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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 127 records · Page 7
All sourcesNASA NTRSDOE OSTI
NASA NTRS2016

Compact Multi-Channel Infrared Laser Absorption Spectrometer for Spacecraft Fire Safety Monitoring

We report on the design of a six-channel tunable laser absorption spectroscopy instrument for measuring ambient gas-phase concentrations of CO, HCl, HCN, HF, CO2, and O2 in spacecraft environments. Monitoring of these compounds can provide early warning detection of fire events while also indicating what materials have been exposed to heating. Continued post-fire monitoring of these hazardous gases can also facilitate safe and effective cleanup. The sensor is a miniaturized version of a five-channel prototype that was previously validated in ground-based oxidative pyrolysis tests. Here, we describe absorption line selection and theoretical detection limits for a sensor with reduced absorption pathlengths for each detection channel, which allows for a substantial reduction in overall instrument footprint. Ultimately, the new instrument is designed to be used in fire safety tests conducted by NASA, where various materials will undergo oxidative pyrolysis in an unmanned spacecraft returning from low Earth orbit.

Briggs, Ryan M.↗
NASA NTRS2020

Miniaturized Laser Absorption Spectrometer for Combustion Calorimetry and Process Monitoring

A miniaturized tunable laser absorption spectrometer capable of measuring gas-phase concentrations of CO, CO2, and O2 has been developed for operation in spacecraft environments. As part of the Spacecraft Fire Safety Demonstration (Saffire) project, we previously demonstrated the Combustion Product Monitor (CPM) instrument to characterize pyrolysis of relevant test materials in low gravity aboard a transfer vehicle returning from low Earth orbit. Here, we adapted the CPM instrument design to achieve detection of CO, CO2, and O2 with improved minimum detection limits and dynamic range as well as reduced instrument size and power. The instrument can be operated in either an open or sealed configureation, allowing for ambient gas composition measuremnts or in-line monitoring of gas streams. By accurately monitoring CO, CO2, and O2 with broad pressure/temperature calibration and response time on the order of 1 s, the instrument can be used to characterize the dynamics of combustion reactions in a variety of environments.

Briggs, Ryan M.↗
DOE OSTI2022

Feasibility of source-free DAS logging for next-generation borehole imaging

Characterizing and monitoring geologic formations around a borehole are crucial for energy and environmental applications. However, conventional wireline sonic logging usually cannot be used in high-temperature environments nor is the tool feasible for long-term monitoring. We introduce and evaluate the feasibility of a source-free distributed-acoustic-sensing (DAS) logging method based on borehole DAS ambient noise. Our new logging method provides a next-generation borehole imaging tool. The tool is source free because it uses ever-present ambient noises as sources and does not need a borehole sonic source that cannot be easily re-inserted into a borehole after well completion for time-lapse monitoring. The receivers of our source-free DAS logging tool are fiber optic cables cemented behind casing, enabling logging in harsh, high-temperature environments, and eliminating the receiver repeatability issue of conventional wireline sonic logging for time-lapse monitoring. We analyze a borehole DAS ambient noise dataset to obtain root-mean-squares (RMS) amplitudes and use these amplitudes to infer subsurface elastic properties. We find that the ambient noise RMS amplitudes correlate well with anomalies in conventional logging data. The source-free DAS logging tool can advance our ability to characterize and monitor subsurface geologic formations in an efficient and cost-effective manner, particularly in high-temperature environments such as geothermal reservoirs. Further validation of the source-free DAS logging method using other borehole DAS ambient noise data would enable the new logging tool for wider applications.

58 GEOSCIENCES↗
NASA NTRS2019

The Combustion Product Monitor instrument for the spacecraft fire safety demonstration project

The Combustion Product Monitor (CPM) instrument is a six-channel tunable laser absorption spectrometer capable of measuring ambient gas-phase concentrations of CO, HCl, HCN, HF, CO2, and O2 in spacecraft environments. Monitoring of these compounds can provide early warning detection of combustion events and can also facilitate safe post-fire cleanup. Here, we will describe the development of a CPM instrument optimized for operation as part of the Spacecraft Fire Safety Demonstration (Saffire) Project. As part of Saffire, the CPM instrument will measure concentrations of the target gases during low-gravity, reduced pressure oxidative pyrolysis of relevant test materials aboard a transfer vehicle returning from low Earth orbit. We will describe the CPM instrument design, absorption line selection,theoretical and experimental detection limits, and environmental testing.

Briggs, Ryan M.↗
NASA NTRS2022

An Adaptation of ISO 11204 using Customized Correction Grades to Mitigate Ambient Noise Effects when Computing Sonic Boom Loudness Levels

A spectral-based correction adapted from ISO 11204 [1] is investigated here to mitigate the effects of ambient noise contamination of sonic booms recorded by noise monitors during field tests. The algorithm from sections 5.4.2 and 7 of ISO 11204 is customized using six nonstandard correction grades in addition to implementing the two standardized grades described in ISO 11204. The six nonstandard grades allow for more aggressive correction of the levels of the sonic boom spectrum when they are proximate to the ambient spectrum. Of the eight correction grades, the most aggressive custom correction grade, termed “Custom F” here, performed best under the conditions that were studied. Consequently, “Custom F” is recommended for use when processing in-field recordings of X-59 sonic booms. To evaluate the eight correction grades, mock X-59 acoustic recordings were generated using predicted ground-level X-59 sonic booms. These ground-level waveforms were created by Doebler [2] by propagating nearfield CFD solutions of the X-59 C612A configuration to the ground using PCBoom [3] (please see Acknowledgements and Refs. [4, 5, 2, 6]). To generate the mock acoustic recordings from those ground-level waveforms, they were further modified using turbulence filters developed during the NASA SonicBAT effort [7], post boom noise audio clips from the NASA SonicBAT tests [7], and ambient noise from the NASA QSF18 test [8, 9]. These mock acoustic recordings enabled evaluation of the ambient noise mitigation methods since the proper loudness levels of the X-59 waveforms in absence of ambient noise are known. Specifically, these known levels provide a benchmark against which the corrected loudness levels are compared, where the corrected loudness levels are computed when ambient noise is present within the waveforms. Importantly, similar analyses using in-field recordings are not possible since the proper loudness levels of the sonic boom waveforms in absence of ambient noise are unknowable when analyzing in-field recordings. Consequently, if additional analyses of ambient noise mitigation methods are needed, then use of mock recordings like those used here is recommended.

Sonic boom↗
DOE OSTI2021

Stem CO2 Efflux measurements from Manaus, Brazil, 2017

This data was collected in order to test the effects of temperatures on the autotrophic respiratory process in the tropics. This data package contains raw real-time stem CO2 efflux files during the night and day from 3 different species near the K34 in Manaus during the day and the night. Raw and derived data files are included in the format of .csv and .xlsx and information about the canopy trees and temperatures recorded can be found in the field event log using microsoft excel. The data was collected from three canopy dominant trees in the central Amazon near the K34 tower. Real-time stem CO2 efflux was determined using a Li7000 gas analyzer configured in differential mode and connected to a dynamic stem chamber secured to the stem at breast height using straps to generate a reasonable seal. Ambient air was continuously pumped into the stem chamber and CO2 concentrations of the air entering and exiting the chamber were continuously monitored. CO2 efflux was calculated based on the CO2 concentration difference between ambient and stem chambers, the flow rate of air through the chamber, and the area of the enclosed stem. Additional auxiliary data, including sap flow and crown temperature were also measured. No data processing or QA/QC was done on the raw data packages.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2026

Formation of Bimetallic Nanoparticles via Exsolution Using a Reducible Metal Oxide Capping Layer

Bimetallic nanoparticles are promising catalysts that can improve performance in heterogeneous catalysis and solid-state electrochemistry. Exsolution is a useful method for forming such nanoparticles; however, it is limited by the elements present within the host oxide lattice. Here, in this work, we develop and demonstrate a strategy to form bimetallic particles from La 0.5 Sr 0.5 Ti 0.94 Ni 0.06 O 3 (LSTN) exsolution and using a reducible SnO 2 capping layer, expanding the range of elements available for bimetallic nanoparticle formation. Using this capping layer strategy, we formed nickel–tin (Ni 0 –Sn 0 ) bimetallic nanoparticles via exsolution. We used in situ near-ambient pressure X-ray photoelectron spectroscopy to monitor surface chemical changes during exsolution, showing that first, SnO 2 volatilized. This SnO 2 loss exposed the perovskite surface of LSTN to reducing conditions, which induced Ni exsolution, and compounded with SnO 2 reduction led to the formation of bimetallic Ni 0 –Sn 0 particles. To evaluate the associated microstructural evolution, we measured grazing incidence small-angle X-ray scattering (GISAXS), which confirmed the loss of the SnO 2 capping layer, and scattering simulations suggested the formation of bimetallic particles. We confirmed the bimetallic nanoparticle composition and morphology by Auger spectroscopy and scanning transmission electron microscopy. The resulting bimetallic nanoparticles were smaller and more thermally stable than the monometallic Ni counterparts on LSTN. This capping layer and exsolution approach allow synthesizing multimetallic nanoparticles and can be applied to other reducible metal oxides and perovskite hosts, broadening the compositional space for advanced catalytic materials.

36 MATERIALS SCIENCE↗
DOE OSTI2021

δ 13 C methane source signatures from tropical wetland and rice field emissions

The atmospheric methane (CH 4 ) burden is rising sharply, but the causes are still not well understood. One factor of uncertainty is the importance of tropical CH 4 emissions into the global mix. Isotopic signatures of major sources remain poorly constrained, despite their usefulness in constraining the global methane budget. Here, a collection of new δ 13 C CH 4 signatures is presented for a range of tropical wetlands and rice fields determined from air samples collected during campaigns from 2016 to 2020. Long-term monitoring of δ 13 C CH 4 in ambient air has been conducted at the Chacaltaya observatory, Bolivia and Southern Botswana. Both long-term records are dominated by biogenic CH 4 sources, with isotopic signatures expected from wetland sources. From the longer-term Bolivian record, a seasonal isotopic shift is observed corresponding to wetland extent suggesting that there is input of relatively isotopically light CH 4 to the atmosphere during periods of reduced wetland extent. This new data expands the geographical extent and range of measurements of tropical wetland and rice δ 13 C CH 4 sources and hints at significant seasonal variation in tropical wetland δ 13 C CH 4 signatures which may be important to capture in future global and regional models.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

Rapidly Deployable Acoustic Monitoring and Localization System Based on a Low-Cost Wave Buoy Platform

The primary objective of this project is to develop a cost-effective, fit-for-purpose environmental monitoring system, “NoiseSpotter®,” that characterizes, classifies, and provides accurate location information for anthropogenic and natural sounds in near real-time. NoiseSpotter was developed to support the evaluation of potential acoustic effects of marine energy (ME) projects. By utilizing a compact array of three acoustic particle motion sensors, NoiseSpotter triangulates individual bearings to provide sound source localization to within 5% accuracy, allowing the ability to discern ME device sounds relative to other confounding sounds in the environment, while providing location estimates to nearby marine mammals for environmental mitigation purposes. The ME industry needs proven solutions to meet environmental impact assessment needs. The NoiseSpotter® includes off-the-shelf, modular components that are easy to assemble and disassemble. Its acoustic particle motion sensors are commercially available and the data logger and real-time telemetry system is designed to be plug-and-play. The entire system is relatively compact and can be deployed from small vessels. NoiseSpotter’s near real-time capability enables operational monitoring of ME sounds, particularly during early stages of technology adoption to facilitate mitigation of potential noise effects. Widespread adoption of the technology for acoustic monitoring of ME devices requires that it be cost effective; hence the anticipated commercial cost of system hardware is $35,000. This project contributes to reducing barriers to ME testing through support of scientific research focused on reducing or mitigating environmental risks and lowering costs and complexity of environmental monitoring. This project has developed an acoustic monitoring system, NoiseSpotter® (U.S. Patent No. 11,156,734 and U.S. Registered Trademark No. 6,442,313), to detect and characterize baseline noise and sounds from ME operations and support geolocation of detected sounds. The intended outcome of the project is to mitigate concerns about the potential for ME device noise to alter marine mammal or fish behavior. NoiseSpotter® enables cost-effective, near real-time acoustic monitoring of an operational ME device relative to ambient environmental noise and provides a technical basis for ME developers seeking to navigate the permitting process in an efficient manner.

16 TIDAL AND WAVE POWER↗
NASA NTRS1999

Microcalorimetric Measurements of Hydrogen Peroxide Stability

Recent interest in propellants with nontoxic reaction products has led to a resurgence of interest in hydrogen peroxide for various propellant applications. Because hydrogen peroxide is sensitive to contaminants and materials interactions, stability and shelf life are issues. A relatively new, ultrasensitive heat measurement technique, isothermal microcalorimetry, is being used at the White Sands Test Facility to monitor the decomposition of hydrogen peroxide at near ambient temperatures. Isothermal microcalorimetry measures the beat flow from a reaction vessel into a surrounding heat sink. In these applications, microcalorimetry is approximately 1,000 times more sensitive than accelerating rate calorimetry or differential scanning calorimetry for measuring thermal events. Experimental procedures have been developed for the microcalorimetric measurement of the ultra-small beat effects caused by incompatible interactions of hydrogen peroxide. The decomposition rates of hydrogen peroxide at the picomole/sec/gram level have been measured showing the effects of stabilizers and peroxide concentration. Typical measurements are carried out at 40 C over a 24-hour period, This paper describes a method for the conversion of the heat flow measurements to chemical reaction rates based on thermochemical considerations. The reaction rates are used in a study of the effects of stabilizer levels on the decomposition of propellant grade hydrogen peroxide.

Davis, Dennis D.↗
DOE OSTI2020

The EGS Collab Project: Learnings from Experiment 1

The primary objective of the EGS Collab Project sponsored by DOE is to increase the understanding needed to efficiently implement enhanced geothermal systems (EGS). One goal of the EGS Collab project is to create a collaborative research environment in which to study stimulation of crystalline rock at the 10 meter scale. Key to this effort is the collection of high quality data to allow comparison to numerical coupled process models in an effort to build confidence in the codes and modeling techniques used. In response to this, the EGS Collab team has created an underground test bed at the Sanford Underground Research Facility (SURF) in Lead SD at a depth of approximately 1.5 km to examine hydraulic fracturing (Experiment 1). We are currently designing a second test bed aimed at investigating shear stimulation (Experiment 2). At the Experiment 1 location, we have characterized our host rock using laboratory testing and numerous field-based geophysical and geological techniques, and created a well-instrumented test bed to allow us to carefully monitor stimulation events and flow tests. In addition to the installed geophysical sensors, we have used tracer tests, differences in the ambient microbial communities at flow collection locations, and cold water injection to inform us about dynamic flow pathways. In Experiment 1, we have hydraulically stimulated the host rock in a number times at several locations in one well, creating new fractures that connect to existing fractures between the injection and production boreholes. We have performed long-term ambient and chilled water injection tests as an analog to EGS, and have monitored system changes resulting from these water injections through geophysical monitoring, flow and pressure measurements, tracer tests, and microbiology. Here, we summarize the tests performed, issues identified including poroelastic and thermoelastic effects, Joule-Thomson effects, restarting effects, indications of flow channeling, and the primary learnings from Experiment 1.

Enhanced Geothermal Systems, EGS Collab, stimulati↗
NASA NTRS2024

Components Refurbishment and Chemical Analysis Facility, Hot Spot 1 Solid Waste Management Unit #041 Year 4 Annual Performance Monitoring Report Kennedy Space Center, Florida

This Year 4 Annual Performance Monitoring Report (PMR) presents the operations, maintenance, and monitoring activities for the Hydraulic Containment System (HCS) Interim Measure (IM) at the Components Refurbishment and Chemical Analysis (CRCA) facility located at John F. Kennedy Space Center (KSC), Florida. The primary objective of the HCS is to attain hydraulic control of the dissolved-phase chlorinated volatile organic compound (CVOC) plume, with the secondary objective to reduce concentrations of CVOCs in the high-concentration plume to support transition to monitored natural attenuation (MNA). CRCA has been designated Solid Waste Management Unit 041 under the KSC Resource Conservation and Recovery Act Corrective Action Program. The timeframe for activities documented in this Year 4 PMR extends from November 2022 through September 2023. Baseline sampling activities were completed in June 2019, and full-scale startup of the HCS IM was completed in July-August 2019. The operational runtime of the HCS for the Year 4 reporting period was approximately 94%, with the majority of downtime attributed to associated groundwater sampling events, maintenance, and Hurricane Nicole. Almost five million gallons of groundwater were treated during Year 4 of HCS operations, and concentrations of the site’s contaminants of concern (trans-1,2-dichloroethene and vinyl chloride) have been reduced by over 99%. This PMR describes the activities that were performed during Year 4 to operate and monitor the HCS IM, which includes three extraction wells, seven injection wells, and conveyance piping to a modular structure containing the control panel and an air stripper. Influent and effluent sampling results from the air stripper show that the system is operating as designed and is reducing concentrations of contaminants of concern to below detection limits. In addition to HCS operation, this PMR also discusses performance monitoring that has been implemented to assess progress of the HCS IM and overall plume conditions through scheduled groundwater (quarterly and semi-annual) and sub-slab soil gas (quarterly) sampling and analysis. Two ambient air samples were also collected on a quarterly basis in the vicinity of the modular structure and the paved driveway east of the Solvent Reclamation Area during routine operation and maintenance (O&M) activities to ensure safe breathing zone air quality for on-site personnel. All sub-slab soil gas and ambient air sampling conducted during the Year 4 operational period showed results below applicable regulatory air screening limits. Predictions made during the Year 2 groundwater model updates were in close correlation to post Year 4 plume conditions. A supplemental DPT study conducted in 2022 and 2023. This study indicated that low-concentration plume conditions, where concentrations exceed State of Florida Groundwater Cleanup Target Levels, expanded westward to Kennedy Parkway North and northward to the vicinity of the railroad tracks. Based on these results, recommendations were made to install 14 wells to monitor the downgradient and boundary conditions of the expanded LCP. The contents of this Year 4 PMR were presented during the November 2023 KSC Remediation Team meeting, where Team consensus was reached on several items including continued O&M of the HCS, and continued monitoring of groundwater, ambient air, and sub-slab soil gas. Sampling for per- and polyfluoroalkyl substances at CRCA is ongoing and will be submitted under separate cover.

K. Alex Murphy↗
NASA NTRS2023

Components Refurbishment and Chemical Analysis Facility, Hot Spot 1 SWMU #041 Year 3 Annual Performance Monitoring Report Kennedy Space Center, Florida

This Year 3 Annual Performance Monitoring Report (PMR) presents the operations, maintenance, and monitoring activities for the Hydraulic Containment System (HCS) Interim Measure (IM) at the Components Refurbishment and Chemical Analysis (CRCA) facility located at John F. Kennedy Space Center (KSC), Florida. The primary objective of the HCS is to attain hydraulic control of the dissolved-phase chlorinated volatile organic compound (CVOC) plume, with the secondary objective to reduce concentrations of CVOCs in the high-concentration plume to support transition to monitored natural attenuation (MNA). CRCA has been designated Solid Waste Management Unit 041 under the KSC Resource Conservation and Recovery Act Corrective Action Program. The timeframe for activities documented in this Year 3 PMR extends from September 2021 through October 2022. Baseline sampling activities were completed in June 2019, and full-scale startup of the HCS IM was completed in July-August 2019. The operational runtime of the HCS for the Year 3 reporting period was approximately 91%, with the majority of downtime attributed to system maintenance and repair. This is generally consistent with Year 1 and Year 2 runtimes of 85% and 92%, respectively. To help reduce downtime, an anti-scaling amendment, Redux 390, has been used to reduce scaling and help maintain system design parameters. Over nine million gallons of groundwater were treated during Year 3 of HCS operations, and concentrations of the site’s contaminants of concern (trans-1,2-dichloroethene and vinyl chloride) have been reduced by over 97%. This PMR describes the activities that were performed during Year 3 to operate and monitor the HCS IM, which includes three extraction wells, seven injection wells, and conveyance piping to a modular structure containing the control panel and an air stripper. Influent and effluent sampling results from the air stripper show that the system is operating as designed and is reducing concentrations of contaminants of concern to below detection limits. In addition to HCS operation, this PMR also discusses performance monitoring that has been implemented to assess progress of the HCS IM and overall plume conditions through scheduled groundwater (quarterly and semi-annual) and sub-slab soil gas (quarterly) sampling and analysis. Two ambient air samples were also collected on a quarterly basis in the vicinity of the modular structure and the paved driveway east of the Solvent Reclamation Area during routine operation and maintenance (O&M) activities to ensure safe breathing zone air quality for on-site personnel. All sub-slab soil gas and ambient air sampling conducted during the Year 3 operational period showed results below applicable regulatory air screening limits. Predictions made during the Year 2 groundwater model updates were in close correlation to post Year 3 plume conditions. Therefore, it can be assumed that the projected path remains valid for transition to MNA in one to two years of continuous HCS operation. The contents of this Year 3 PMR were presented during the February 2023 KSC Remediation Team meeting, where Team consensus was reached on several items including continued O&M of the HCS, and continued monitoring of groundwater, ambient air, and sub-slab soil gas. Replacement of MW0019 and VMP04 was also recommended, as well as additional direct-push technology sampling to further delineate the downgradient plume and confirm overall site-wide low-concentration plume boundaries. Sampling for per- and polyfluoroalkyl substances at CRCA is ongoing and will be submitted under separate cover.

K. Alex Murphy↗
DOE OSTI2024

Ambient energy for buildings: Beyond energy efficiency

The following Key Messages comprise the salient findings of this study: 1. Ambient energy (from sun, air, ground, and sky) can heat and cool buildings; provide hot water, ventilation and daylighting; dry clothes; and cook food. These services account for about three-quarters of building energy consumption and a third of total US demand. Biophilic design (direct and indirect connections with nature) is an intrinsic adjunct to ambient energy systems, and improves wellness and human performance. 2. The current strategy of electrification and energy efficiency for buildings will not meet our climate goals, because the transition to an all-renewable electric grid is too slow. Widespread adoption of ambient energy is needed. Solar-heated buildings also flatten the seasonal demand for electricity compared to all-electric buildings, reducing required production capacity and long-term energy storage. In addition, ambient-conditioned buildings improve resilience by remaining livable during power outages. 3. National policies, incentives, and marketing should be enacted to promote ambient energy use. Federal administrative priorities should reflect the importance of ambient energy for buildings. Use of ambient energy should be encouraged through existing and new building codes and standards. 4. Ambient energy system design tools are needed for architects, engineers, builders, building scientists, realtors, appraisers, and consumers. PVWatts is used over 100 million times per year for photovoltaic system design. A similar, simple, and accessible tool for ambient design is crucial. 5. Training on ambient energy is needed throughout secondary, post-secondary, and continuing education for workforce development. Currently, only about 10% of colleges teach courses on passive heating and cooling systems. 6. Ambient-conditioned buildings should be demonstrated in all US climate zones. Performance should be monitored and reported, with quantitative case studies made widely available. 7. While current technology is sufficient to build high-performance ambient buildings now, research is needed to develop new technologies to harness ambient energy more effectively and more economically. Such advancements will facilitate adoption of ambient energy technologies in a wider range of buildings, including retrofits. Examples include windows with much lower thermal losses, use of the building shell as thermal storage, alternative light-weight thermal storage systems, sky radiation cooling systems, automated controls for solar gains and passive cooling, and ground coupling.

14 SOLAR ENERGY↗
NASA NTRS2010

Developing NDE Techniques for Large Cryogenic Tanks - Year 2 Report

The Shuttle Program requires very large cryogenic ground storage tanks in which to store liquid oxygen and hydrogen. The existing Launch Complex-39 Pad tanks, which will be passed onto future launch programs, are over 40 years old and have received minimal refurbishment and only external inspections over the years. The majority of the structure is inaccessible without a full system drain of cryogenic liquid and insulation in the annular region. It was previously thought that there was a limit to the number of temperature cycles that the tanks could handle due to possible insulation compaction before undergoing a costly and time consuming complete overhaul; therefore the tanks were not drained and performance issues with these tanks, specifically the Pad B LH2 tank, were accepted. There is a need and an opportunity, as the Shuttle program ends and work to upgrade the launch pad progresses, to develop innovative non-destructive evaluation (NDE) techniques to analyze the current tanks. Techniques are desired that can aid in determining the extent of refurbishment required to keep the tanks in service for another 20+ years. A non-destructive technique would also be a significant aid in acceptance testing of new and refurbished tanks, saving significant time and money, if corrective actions can be taken before cryogen is introduced to the systems. Year one of this project concentrated on analysis of the current tanks located at LC-39 while cryogen was present. Year two of this project concentrated on analysis of detectable thermal variations on the outer surface of the tanks as the cryogen was drained and the inner vessel warmed to ambient conditions. Two techniques have been deployed in the field to monitor the tank. The first consisted of a displacement sensor to monitor for any expansions at the base of the tank during warm-up that could indicate a compaction issue with the insulation. The second technique was continued thermal monitoring of the tank through and after warm up. The indications noted in the thermal images were compared to bore-scope images of the annular region taken once the tank was inert and warmed to ambient conditions. Similar thermal imaging was performed on a smaller tank where an insulation void was induced to compare the effectiveness of thermal imagining on a different tank geometry.

Arens, Ellen↗
DOE OSTI2022

In Situ Monitoring of H 2 -Induced Nonstoichiometry in Cu 2 O

Nonstoichiometry plays a pivotal role in the functioning of oxide materials, but it is challenging to measure the non-stoichiometric formation and the resulting charge redistribution around the point defects. Using ambient-pressure X-ray photoelectron spectroscopy and Auger electron spectroscopy to monitor the reduction of Cu 2 O in H 2 , we identify the formation of an intermediate, oxygen-deficient Cu 2 O phase and its progressive inward growth into the deeper region of the oxide. Complemented by DFT modeling, we show that the oxygen-deficient Cu 2 O formation occurs via molecular H 2 adsorption at the Cu 2 O surface, which results in the loss of lattice O from the formation of H 2 O molecules that desorb spontaneously from the oxide surface. The resulting oxy-gen-deficient Cu 2 O is a stable intermediate that persists before the Cu 2 O is fully reduced to metallic Cu. The O vacancy induced charge redistribution of the coordinating Cu atoms results in a satellite feature in Cu LMM, which can be used a fingerprint to identify the nonstoichiometry and local charge transfer in non-stoichiometric oxides.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Interaction of molecular nitrogen with vanadium oxide in the absence and presence of water vapor at room temperature: Near-ambient pressure XPS

Interactions of N2 at oxide surfaces are important for understanding electrocatalytic nitrogen reduction reaction (NRR) mechanisms. Interactions of N2 at the polycrystalline vanadium oxide/vapor interface were monitored at room temperature and total pressures up to 10−1 Torr using Near-Ambient Pressure X-ray Photoelectron Spectroscopy (NAP-XPS). The oxide film was predominantly V(IV), with V(III) and V(V) components. XPS spectra were acquired in environments of both pure N2 and equal pressures of N2 and H2O vapor. In pure N2, broad, partially resolved N1s features were observed at binding energies of 401.0 and 398.7 eV, with a relative intensity of ∼3:1, respectively. These features remained upon subsequent pumpdown to 10−9 Torr. The observed maximum N surface coverage was ∼1.5 × 1013 cm−2—a fraction of a monolayer. In the presence of equal pressures of H2O, the adsorbed N intensity at 10−1 Torr is ∼25% of that observed in the absence of H2O. The formation of molecularly adsorbed H2O was also observed. Density functional theory-based calculations suggest favorable absorption energies for N2 bonding to both V(IV) and V(III) cation sites but less so for V(V) sites. Hartree–Fock-based cluster calculations for N2–V end-on adsorption show that experimental XPS doublet features are consistent with the calculated shake-up and normal, final ionic configurations for N2 end-on bonding to V(III) sites but not V(IV) sites. The XPS spectra of vanadium oxide transferred in situ between electrochemical and UHV environments indicate that the oxide surfaces studied here are stable upon exposure to the electrolyte under NRR-relevant conditions.

Balogun, K.↗