodynamic simulations of externally magnetized z-pinches

It is shown that externally magnetized gas-puff z-pinches under compression can exhibit robust axial flux amplification under suitable axial boundary conditions. This effect relies upon the Hall term in the generalized Ohm's law to generate azimuthal currents in the presence of a driving axial electric field. Under dynamic compression, the total current tends to flow in a mostly force-free boundary layer, separating the predominately azimuthal field outside the layer and the predominately axial field inside the layer. The effect only appears to occur if the axial boundaries allow for outflow or absorption of electromagnetic energy. The effect is mitigated by imposing either periodic or conducting axial boundary conditions. A semi-analytic equilibrium analysis agrees with steady-state solutions of the time-dependent electron-magnetohydrodynamic equations and provides an estimate of the scaling of the boundary layer as well as suggesting a scenario for the formation of the boundary layer. When operative, the effect can significantly impede plasma compression due to the increase in axial flux that diffuses into the pre-compressed plasma or through the presence of conductors that inhibit movement of the generated axial flux. Several facilities have noted unusual implosion behavior in z-pinch experiments with applied axial fields that does not appear to be explainable within the standard magnetohydrodynamic model. In conclusion, it is suggested that these experiments can be explained by the axial flux amplification and concentration effect

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS1992

Navier-Stokes analysis and experimental data comparison of compressible flow within ducts

Many aircraft employ ducts with centerline curvature or changing cross-sectional shape to join the engine with inlet and exhaust components. S-ducts convey air to the engine compressor from the intake and often decelerate the flow to achieve an acceptable Mach number at the engine compressor by increasing the cross-sectional area downstream. Circular-to-rectangular transition ducts are used on aircraft with rectangular exhaust nozzles to connect the engine and nozzle. To achieve maximum engine performance, the ducts should minimize flow total pressure loss and total pressure distortion at the duct exit. Changes in the curvature of the duct centerline or the duct cross-sectional shape give rise to streamline curvature which causes cross stream pressure gradients. Secondary flows can be caused by deflection of the transverse vorticity component of the boundary layer. This vortex tilting results in counter-rotating vortices. Additionally, the adverse streamwise pressure gradient caused by increasing cross-sectional area can lead to flow separation. Vortex pairs have been observed in the exit planes of both duct types. These vortices are due to secondary flows induced by pressure gradients resulting from streamline curvature. Regions of low total pressure are produced when the vortices convect boundary layer fluid into the main flow. The purpose of the present study is to predict the measured flow field in a diffusing S-duct and a circular-to-rectangular transition duct with a full Navier-Stokes computer program, PARC3D, and to compare the numerical predictions with new detailed experimental measurements. The work was undertaken to extend previous studies and to provide additional CFD validation data needed to help model flows with strong secondary flow and boundary layer separation. The S-duct computation extends the study of Smith et al, and Harloff et al, which concluded that the computation might be improved by using a finer grid and more advanced turbulence models. The present study compares results for both the Baldwin-Lomas and k-epsilon turbulence models and is conducted with a refined grid. For the transition duct, two inlet conditions were considered, the first with straight flow and the second with swirling flow. The first case permits examination of the effects of the geometric transition on the flow field, while the second case includes the rotational flow effect characteristic of a gas turbine engine.

Harloff, G. J.↗

NASA NTRS1998

Monitoring of Volcanogenic CO2-Induced Tree Kills with AVIRIS Image Data at Mammoth Mountain, California

Elevated cold CO2 emissions from the flank of Mammoth Mountain volcano on the southwest rim of the Long Valley Caldera, eastern California, have been the cause of over 100 acres of dead trees in that area since 1990. The source of the CO2 gas is thought to be from one or more magmatic intrusion(s) beneath Mammoth Mountain and is probably related to a period of seismic unrest that began in 1989. The gas rises to the surface probably from depths of a few kilometers, along faults and fracture zones. The gas is at ambient temperature and diffuses from the soil rather than discharging from distinct vents. Typically, soil gas concentrations in tree-kill areas range from 10% to over 90% CO2 by volume, as compared to normal background of < 1% in healthy forest. The gas composition is predominantly CO2 mixed with air (sulfur gases are not elevated), and C and He isotopic ratios are consistent with a magmatic origin for the gas. The total CO2 emission has been estimated at 1200 tons/day, comparable to the emissions at Kilauea. Some of the dead trees are as old as 250 years, suggesting that similar anomalous gas discharge has not occurred over the previous few hundred years. The delta C-13/12 ratio in the Mammoth Mountain CO2 emission averages about -4.5 (PDB standard). This is consistent with a mantle source for the carbon. However, the large volume of the emission suggests that not all of the CO2 is necessarily being generated from the 1989 intrusion. The voluminous gas could be leaking from a vapor-rich zone, capped by an impermeable layer, that was supplied CO2 from degassing of many small magma bodies that intruded beneath the mountain over a period of decades or centuries. Earthquakes in 1989 could have fractured the capping layer and provided pathways for the escape Of CO2 to the surface. Alternatively, some of the CO2 could be derived from contact metamorphism of carbonate rocks intruded by magma. Carbonate-bearing Paleozoic roof pendents crop out in close proximity to Mammoth Mountain. It is possible that similar rocks could occur at depth beneath Mammoth Mountain, and could have contributed CO2 from thermal decomposition caused from recent intrusions. We hope to determine the C-13/12 ratio of a suite of samples to demonstrate if the carbonate rocks could be the source of at least part of the 1990-97 CO2 emission. To better understand the behavior of the CO2 gas, we have used hyperspectral imagery data of Mammoth Mountain acquired from the Airborne Visual/Infrared Imaging Spectrometer (AVIRIS) to map out areas of dead trees. The areas of tree kill have increased in size from about 50 acres in 1994 to about 100 acres in 1997. Tree kill is the major surface manifestation of the carbon dioxide flux at Mammoth Mountain, is widely dispersed, and has been cursorily mapped by regular field mapping techniques in the area. Initial investigations using airborne digital imagery from the Thematic Mapper Simulator (NS001) and AVIRIS instruments have shown extremely encouraging results for complete delineation of the vegetation anomalies. The most successful maps (when compared with ground truth) were developed using AVIRIS data with spectral angle mapper and matched filter algorithms with a data set that was reduced to maximum variance via the minimum noise fraction transformation. The result of this work is a series of maps that show the tree kill areas occurring in an halo-pattern surrounding the base of Mammoth Mountain. We are applying these same techniques to earlier AVIRIS images of Mammoth Mountain to examine the progression of the tree kill areas over time. Temporal maps of the tree kill areas may assist in constructing a picture of the structure beneath Mammoth Mountain.

Hausback, Brian P.↗

NASA NTRS1976

Sulfidation of 310 stainless steel at sulfur potentials encountered in coal conversion systems

The sulfidation of SAE 310 stainless steel was carried out in gas mixtures of hydrogen and hydrogen sulfide over a range of sulfur potentials anticipated in advanced coal gasification processes. The kinetics, composition, and morphology of sulfide scale formation were studied at a fixed temperature of 1,065 K over a range of sulfur potentials from .00015 Nm to the -2nd power to 900 Nm to the -2nd power. At all sulfur potentials investigated, the sulfide scales were found to be multilayered. The relative thickness of the individual layers as well as the composition was found to depend on the sulfur potential. The reaction was found to obey the parabolic rate law after an initial transient period. Considerably longer transient periods were found to be due to unsteady state conditions resulting from compositional variations in the spinel layer. The sulfur pressure dependence on the parabolic rate constant was found to best fit the equation K sub p equals const. (P sub S2) to the 1/nth power, where n equals 3.7. The growth of the outer layers was found to be primarily due to the diffusion of metal ions, iron being the predominant species. The inner layer growth was due to the dissociation of the primary product at the alloy scale interface and depended on the activity of chromium.

Rao, D. B.↗

DOE OSTI2023

Analysis of furnace contamination on superconducting radio frequency niobium using secondary-ion mass spectrometry

Detection of surface contamination on niobium materials used in superconducting radio frequency (SRF) applications is difficult due to quantitative sensitivity and near-atomic depth resolution needed. Inspection of samples known to have experienced surface contamination was found to have inconsistent nitride coverage after high-temperature nitrogen gas exposure (“doping”). Here we compare contaminating species found on samples treated in several different vacuum furnaces, both “exposed” directly in the chamber and “protected” by containment shielding from evaporative sources with “furnace caps.” Typically, furnace caps are used to impede contamination from reaching the interior surface of cavities during the high-temperature vacuum bake that immediately precedes exposure to nitrogen gas. Although, to date, little is known about the effectiveness of these caps, SIMS results showed that they were effective in limiting contamination arising from the furnace environment. Inspection of sample surfaces by SEM showed a lack of nitrides present on contaminated specimens. TEM with energy dispersive spectroscopy performed on these samples revealed that a carbon-rich layer now existed, indicating that a relatively high contaminant load prevents the nucleation and growth of surface nitrides, while thus inhibiting interstitial nitrogen uptake. Except in extreme cases, subsequent removal of the top several micrometers of the surface via electropolishing appears to effectively eliminate any strong influence on the subsequent SRF cavity performance. With the absence of furnace cleaning, carbon contamination was found to be nearly 10× higher for protected nitrogen-doped and electropolished samples, with minimal metallic contamination detected for both processes. SIMS analysis was also performed to compare the cleanliness of samples fully prepared by such nitrogen “doping” with those prepared by a related process, involving the dissolution of niobium surface oxide and diffusion of oxygen into the surface. This oxygen doping or alloying process offers attractive advantages.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2021

Evaluating the Feasibility of Measuring and Analyzing Strain Caused by Changes in Barometric Pressure in the Vadose Zone

Changes in barometric pressure propagate into the subsurface where they can affect water level measurements in wells and cause vertical strain. Previous strain sensors were developed to measure vertical strain, but they were limited to measurements at a single depth, making it difficult to evaluate strains from a migrating pressure wave. Technology known as Coherence-length-gated Microwave Photonics Interferometry (CMPI) uses optical fiber sensors to measure strain at multiple locations. It has the potential to detect strain caused by variations in barometric pressure at multiple depths in the subsurface. The goal of this study is to evaluate the feasibility of using this technology to record the changes in vertical strain in the vadose zone from small fluctuations in air pressure. Propagation of these air pressure fluctuations is affected by hydrogeological properties such as water content and permeability. A second goal of this study is to evaluate how these properties affect the air pressure distribution, strain, and gas-phase diffusivity with a long-term goal of using strain to monitor the vadose zone. The focus of this study is on a suite of laboratory experiments that used a sand-filled column with an open head space. The CMPI fiber was packaged and embedded along the axis of the column to measure the strain at multiple locations while air pressure transducers were installed through the wall of the column. Small periodic fluctuations in air pressure, similar to barometric pressure fluctuations, were created in the head space of the column using an audio driven speaker driven at 4 Hz using a sinusoidal signal created by a function generator. Then, the fluctuations propagated along the column where they were measured by the transducers and recorded as functions of time. Initial tests were conducted using dry sand, but then additional tests were conducted after injecting water into the column, which changed the hydrologic and mechanical properties. Another experiment was conducted after creating a thin barrier to air flow, which was designed to simulate a thin layer of saturated ground during rainfall. A final experiment was conducted by changing the grain size of the material to create a heterogeneity in the upper half of the column. The suite of six experiments was conducted to highlight effects of variations in water content and heterogeneities on air pressure and vertical strain. Numerical simulations were also created to evaluate the laboratory data and to provide a baseline analysis for the results. The numerical simulations used the governing equations to linear poroelasticity and two-phase flow with boundary conditions representing the experiments. The conceptual model for strain caused by barometric pressure recognizes that a fluctuating barometric pressure causes fluctuations in the air pore pressure that decrease in amplitude and lag in time with increase depth. The pressure distribution results in two different loads that cause strain: 1.) a mechanical load as the barometric pressure acts on the ground surface; and 2.) pressure loading in the pore space. The results show that the total vertical strain is a contribution of both of these loads, and this is the strain that was observed in the laboratory. The lab experiments show that both air pressure and strain vary as sinusoids that propagate with depth. The amplitude of the air pressure and strain decrease as a function of depth in all the conditions that were evaluate. For example, in the dry sand, the amplitude of the air pressure decreases from 25 Pa at the head space to 5 Pa at a depth of 70 cm, whereas the amplitude of the strain decreases from 0.15 to 0.06 µε over the same depth interval. In many cases the amplitudes decrease is approximately negative exponential functions of depth. When water was injected into the sand and the saturation increased, the amplitude of the air pressure increased in the partially saturated sand but decreased sharply to zero where the soil was saturated. The strain decreased with depth, but the transition from partially to fully saturated conditions had little effect on the strain profile, even though it had a major effect on the air pressure. This apparently is because strain is caused by variations in both water and air pressure. The fluctuating air pressure caused the water pressure to fluctuate, which caused strain throughout the column. Phase delay of the air pressure and the strain both increase as linear to bi-linear functions of depth. The phase delays indicate that pressure propagates at a velocity of 7 to 8 m/s in dry or partially saturated sand, but it drops by more than an order of magnitude in the vicinity of the capillary fringe. The phase delays indicate the strain propagates faster than the pressure. The data indicate that the strain propagates from 1.2 to more than 4x faster than the pressure. Switching from sand to silt in the column caused the velocity of the pressure to drop by roughly half for both pressures, but curiously, it had little effect on the velocity of the strain.

54 ENVIRONMENTAL SCIENCES↗