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DOE OSTI2021

In Situ ATR-FTIR Study of the Cathode–Electrolyte Interphase: Electrolyte Solution Structure, Transition Metal Redox, and Surface Layer Evolution

We present a study of the lithium nickel manganese cobalt oxide (LiNi 0.6 Mn 0.2 Co 0.2 O 2 , NMC622) cathode-electrolyte interphase (CEI) during galvanostatic charging and discharging using in situ attenuated total reflectance Fourier transform infrared (ATR-FTIR) methods to investigate the voltage dependent electrolyte solution structure changes at the interface, transition metal (TM) redox chemistry, and cathode/electrolyte interfacial layer evolution. Furthermore, our in situ cell design provides both reliable electrochemical device testing and strong FTIR vibrational absorption signals near the cathode surface. Specifically, advanced spectral analysis elucidates changes of near-surface Li+ ion (de)solvation by solvent molecules during galvanostatic cycling. Moreover, cathode metal-oxygen vibrational absorptions, sensitive to TM redox behaviors and subsequent local structural variations, were correlated to cathode de-lithiation (and lithiation) and electrolyte solution structure changes. In addition, we have detected the formation and evolution of a CEI surface layer on the NMC622 cathode that contributes to the cell's capacity fade.

25 ENERGY STORAGE↗

NASA NTRS1990

Mars in situ propellants: Carbon monoxide and oxygen ignition experiments

Carbon monoxide and oxygen were tested in a standard spark-torch igniter to identify the ignition characteristics of this potential Mars in situ propellant combination. The ignition profiles were determined as functions of mixture ratio, amount of hydrogen added to the carbon monoxide, and oxygen inlet temperature. The experiments indicated that the carbon monoxide and oxygen combination must have small amounts of hydrogen present to initiate reaction. Once the reaction was started, the combustion continued without the presence of hydrogen. A mixture ratio range was identified where ignition occurred, and this range varied with the oxygen inlet temperature.

Linne, Diane L.↗

NASA NTRS1990

Mars in situ propellants - Carbon monoxide and oxygen ignition experiments

Linne, Diane L.↗

NASA NTRS2003

Model-Data Assimilation of Internal Waves during ASIAEX-2001

In recent Asian Seas International Acoustics Experiment (ASIAEX), extensive moorings have been deployed around the continental shelf break area in the northeast of South China Sea in May 2001. Simultaneous RADARSAT SAR images have been collected during the field test to integrate with the in-situ measurements from moorings, ship-board sensors, and CTD casts. Besides it provides synoptic information, satellite imagery is very useful for tracking the internal waves, and locating surface fronts and mesoscale features. During ASIAEX in May 2001, many large internal waves were observed at the test area and were the major oceanic features for acoustic volume interaction. Based on the internal wave distribution maps compiled from satellite data, the wave crest can be as long as 200 km with amplitude of 100 m. Environmental parameters have been calculated based on extensive CTD casts data near the ASIAEX area. Nonlinear internal wave models have been applied to integrate and assimilate both SAR and mooring data. Using SAR data in deep water as an initial condition, numerical simulations produce the wave evolution on the continental shelf and compared reasonably well with the mooring measurements at the downstream station. The shoaling, turning, and dissipation of large internal waves on the shelf break, elevation solitons, and wave-wave interaction have been studied and are very important issues for acoustic propagation. The internal wave effects on acoustic modal coupling has been implicated and discussed.

Liu, Antony↗

DOE OSTI2025

Demonstration of the surveillance test article for an advanced reactor surveillance test program

Operational environments in generation IV reactors involve corrosive and irradiative conditions at elevated temperatures. Typical reactor operations consist of transients which impose cyclic loads on reactor components. These cyclic loads, combined with corrosive and irradiative environments, result in synergistic degradation of component materials. However, limited data exists on the coupled damage effects on materials for reactor environments. While the surrogate material surveillance concept has been used in light water reactors to assess irradiation damage, existing material surveillance technologies are not suitable for in-situ monitoring of coupled material degradation. The materials surveillance program focuses on material degradation management and the estimation of remaining life of reactor components through surveillance test articles. This paper presents the design and analysis methodology of a bi-metal surveillance test article, which uses difference in thermal expansion coefficient between two metals to induce in-situ cyclic loads. This report presents the work conducted in FY 25, to test the surveillance test article in air and salt environments. These test specimens were evaluated after thermal cycle exposure and remaining life is measured through creep test.

36 - MATERIALS SCIENCE↗

NASA NTRS1991

Lunar regolith densification

Core tube samples of the lunar regolith obtained during the Apollo missions showed a rapid increase in the density of the regolith with depth. Various hypotheses have been proposed for the possible cause of this phenomenon, including the densification of the loose regolith material by repeated shaking from the seismic tremors which have been found to occur at regular monthly intervals when the moon and earth are closest to one another. A test bed was designed to study regolith densification. This test bed uses Minnesota Lunar Simulant (MLS) to conduct shaking experiments in the geotechnical centrifuge with an inflight shake table system. By reproducing realistic in-situ regolith properties, the experiment also serves to test penetrator concepts. The shake table system was designed and used for simulation experiments to study effects of earthquakes on terrestrial soil structures. It is mounted on a 15 g-ton geotechnical centrifuge in which the self-weight induced stresses are replicated by testing an n-th scale model in a gravity field which is n times larger than Earth's gravity. A similar concept applies when dealing with lunar prototypes, where the gravity ratio required for proper simulation of lunar gravity effects is that between the centrifugal acceleration and the lunar gravity. Records of lunar seismic tremors, or moonquakes, were obtained. While these records are being prepared for use as the input data to drive the shake table system, records from the El Centro earthquake of 1940 are being used to perform preliminary tests, using a soil container which was previously used for earthquake studies. This container has a laminar construction, with the layers free to slide on each other, so that the soil motion during the simulated earthquake will not be constrained by the otherwise rigid boundaries. The soil model is prepared by pluviating the MLS from a hopper into the laminar container to a depth of 6 in. The container is mounted on the shake table and the centrifuge is operated to generate an acceleration of 10 times Earth's gravity or 60 times the lunar gravity, thus simulating a lunar regolith thickness of 30 ft. The shake table is then operated using the scaled 'moonquake' as the input motion. One or more model moonquakes are used in each experiment, after which the soil is analyzed for its density profile with depth. This is accomplished by removing from the soil bed a column of soil contained within a thin rubber sleeve which has been previously embedded vertically in the soil during pluviation. This column of soil is transferred to a gamma ray device, in which the gamma ray transmission transversely through the soil is measured and compared with standard calibration samples. In this manner, the density profile can be determined. Preliminary results to date are encouraging, and the Center plans to study the effects of duration of shaking, intensity of the shaking motion, and the frequency of the motion.

Ko, Hon-Yim↗

DOE OSTI2025

Design Report on the MiniFuel Instrumented Test Apparatus for Understanding Radiation Effects

Most nuclear fuels irradiations at Oak Ridge National Laboratory (ORNL) over the past decade have been conducted using MiniFuel—a static capsule design employing subscale fuel specimens to collect separate-effects irradiated fuel performance data. Irradiation conditions for MiniFuel experiments are predicted pre-test using reactor physics, and thermal models are verified post-irradiation via SiC dilatometry and various spectrometry methods. Relevant fuel performance parameters are also observed post-irradiation in a hot cell, thereby providing a single data point for each parameter representing the cumulative effects of the irradiation conditions. Substantially more data can be harvested from a single test and within a shorter duration by instrumenting irradiation vehicles and measuring desired quantities in situ. This report presents the design and analysis of the MiniFuel INstrumented Irradiation Test Apparatus for Understanding Radiation Effects (MINITAURE)—an instrumented test rig based on the separate-effects MiniFuel concept that aims to capture fission gas release (FGR) and thermal conductivity degradation of fuel specimens during irradiation in the High Flux Isotope Reactor (HFIR). MINITAURE will be integrated with the Materials Irradiation Facility (MIF) located in the HFIR building outside the reactor containment. The MIF will act as the instrumentation and control center for the experiment, enabling real-time feedback from in situ sensors and control of irradiation temperatures via a gas delivery system. Two unique capsule designs were developed to capture each phenomenon: the thermal conductivity capsule, which uses a thermopile method to estimate fuel specimen thermal conductivity, and the fission gas release capsule, which will have continuous flowing gas communication to high-purity germanium detectors that are housed in the MIF for monitoring FGR. This report details the reactor physics and heat transfer modeling activities that were used to inform the experiment design and predict capsule performance. It also describes out-of-pile activities conducted to stand up this new capability and verify the measurement techniques. Modeling efforts to date have demonstrated the feasibility of the in situ measurement techniques and supported the development of the MINITAURE assembly configuration. Out-of-pile testing of the thermal conductivity measurement shows promise in capturing relative changes in thermal conductivity. However, significant errors exist in the measured absolute value, posing a need for further refinement.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Development and Implementation of Digital Image Correlation for Out-of-Cell Burst Testing

This report details the progress made towards utilizing in-situ methods to observe and quantify unirradiated Zircaloy-4 (Zr4) fuel cladding deformation during out-of-cell design basis accident conditions, specifically during loss-of-coolant accident (LOCA) burst testing in the Severe Accident Test Station at Oak Ridge National Laboratory. Digital image correlation (DIC) was implemented to calculate cladding strain during burst and infrared (IR) thermography was used to attempt a correlation of strain with temperature and to investigate thermal gradients. For both techniques, early experimentation revealed experimental modifications were necessary for implementation. For DIC, this manifested as shortened cladding lengths which could be centered in front of the viewing chamber bored through the IR furnace side, and for IR thermography this meant conducting burst tests in air without a reaction tube and the incorporation of a SiC shell to eliminate direct IR reflections from the tungsten lamps. In the following, the technical issues and subsequent origin of these modifications are discussed, laying the framework for a proof-of-concept DIC/IR characterization of a burst test in the final section.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1980

In situ ozone data for evaluation of the laser absorption spectrometer ozone remote sensor: 1979 southeastern Virginia urban plume study summer field program

Ozone data from the 1979 Southeastern Virginia Urban Study (SEV-UPS) field program are presented. The SEV-UPS was conducted for evaluation of an ozone remote sensor, the Laser Absorption Spectrometer. During the measurement program, remote-sensor evaluation was in two areas; (1) determination of the remote sensor's accuracy, repeatability, and operational characteristics, and (2) demonstration of the application of remotely sensed ozone data in air-quality studies. Data from six experiments designed to provide in situ ozone data for evaluation of the sensor in area 1, above, are presented. Experiments consisted of overflights of a test area with the remote sensor aircraft while in situ measurements with a second aircraft and selected surface stations provided correlative ozone data within the viewing area of the remote sensor.

Gregory, G. L.↗

NASA NTRS2019

Bionutrients-1, On-Demand Production of Nutrients in Space

Future long-duration missions face significant challenges maintaining crew health. A critical area is supplying adequate nutrition, as certain vitamins and nutrients in supplied foods and supplements demonstrate substantial degradation during extended storage. To address this issue, we are developing and flight-testing a platform technology that demonstrates in situ microbial production of targeted nutrients over extended mission durations. This 5-year experiment, known as BioNutrients-1, was started on the International Space Station in May 2019. It involves two components: an on-orbit hydration and production experiment; and the development of space-compatible, key bio-manufacturing microorganisms. On-orbit testing utilizes a small “production pack” system that encloses sterile edible growth substrate and desiccated Saccharomyces cerevisiae strains genetically engineered to produce the nutrients beta-carotene or zeaxanthin. On hydration and mixing of the production pack, the organisms revive and grow until limited by the depletion of growth media, hypothetically leading to consistent amounts of biomass and nutrients. In eventual mission applications, the packet contents would be heat treated to inactivate the microorganisms prior to consumption. For these flight experiments, the packet will not be heat treated, but will instead be frozen for return to Earth for analyses. In addition to the production pack trials, 14 different microorganisms/treatments were also delivered to ISS for long-duration storage. These samples will be intermittently returned to Earth and analyzed to determine survival rates and genomics. For this presentation, initial data from returned samples and ground controls will be discussed.

Hindupur, Aditya↗

NASA NTRS2019

BioNutrients-1: On-Demand Production of Nutrients in Space

Future long-duration missions face significant challenges maintaining crew health. A critical area is supplying adequate nutrition, as certain vitamins and nutrients in supplied foods and supplements demonstrate substantial degradation during extended storage. To address this issue, we are developing and flight-testing a platform technology that demonstrates in situ microbial production of targeted nutrients over extended mission durations. This 5-year experiment, known as BioNutrients-1, was started on the International Space Station in May 2019. It involves two components: an on-orbit hydration and production experiment; and the development of space-compatible, key bio-manufacturing microorganisms. On-orbit testing utilizes a small "production pack" system that encloses sterile edible growth substrate and desiccated Saccharomyces cerevisiae strains genetically engineered to produce the nutrients beta-carotene or zeaxanthin. On hydration and mixing of the production pack, the organisms revive and grow until limited by the depletion of growth media, hypothetically leading to consistent amounts of biomass and nutrients. In eventual mission applications, the packet contents would be heat treated to inactivate the microorganisms prior to consumption. For these flight experiments, the packet will not be heat treated, but will instead be frozen for return to Earth for analyses. In addition to the production pack trials, 14 different microorganisms/treatments were also delivered to ISS for long-duration storage. These samples will be intermittently returned to Earth and analyzed to determine survival rates and genomics. For this presentation, initial data from returned samples and ground controls will be discussed.

Hindupur, Aditya↗

DOE OSTI2022

Ductile failure and damage localization in Al6061-T6 characterized by in situ X-ray computed tomography and neural network segmentation

Damage initiation and localization in uniaxial tension tests of an Al6061-T6 alloy are evaluated and quantified using in situ X-ray computed tomography and a neural network segmentation strategy. This segmentation strategy offers significant advantages over traditional thresholding in quantifying microstructural and damage evolution metrics. Void nucleation was observed to occur throughout the deformation process, whereas void volume did not grow significantly until later stages of deformation. Localized analysis determined that void nucleation begins in and around the necked region during the early stages of deformation, whereas limited damage nucleation occurs outside of the neck until late stages of deformation. Lastly, inhomogeneities in void and particle spacing in the initial undeformed state of the material are observed to correlate well with the location of damage localization and necking during deformation. These results provide new insights into the ductile failure of Al alloys and how preexisting defects influence damage and rupture.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Hardening in Au-Ag nanoboxes from stacking fault-dislocation interactions

Porous, nano-architected metals with dimensions down to ~10 nm are predicted to have extraordinarily high strength and stiffness per weight, but have been challenging to fabricate and test experimentally. Here, we use colloidal synthesis to make ~140 nm length and ~15 nm wall thickness hollow Au-Ag nanoboxes with smooth and rough surfaces. In situ scanning electron microscope and transmission electron microscope testing of the smooth and rough nanoboxes show them to yield at 130 ± 45 MPa and 96 ± 31 MPa respectively, with significant strain hardening. A higher strain hardening rate is seen in rough nanoboxes than smooth nanoboxes. Finite element modeling is used to show that the structure of the nanoboxes is not responsible for the hardening behavior suggesting that material mechanisms are the source of observed hardening. Molecular dynamics simulations indicate that hardening is a result of interactions between dislocations and the associated increase in dislocation density.

42 ENGINEERING↗

NASA NTRS2012

Miniature Variable Pressure Scanning Electron Microscope for In-Situ Imaging and Chemical Analysis

NASA Marshall Space Flight Center (MSFC) is leading an effort to develop a Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) for in-situ imaging and chemical analysis of uncoated samples. This instrument development will be geared towards operation on Mars and builds on a previous MSFC design of a mini-SEM for the moon (funded through the NASA Planetary Instrument Definition and Development Program). Because Mars has a dramatically different environment than the moon, modifications to the MSFC lunar mini-SEM are necessary. Mainly, the higher atmospheric pressure calls for the use of an electron gun that can operate at High Vacuum, rather than Ultra-High Vacuum. The presence of a CO2-rich atmosphere also allows for the incorporation of a variable pressure system that enables the in-situ analysis of nonconductive geological specimens. Preliminary testing of Mars meteorites in a commercial Environmental SEM(Tradmark) (FEI) confirms the usefulness of lowcurrent/low-accelerating voltage imaging and highlights the advantages of using the Mars atmosphere for environmental imaging. The unique capabilities of the MVP-SEM make it an ideal tool for pursuing key scientific goals of NASA's Flagship Mission Max-C; to perform in-situ science and collect and cache samples in preparation for sample return from Mars.

Gaskin, Jessica A.↗

DOE OSTI2021

In situ TEM measurement of electrical properties of individual BaTiO 3 nanocubes

We report on the measurement of the electrical properties of individual pristine and doped BaTiO 3 nanocubes by using in situ transmission electron microscopy with a two-electrode configuration. The dimensions of the nanocubes tested are between 10 and 20 nm, which rendered their in situ electrical characterization challenging. We characterized 4%Cr and 5%La (atomic percentage) doped BaTiO 3 nanocubes and compared them with the properties of pristine BaTiO3 nanocubes synthesized by the same solvothermal method. We found that the resistance of all three types of nanocubes when displayed in log-scale shows a nearly linear dependence on the applied electric field (R2 ≥ 0.95) over a wide range of electric fields (50–900 kV/cm). Compared with pristine BaTiO 3 nanocubes, the resistance of both 4%Cr and 5%La doped nanocubes showed reduced variation rates with respect to the electric field, with 5%La doping, demonstrating a better reduction in the variation rate. By developing techniques capable of evaluating the properties of individual BaTiO 3 nanocubes, we expect that our work to open the door to the use of BaTiO 3 nanomaterials in the design of future multilayer ceramic capacitors with improved volumetric efficiency and ferroelectrics-enabled nanodevices with advanced functionality.

36 MATERIALS SCIENCE↗

NASA NTRS2013

Damage Detection Response Characteristics of Open Circuit Resonant (SansEC) Sensors

The capability to assess the current or future state of the health of an aircraft to improve safety, availability, and reliability while reducing maintenance costs has been a continuous goal for decades. Many companies, commercial entities, and academic institutions have become interested in Integrated Vehicle Health Management (IVHM) and a growing effort of research into "smart" vehicle sensing systems has emerged. Methods to detect damage to aircraft materials and structures have historically relied on visual inspection during pre-flight or post-flight operations by flight and ground crews. More quantitative non-destructive investigations with various instruments and sensors have traditionally been performed when the aircraft is out of operational service during major scheduled maintenance. Through the use of reliable sensors coupled with data monitoring, data mining, and data analysis techniques, the health state of a vehicle can be detected in-situ. NASA Langley Research Center (LaRC) is developing a composite aircraft skin damage detection method and system based on open circuit SansEC (Sans Electric Connection) sensor technology. Composite materials are increasingly used in modern aircraft for reducing weight, improving fuel efficiency, and enhancing the overall design, performance, and manufacturability of airborne vehicles. Materials such as fiberglass reinforced composites (FRC) and carbon-fiber-reinforced polymers (CFRP) are being used to great advantage in airframes, wings, engine nacelles, turbine blades, fairings, fuselage structures, empennage structures, control surfaces and aircraft skins. SansEC sensor technology is a new technical framework for designing, powering, and interrogating sensors to detect various types of damage in composite materials. The source cause of the in-service damage (lightning strike, impact damage, material fatigue, etc.) to the aircraft composite is not relevant. The sensor will detect damage independent of the cause. Damage in composite material is generally associated with a localized change in material permittivity and/or conductivity. These changes are sensed using SansEC. The unique electrical signatures (amplitude, frequency, bandwidth, and phase) are used for damage detection and diagnosis. An operational system and method would incorporate a SansEC sensor array on select areas of the aircraft exterior surfaces to form a "Smart skin" sensing surface. In this paper a new method and system for aircraft in-situ damage detection and diagnosis is presented. Experimental test results on seeded fault damage coupons and computational modeling simulation results are presented. NASA LaRC has demonstrated with individual sensors that SansEC sensors can be effectively used for in-situ composite damage detection of delamination, voids, fractures, and rips. Keywords: Damage Detection, Composites, Integrated Vehicle Health Monitoring (IVHM), Aviation Safety, SansEC Sensors

Dudley, Kenneth L.↗

NASA NTRS2023

Transient Liquefaction on the Lunar or Martian Surface Operational Demonstration

The Cryogenic Fluid In-situ Liquefaction for Landers (CryoFILL) activity has been investigating concepts for the liquefaction of cryogenic fluids produced on the surface of the Moon and Mars. Liquefaction testing of oxygen in a scaled lander tank using an integrated, industrial cryocooler system was completed. The testing covered the determination of the nominal performance operation of the system, constant liquefaction performance, and transient liquefaction performance. The goal of the testing was to demonstrate cryogenic liquefaction operational capabilities on the Lunar and Martian surfaces for landers and In Situ Resource Utilization. The testing met all key performance parameter threshold values including liquefaction rate (demonstrated 1.6 kg/hr compared to threshold of 1.1 kg/hr), number of variables as transient (goal of 3: liquefaction flow, environmental temperature, and cryocooler input power – all demonstrated), and number of fill levels (goal of 3: < 5%, 50%, and 90% - all demonstrated). Key testing results from oxygen liquefaction testing will be discussed including sensitivities provided by the analysis team.

Liquefaction↗

NASA NTRS2002

Nonlinear Internal Waves in the South China Sea During ASIAEX

Internal wave distribution maps have been compiled from more than one hundred ERS-1/2, RADARSAT and Space Shuttle SAR images in the South China Sea (SCS) from 1993 to 2000. Based on these distribution maps, most of internal waves in the northeast part of SCS were propagating westward. The wave crest can be as long as 200 km with amplitude of 100 m, due to strong current from the Kuroshio branching out into the SCS. In recent Asian Seas International Acoustics Experiment (ASIAEX), moorings have been deployed in April 2000 and May 2001. Simultaneous RADARSAT ScanSAR images have been collected during the field test to integrate with the model and the in-situ measurements in the SCS. During ASIAEX in May 2001, many large internal waves were observed at the test area and were the major features for acoustic volume interaction. The environmental parameters have been calculated based on extensive CTD castings and mooring data. Nonlinear internal wave models have been applied to simulate the wave evolution on the continental shelf and the results compare reasonably with mooring measurements. The evolution and dissipation of huge internal waves on the shelf break, mode-two waves, elevation waves, and wave-wave interaction are very important issues for acoustic propagation. The implication of internal wave effects on acoustic propagation will also be discussed.

ACOUSTIC PROPAGATION↗