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At least 451 records · Page 25

All sources NASA NTRS DOE OSTI

DOE OSTI2024

Open-source electrochemical cell for in situ X-ray absorption spectroscopy in transmission and fluorescence modes

X-ray spectroscopy is a valuable technique for the study of many materials systems. Characterizing reactions in situ and operando can reveal complex reaction kinetics, which is crucial to understanding active site composition and reaction mechanisms. In this project, the design, fabrication and testing of an open-source and easy-to-fabricate electrochemical cell for in situ electrochemistry compatible with X-ray absorption spectroscopy in both transmission and fluorescence modes are accomplished via windows with large opening angles on both the upstream and downstream sides of the cell. Using a hobbyist computer numerical control machine and free 3D CAD software, anyone can make a reliable electrochemical cell using this design. Onion-like carbon nanoparticles, with a 1:3 iron-to-cobalt ratio, were drop-coated onto carbon paper for testing in situ X-ray absorption spectroscopy. Cyclic voltammetry of the carbon paper showed the expected behavior, with no increased ohmic drop, even in sandwiched cells. Chronoamperometry was used to apply 0.4 V versus reversible hydrogen electrode, with and without 15 min of oxygen purging to ensure that the electrochemical cell does not provide any artefacts due to gas purging. The XANES and EXAFS spectra showed no differences with and without oxygen, as expected at 0.4 V, without any artefacts due to gas purging. The development of this open-source electrochemical cell design allows for improved collection of in situ X-ray absorption spectroscopy data and enables researchers to perform both transmission and fluorescence simultaneously. It additionally addresses key practical considerations including gas purging, reduced ionic resistance and leak prevention.

08 HYDROGEN↗

DOE OSTI2023

A novel in-situ Raman spectroscopic cell for aqueous geochemistry at the solid–liquid interface

In-situ Raman spectroscopy has the potential to be a powerful technique for monitoring geochemical reactions at a solid–liquid interface in real time. In this article, we present the development and testing of an in-situ Raman spectroscopic cell, which can be used for reaction systems at moderate temperatures and pressure [<1000 psi (6.89 MPa), <100 °C, relevant to subsurface geologic systems] and can hold samples large enough for chemical mapping of heterogeneous rock surfaces. The system is validated by measuring the temperature-dependent conversion of gypsum to calcite over time. Near total conversion of gypsum to calcite on the mineral surface took 29 hours at room temperature and 150 minutes at 100 °C, corresponding to an 11.6-fold increase in the conversion rate. Further, we anticipate that this cell can be an important tool in quantifying the rates of carbon mineralization relevant to geologic carbon sequestration, particularly for the elevated rates recently observed in mafic/ultramafic rocks.

47 OTHER INSTRUMENTATION↗

NASA NTRS1979

Simulated EVA operation of a remote connector assembly test report

The features of a connector concept with respect to timelines and ease of connection by EVA (extravehicular activity), in various mating orientations were evaluated. The connector tests were conducted by thee EVA astronaut test subjects. Each of four test conditions (baseline, off angle, overhead, and with visual obstruction) were run three times by each of the test subjects. Time data were taken on each test run. Visual and voice communications with the subjects were recorded. The tests demonstrated that EVA personnel can perform connection tasks in relatively short times (generally one minute) and the connector configuration was a reasonable design base for such tasks. The in-situ communications and post-test comments indicated that the connector was generally acceptable but requires improvement to its manual interface features.

Lefever, A.↗

DOE OSTI2023

In situ chamber for studying battery failure using high-speed synchrotron radiography

The investigation of lithium-ion battery failures is a major challenge for personnel and equipment due to the associated hazards (thermal reaction, toxic gases and explosions). To perform such experiments safely, a battery abuse-test chamber has been developed and installed at the microtomography beamline ID19 of the European Synchrotron Radiation Facility (ESRF). The chamber provides the capability to robustly perform in situ abuse tests through the heat-resistant and gas-tight design for flexible battery geometries and configurations, including single-cell and multi-cell assemblies. High-speed X-ray imaging can be complemented by supplementary equipment, including additional probes (voltage, pressure and temperature) and thermal imaging. Together with the test chamber, a synchronization graphical user interface was developed, which allows an initial interpretation by time-synchronous visualization of the acquired data. Enabled by this setup, new meaningful insights can be gained into the internal processes of a thermal runaway of current and future energy-storage devices such as lithium-ion cells.

25 ENERGY STORAGE↗

DOE OSTI2024

Real-Time Observation of Nanoscale Kink Band Mediated Plasticity in Ion-Irradiated Graphite: An In Situ TEM Study

Graphite IG-110 is a synthetic polycrystalline material used as a neutron moderator in reactors. Graphite is inherently brittle and is known to exhibit a further increase in brittleness due to radiation damage at room temperature. To understand the irradiation effects on pre-existing defects and their overall influence on external load, micropillar compression tests were performed using in situ nanoindentation in the Transmission Electron Microscopy (TEM) for both pristine and ion-irradiated samples. While pristine specimens showed brittle and subsequent catastrophic failure, the 2.8 MeV Au2+ ion (fluence of 4.378 × 1014 cm−2) irradiated specimens sustained extensive plasticity at room temperature without failure. In situ TEM characterization showed nucleation of nanoscale kink band structures at numerous sites, where the localized plasticity appeared to close the defects and cracks while allowing large average strain. We propose that compressive mechanical stress due to dimensional change during ion irradiation transforms buckled basal layers in graphite into kink bands. The externally applied load during the micropillar tests proliferates the nucleation and motion of kink bands to accommodate the large plastic strain. The inherent non-uniformity of graphite microstructure promotes such strain localization, making kink bands the predominant mechanism behind unprecedented toughness in an otherwise brittle material.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Tensile behavior and microstructural evolution of a Fe-25Ni-20Cr austenitic stainless steel (alloy 709) from room to elevated temperatures through in-situ synchrotron X-ray diffraction characterization and transmission electron microscopy

Uniaxial tensile tests were done on Fe-25Ni-20Cr Austenitic Stainless Steel (Alloy 709) along with in-situ synchrotron measurement at different temperatures (25 degrees C, 500 degrees C, 700 degrees C and 900 degrees C). The X-Ray diffraction data was collected in-situ in order to follow the phases present as well as to derive the dislocation density as a function of strain through peak broadening analysis based on the modified Williamson-Hall method and see how trends are affected as a function of temperature. The XRD data were complemented by TEM and STEM-EDX characterization done on the post-experiment samples to observe the deformed microstructures. Finally, the paper presents a depiction of the tensile behavior of this advanced steel by interpreting the stress-strain curves and the effect of temperature through the information gained by in-situ XRD and TEM observations as well as fractography done ex-situ on the samples tested to rupture.

36 MATERIALS SCIENCE↗

NASA NTRS2002

Lightweight, Actively Cooled Ceramic Matrix Composite Thrustcells Successfully Tested in Rocket Combustion Lab

In a joint effort between the NASA Glenn Research Center and the NASA Marshall Space Flight Center, regeneratively cooled ceramic matrix composite (CMC) thrustcells were developed and successfully tested in Glenn's Rocket Combustion Lab. Cooled CMC's offer the potential for substantial weight savings over more traditional metallic parts. Two CMC concepts were investigated. In the first of these concepts, an innovative processing approach utilized by Hyper-Therm, Inc., allowed woven CMC coolant containment tubes to be incorporated into the complex thruster design. In this unique design, the coolant passages had varying cross-sectional shapes but maintained a constant cross-sectional area along the length of the thruster. These thrusters were silicon carbide matrix composites reinforced with silicon carbide fibers. The second concept, which was supplied by Ceramic Composites, Inc., utilized copper cooling coils surrounding a carbon-fiber-reinforced carbon matrix composite. In this design, a protective gradient coating was applied to the inner thruster wall. Ceramic Composites, Inc.'s, method of incorporating the coating into the fiber and matrix eliminated the spallation problem often observed with thermal barrier coatings during hotfire testing. The focus of the testing effort was on screening the CMC material's capabilities as well as evaluating the performance of the thermal barrier or fiber-matrix interfacial coatings. Both concepts were hot-fire tested in gaseous O2/H2 environments. The test matrix included oxygen-to-fuel ratios ranging from 1.5 to 7 with chamber pressures to 400 psi. Steady-state internal wall temperatures in excess of 4300 F were measured in situ for successful 30-sec test runs. Photograph of actively cooled composite thrustcell fabricated by Hyper-Therm is shown. The thrustcell is a silicon-carbide-fiber-reinforced silicon carbide matrix composite with woven cooling channels. The matrix is formed via chemical vapor infiltration. Photograph of hot-fire test of an actively cooled carbon-fiber-reinforced carbon matrix composite thrustcell is also shown. This composite thrustcell, which was fabricated by CCI, Inc., was wound with copper cooling coils to contain the water coolant. The tests were run with oxygen fuel ratios up to seven with chamber pressures of 200 psia.

Jaskowiak, Martha H.↗

NASA NTRS2025

CFD Validation and Scaling of a Condenser Used in an ISRU Propellant Production System

This work develops a Computational Fluid Dynamics (CFD) model of a Commercial-Off-The-Shelf (COTS) condenser used for ground-based testing of an In-Situ Resource Utilization (ISRU) propellant production system. STAR-CCM+ was used to simulate water condensing through the condenser downstream of a methanation reactor. The computational data of the digital model is validated with test cases using nitrogen and water in ambient conditions. After validation with the test data, the digital model can be used to predict scale at higher production targets. The StarCCM+ simulation of the digital model shows good agreement with the test data provided. From the simulation, the condensation rate calculated was 18.3 g/hr and the process gas mass flow rate was 709.2 g/hr. The test data measured an average 16.9 g/hr condensation rate and 693.6 g/hr process gas mass flow rate. The simulation shows a 7.3% error in the water condensation and 2.2% error in the process gas at the outlet.

Condenser↗

DOE OSTI2020

In-Situ Stress Measurements at the Utah Frontier Observatory for Research in Geothermal Energy (FORGE) Site

A scientific injection campaign was conducted at the Utah Frontier Observatory for Research in Geothermal Energy (FORGE) site in 2017 and 2019. The testing included pump-in/shut-in, pump-in/flowback, and step rate tests. Various methods have been employed to interpret the in-situ stress from the test dataset. This study focuses on methods to interpret the minimum in-situ stress from step rate, pump-in/extended shut-in tests data obtained during the stimulation of two zones in Well 58-32. This well was drilled in low-permeability granitoid. A temperature of 199 °C was recorded at the well’s total depth of 2297 m relative to the rotary Kelly bushing (RKB). The lower zone (Zone 1) consisted of 46 m of the openhole at the toe of the well. Fractures in the upper zone (Zone 2) were stimulated between 2123–2126 m measured depths (MD) behind the casing. The closure stress gradient variation depended on the depth and the injection chronology. The closure stress was found to increase with the pumping rate/volume. This stress variation could indicate that poroelastic effects (“back stress”) and the presence of adjacent natural fractures may play an important role in the interpretation of fracture closure stress. Further, progressively increasing local total stresses may, consequently, have practical applications when moderate volumes of fluid are injected in a naturally fractured or high-temperature reservoir. The alternative techniques that use pump-in/flowback tests and temperature signatures provide a valuable perspective view of the in-situ stress measurements.

15 GEOTHERMAL ENERGY↗

DOE OSTI2020

Understanding Li-Ion Cell Internal Short Circuit and Thermal Runaway through Small, Slow and In Situ Sensing Nail Penetration

Here we report a small, slow and in situ sensing (3S) nail penetration test method to understand Li-ion cell internal short circuit (ISC) and thermal runaway. The method not only keeps conventional nail penetration's advantage of simple implementation, but also enhances its relevance to field failures and enables detailed in situ diagnosis. It was applied to 3-Ah pouch cells and revealed insights that could not be captured by conventional methods. Most interestingly, multiple in situ temperature peaks were observed during a period of over 100 s before thermal runaway. These initial peaks exceeded safety limit but the temperature rapidly decreased after each peak instead of causing immediate thermal runaway. Further investigation suggested that the initial temperature peaks occurred when nail tip reached aluminum foil current collector to form a low resistance ISC between anode and aluminum foil. The rapid temperature decrease after each peak can be attributed to sudden drop of ISC current, which can be further attributed to rupture of aluminum foil and increase of contact resistance. The findings show that 3S nail penetration test can separate processes of ISC from thermal runaway and provide details of ISC at the level of individual electrode and current collector.

25 ENERGY STORAGE↗

DOE OSTI2024

Acceptance criteria for in situ surveillance of MSR materials based on thermally-loaded mechanical test articles

This report describes practices and acceptance test procedures for designing, running, and maintaining a material surveillance program in a future operating molten salt reactor. The programs described here rely on test data from passively actuated mechanical test articles inserted into critical regions of the reactor and periodically removed for out-of-reactor testing. The report defines definite acceptance procedures, based on the results of these tests, to determine whether a component can continue to operate accounting for the accumulation of environmentally-assisted mechanical damage in the component materials to date, and extrapolated out through the next inspection period. Additionally, the report describes work on a software tool implementing many of the surveillance methods and procedures described here and progress on simplified methods for inferring damage accumulation in the test articles, based on out-of-reactor thermal cycling, that do not rely on sophisticated numerical analysis.

36 MATERIALS SCIENCE↗

DOE OSTI2025

In Situ Measurement of Stress Corrosion Crack Tip Properties During Environmentally Induced Cracking in Stainless Steel 304L

The influence of the external cathodic area, stress intensity, and electrochemical polarization level on the resultant crack growth rate and crack tip pH and potential was studied for stainless steel 304L in a sodium chloride environment. Before testing, the validity of in situ crack tip property measurements using microprobes and drilled holes was supported through modeling efforts and confirmed with experimental observations. Here, it was found that increasing the R-ratio during corrosion fatigue increased the crack growth rate and decreased the measured crack tip pH of the 304L sample. Decreasing the electrochemical potential (i.e., cathodic polarization) of the bulk sample increased the crack tip pH and stopped measured crack extension under constant K conditions. Conversely, increasing the potential of the bulk sample decreased the crack tip pH and induced cracking under constant K conditions. Decreasing the cathodic area external to the crack increased the measured pH at the crack tip and decreased the crack growth rate under fatigue conditions. For the given configuration, environment, and alloy studied, fatigue crack growth is not sustained by cathodic reactions solely occurring in the crack wake and notch. These results have implications for the ability to predict atmospheric crack growth rates from laboratory, full immersion experiments.

corrosion fatigue↗

DOE OSTI2020

Design of RUSL Irradiation Experiment with Free Standing Sample

During FY19, the MIMIC-RUSL TREAT test successfully measured the shift in resonance of a cantilever beam as it underwent a grain restructuring event in the TREAT reactor core. FY20 efforts focused on a new capsule design which would replace the cantilever beam with a free-free beam. The free-free beam configuration eliminates the cantilever boundary condition and enables internal friction measurements. A test capsule was designed which supported the sample beam at the nodal points of the first flexural vibration mode. Initial tests detected the resonance peak but the signal to noise level was not high enough for in-situ measurements. Several detection probes were tested and a significant increase in the signal to noise was achieved. Although adequate signals and clean resonance peaks were measured when the beam was centered, the beam did not self-center when displaced resulting in distorted and inconsistent resonance peaks. It was concluded that the free-free beam approach is likely not suited for in-situ measurements. Measurement of ZGV plate waves is another option for in-situ microstructure monitoring and should be considered for future work.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

NASA NTRS1971

An experimental study of the mechanism of failure of rocks under borehole jack loading

Laboratory and field tests with an experimental jack and an NX-borehole jack are reported. The following conclusions were made: Under borehole jack loading, a circular opening in a brittle solid fails by tensile fracturing when the bearing plate width is not too small. Two proposed contact stress distributions can explain the mechanism of tensile fracturing. The contact stress distribution factor is a material property which can be determined experimentally. The borehole tensile strength is larger than the rupture flexural strength. Knowing the magnitude and orientation of the in situ stress field, borehole jack test results can be used to determine the borehole tensile strength. Knowing the orientation of the in situ stress field and the flexural strength of the rock substance, the magnitude of the in situ stress components can be calculated. The detection of very small cracks is essential for the accurate determination of the failure loads which are used in the calculation of strengths and stress components.

Van, T. K.↗

NASA NTRSDate not supplied

In-situ Inspection of Reflowable-Interface Composite Joints During Cure in an Autoclave

In structural bonds, the interface between adherend and adhesive is nearly two-dimensional making it susceptible to minute quantities of contamination, which can cause weak bonds. Regulatory organizations such as the Federal Aviation Administration (FAA) often require redundant load paths in secondary-bonded, primary-structures to alleviate concerns with bonded performance. Under NASA’s Convergent Aeronautics Solutions (CAS) project, the Adhesive Free Bonding of Composites (AERoBOND) project is investigating reformulated aerospace epoxy-matrix resins to enable reflow and diffusion of the resin at the joint interface during a secondary bonding and cure process. The reflow and intermixing of the matrix resin during assembly can eliminate the material discontinuity at the interface, thereby removing the dependence of bond performance on adhesion at a nearly two-dimensional boundary. AERoBOND process development has evaluated a multitude of parameters including the materials used, the stoichiometric offset of the epoxy resins, time and temperature of cure, and thickness of each ply. Without in-situ process monitoring, the condition of a test article is unknown until mechanical testing is completed. This presentation describes the use of an in-situ ultrasonic inspection system to monitor the joining of two composite parts assembled using the AERoBOND technique. This work quantifies the elimination of the interface by measuring the wave reflection, or lack thereof, at the joint throughout the cure cycle. In addition, the results indicate when reflow and cure of the epoxy resin at the joint occurred. By using the recently developed in-situ inspection with a mobile ultrasonic transducer, localized results can be obtained across a large portion of the joint with high resolution.

Tyler B Hudson↗

NASA NTRSDate not supplied

In-situ Inspection of Reflowable-Interface Composite Joints During Cure in an Autoclave

Tyler B Hudson↗

NASA NTRSDate not supplied

In-situ Inspection of Reflowable-Interface Composite Joints During Cure in an Autoclave

In structural bonds, the interface between adherend and adhesive is nearly two-dimensional making it susceptible to minute quantities of contamination, which can cause weak bonds. Regulatory organizations such as the Federal Aviation Administration (FAA) often require redundant load paths in secondary-bonded primary-structures to alleviate the inability to certify bonded performance. To address this issue, the NASA Convergent Aeronautics Solutions (CAS): Adhesive Free Bonding of Composites (AERoBOND) project is investigating reformulated aerospace epoxy-matrix resins to enable reflow and diffusion of the resin at the joint interface during a secondary bonding and cure process. The reflow and intermixing of the matrix resin during assembly can eliminate the material discontinuity at the interface, thereby removing the dependence of bond performance on adhesion at a nearly two-dimensional boundary. AERoBOND process development has evaluated a multitude of parameters including the materials used, the stoichiometric offset of the epoxy resins, time and temperature of cure, and thickness of each ply. Without in-situ process monitoring, the condition of a test article is unknown until mechanical testing is completed. This paper describes the use of an in-situ ultrasonic inspection system to monitor the joining of two composite parts assembled using the AERoBOND technique. This work quantifies the interface by measuring the wave reflection, or lack thereof, at the joint throughout the cure cycle. In addition, the results indicate when reflow and cure of the epoxy resin at the joint occurred. By using the recently developed in-situ inspection method with a mobile ultrasonic transducer, localized results can be obtained across a large portion of the joint with high resolution.

Tyler B Hudson↗

NASA NTRS2002

Convectively Induced Turbulence Encountered During NASA's Fall-2000 Flight Experiments

Aircraft encounters with atmospheric turbulence are a leading cause of in-flight injuries aboard commercial airliners and cost the airlines millions of dollars each year. Most of these injuries are due to encounters with turbulence in and around convection. In a recent study of 44 turbulence accident reports between 1990 and 1996, 82% of the cases were found to be near or within convective activity (Kaplan et al. 1999). According to NTSB accident reports, pilots' descriptions of these turbulence encounters include 'abrupt', 'in Instrument Meteorological Conditions (IMC)', 'saw nothing on the weather radar', and 'the encounter occurred while deviating around' convective activity. Though the FAA has provided guidelines for aircraft operating in convective environments, turbulence detection capability could decrease the number of injuries by alerting pilots of a potential encounter. The National Aeronautics and Space Administration, through its Aviation Safety Program, is addressing turbulence hazards through research, flight experiments, and data analysis. Primary focus of this program element is the characterization of turbulence and its environment, as well as the development and testing of hazard estimation algorithms for both radar and in situ detection. The ultimate goal is to operationally test sensors that will provide ample warning prior to hazardous turbulence encounters. In order to collect data for support of these activities, NASA-Langley's B-757 research aircraft was directed into regions favorable for convectively induced turbulence (CIT). On these flights, the airborne predictive wind shear (PWS) radar, augmented with algorithms designed for turbulence detection, was operated in real time to test this capability. In this paper, we present the results of two research flights when turbulence was encountered. Described is an overview of the flights, the general radar performance, and details of four encounters with severe turbulence.

Hamilton, David W.↗