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NASA NTRS1972

Ion and laser microprobes applied to the measurement of corrosion produced hydrogen on a microscopic scale.

Use of an ion microprobe and a laser microprobe to measure concentrations of corrosion-produced hydrogen on a microscopic scale. Hydrogen concentrations of several thousand ppm were measured by both analytical techniques below corroded and fracture surfaces of hot salt stress corroded titanium alloy specimens. This extremely high concentration compares with only about 100 ppm hydrogen determined by standard vacuum fusion chemical analyses of bulk samples. Both the ion and laser microprobes were used to measure hydrogen concentration profiles in stepped intervals to substantial depths below the original corroded and fracture surfaces. For the ion microprobe, the area of local analysis was 22 microns in diameter and for the laser microprobe, the area of local analysis was about 300 microns in diameter. The segregation of hydrogen below fracture surfaces supports a previously proposed theory that corrosion-produced hydrogen is responsible for hot salt stress corrosion embrittlement and cracking of titanium alloys. These advanced analytical techniques suggest great potential for many areas of stress corrosion and hydrogen embrittlement research, quality control, and field inspection of corrosion problems. For example, it appears possible that a contour map of hydrogen distribution at notch roots and crack tips could be quantitatively determined. Such information would be useful in substantiating current theories of stress corrosion and hydrogen embrittlement.

Gray, H. R.↗

NASA NTRS1979

Seismic Q and velocity at depth

Measurements of the p-wave and s-wave internal friction quality factors (Q) and velocities of samples of a moderately outgassed terrestrial analog of lunar basalt exposed simultaneously to temperatures and hydrostatic confining pressures in accordance with the best available estimates of the lunar selenotherm are presented. Q values and velocities are found to increase with simulated depth, and an extrapolation of the Q value to a thoroughly outgassed states provides a Q value in reasonable agreement with those derived from lunar seismic data, suggesting a very dry lunar crust. Results also imply that similar seismic determinations for Mars would be able to distinguish between a dry crust and a crust containing water trapped beneath a layer of ice. Results of thermal cracking tests which demonstrate that high degrees of cracking associated with thermal cycling, as during the lunar day, are not inconsistent with high Q in a dry environment are presented, and it is shown that volatiles with diple moments comparable to H2O can greatly affect Q. Possible attenuation mechanisms are then considered, and velocity measurements on a synthetic anorthosite are presented.

Tittmann, B. R.↗

NASA NTRS1991

Interactions of tectonic, igneous, and hydraulic processes in the North Tharsis Region of Mars

Recent work on the north Tharsis of Mars has revealed a complex geologic history involving volcanism, tectonism, flooding, and mass wasting. Our detailed photogeologic analysis of this region found many previously unreported volcanic vents, volcaniclastic flows, irregular cracks, and minor pit chains; additional evidence that volcanic tectonic processes dominated this region throughout Martian geologic time; and the local involvement of these processes with surface and near surface water. Also, photoclinometric profiles were obtained within the region of troughs, simple grabens, and pit chains, as well as average spacings of pits along pit chains. These data were used together with techniques to estimate depths of crustal mechanical discontinuities that may have controlled the development of these features. In turn, such discontinuities may be controlled by stratigraphy, presence of water or ice, or chemical cementation.

Davis, P. A.↗

NASA NTRS1976

Rolling-contact deformation of MgO single crystals

Magnesium oxide single crystals were used as a model bearing material and deformed by rolling contact with a steel ball 0.64 cm in diameter. A dependence of depth of slip on rolling velocity which persisted with increasing numbers of rolling-contact cycles was discovered. The track width, track hardness and dislocation interactions as observed by transmission electron microscopy all increased in a consistent manner with increasing cycles. The rolling-contact state of stress produces a high density of dislocations in a localized zone. Dislocation interaction in this zone produces cleavage-type cracks after a large number of rolling-contact cycles. The orientation of the crystal influences the character of dislocation accumulation.

Dufrane, K. F.↗

DOE OSTI2023

Influence of Realistic, Cyclic Atmospheric Cycles on the Pitting Corrosion of Austenitic Stainless Steels

Pitting corrosion was evaluated on stainless steels 304H, 304, and 316L the surfaces of which had ASTM seawater printed on them as a function of surface roughness after exposure to an exemplar realistic atmospheric diurnal cycle for up to one year. Methods to evaluate pitting damage included optical imaging, scanning electron microscopy imaging, profilometry analysis, and polarization scans. The developed cyclic exposure environment did not significantly influence pitting morphology nor depth in comparison to prior static exposure environments. Cross-hatching was observed in a majority of pits for all material compositions with the roughest surface finish (#4 finish) and in all surface finishes for the 304H composition. Evidence is provided that cross-hatched pit morphologies are caused by slip bands produced during the grinding process for the #4 finish or by material processing. Additionally, micro-cracking was observed in pits formed on samples with the #4 surface finish and was greatly reduced or absent for pits formed on samples with smooth surface finishes. This suggests that both a low RH leading to an MgCl 2 -dominated environment and a rough surface containing significant residual stress are necessary for micro-cracking. Finally, the use of various characterization techniques and cross sectioning was employed to both qualitatively and quantitatively assess pitting damage across all SS compositions and surface finishes.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Indentation investigation of 304L stainless steel friction stir weld simulated crack repair

Simulated cracks were repaired in 304L stainless steel using low temperature friction stir welding. Indentation studies were carried out to understand the effect of microstructural features on the mechanical property variation across the weld and to measure the size of the weld zones with a quantitative technique. Microhardness and nanoindentation hardness profiles were constructed on a transverse section across the weld. The data obtained were correlated by extrapolating the nanoindentation hardness to greater depths which showed that the nanoindentation hardness closely reflects the microhardness values throughout the weld. Finally, grain size in the stir zone (SZ) was found to vary with the tool temperature which, in turn, alters the nanoindentation modulus variability and higher tool temperature resulted in widening of the SZ.

36 MATERIALS SCIENCE↗

NASA NTRS1975

The effect of initial flaw configuration on leak critical pressure vessel design

The effect of initial flaw shape and depth on the cycles required to produce a pressure leak condition in parent and welded 2219-T87 aluminum was examined for thicknesses from 0.04 to 0.3 inch. Initial flaw aspect ratios of 0.5, 0.3, and 0.15 were examined for tests conducted at a frequency of 4 Hz at room temperature and at 300 F. A computer program developed by Forman was used to predict the cycles to leak curve as a function of initial crack aspect ratio, material thickness, and specimen type and the results compared with the experimental data. Sources of error in the crack propagation analysis and the interface with NDI capabilities are discussed.

Pettit, D. E.↗

DOE OSTI2026

In-line measurements of below-the-surface food deformation during drying with an interference-based optical fiber strain sensor

Real-time measurements of food deformation are important for quality control in drying, yet they pose significant challenges. In this study, we developed an interference-based optical fiber strain sensor to enable in-line, continuous, below-the-surface strain measurements in drying of soft food samples. Compared to a strain resolution of 8 × 10 -4 at zero strain and 7.2 × 10 -3 at 0.20 strain reported in our previously published work, the present study achieves markedly improved resolutions of 1.3 × 10 -4 at zero strain and 7.8 × 10 -4 at 0.25 strain, which strains are the lower and higher boundaries of the dynamic range, respectively. This nearly order-of-magnitude improvement is attributed to the unique interference-based sensing mechanism, no need for calibration to convert optical signals to strain, and the system-design-enabled immunity to fiber-disk misalignments and light source intensity fluctuations. To demonstrate the in-line process monitoring, deformation measurements of fresh banana slices and sugar cookie doughs were carried out in a benchtop oven and an industrial-scale hot-air pilot dryer, respectively. In both dryers, strain measurements were continuously measured during the whole drying process at various depths and radii below the sample surfaces, with the strains up to 25%. Computer vision was used only in the benchtop drying to confirm the faithfulness of the fiber sensor measurements and cannot provide below-the-surface measurements. The measured spatiotemporal deformation allowed us to confirm the shell-hardening effect and to determine the speed and location of large deformation changes in the whole drying process, the latter of which is related to the sample cracking. To the best of the authors’ knowledge, this study is the first to report on an interferometry-based fiber sensor to measure food deformation. This sensor and the sensing mechanism have high potential for real-time process monitoring and control to prevent over-drying or cracking during drying processes.

47 OTHER INSTRUMENTATION↗

DOE OSTI2021

Performance Evaluation of Comparative Vacuum Monitoring and Piezoelectric Sensors for Structural Health Monitoring of Rotorcraft Components

The costs associated with the increasing maintenance and surveillance needs of aging structures are rising at an unexpected rate. Multi-site fatigue damage, hidden cracks in hard-to-reach locations, disbonded joints, erosion, impact, and corrosion are among the major flaws encountered in today’s extensive fleet of aging aircraft and space vehicles. Aircraft maintenance and repairs represent about a quarter of a commercial fleet’s operating costs. The application of Structural Health Monitoring (SHM) systems using distributed sensor networks can reduce these costs by facilitating rapid and global assessments of structural integrity. The use of in-situ sensors for real-time health monitoring can overcome inspection impediments stemming from accessibility limitations, complex geometries, and the location and depth of hidden damage. Reliable, structural health monitoring systems can automatically process data, assess structural condition, and signal the need for human intervention. The ease of monitoring an entire on-board network of distributed sensors means that structural health assessments can occur more often, allowing operators to be even more vigilant with respect to flaw onset. SHM systems also allow for condition-based maintenance practices to be substituted for the current time-based or cycle-based maintenance approach thus optimizing maintenance labor. The Federal Aviation Administration has conducted a series of SHM validation and certification programs intended to comprehensively support the evolution and adoption of SHM practices into routine aircraft maintenance practices. This report presents one of those programs involving a Sandia Labs-aviation industry effort to move SHM into routine use for aircraft maintenance. The Airworthiness Assurance NDI Validation Center (AANC) at Sandia Labs, in conjunction with Sikorsky, Structural Monitoring Systems Ltd., Anodyne Electronics Manufacturing Corp., Acellent Technologies Inc., and the Federal Aviation Administration (FAA) carried out a trial validation and certification program to evaluate Comparative Vacuum Monitoring (CVM) and Piezoelectric Transducers (PZT) as a structural health monitoring solution to specific rotorcraft applications. Validation tasks were designed to address the SHM equipment, the health monitoring task, the resolution required, the sensor interrogation procedures, the conditions under which the monitoring will occur, the potential inspector population, adoption of CVM and PZT systems into rotorcraft maintenance programs and the document revisions necessary to allow for their routine use as an alternate means of performing periodic structural inspections. This program addressed formal SHM technology validation and certification issues so that the full spectrum of concerns, including design, deployment, performance and certification were appropriately considered. Sandia Labs designed, implemented, and analyzed the results from a focused and statistically relevant experimental effort to quantify the reliability of a CVM system applied to Sikorsky S-92 fuselage frame application and a PZT system applied to an S-92 main gearbox mount beam application. The applications included both local and global damage detection assessments. All factors that affect SHM sensitivity were included in this program: flaw size, shape, orientation and location relative to the sensors, as well as operational and environmental variables. Statistical methods were applied to performance data to derive Probability of Detection (POD) values for SHM sensors in a manner that agrees with current nondestructive inspection (NDI) validation requirements and is acceptable to both the aviation industry and regulatory bodies. The validation work completed in this program demonstrated the ability of both CVM and PZT SHM systems to detect cracks in rotorcraft components. It proved the ability to use final system response parameters to provide a Green Light/Red Light (“GO” – “NO GO”) decision on the presence of damage. In additional to quantifying the performance of each SHM system for the trial applications on the S-92 platform, this study also identified specific methods that can be used to optimize damage detection, guidance on deployment scenarios that can affect performance and considerations that must be made to properly apply CVM and PZT sensors. These results support the main goal of safely integrating SHM sensors into rotorcraft maintenance programs. Additional benefits from deploying rotorcraft Health and Usage Monitoring Systems (HUMS) may be realized when structural assessment data, collected by an SHM system, is also used to detect structural damage to compliment the operational environment monitoring. The use of in-situ sensors for health monitoring of rotorcraft structures can be a viable option for both flaw detection and maintenance planning activities. This formal SHM validation will allow aircraft manufacturers and airlines to confidently make informed decisions about the proper utilization of CVM and PZT technology. It will also streamline future regulatory actions and formal certification measures needed to assure the safe application of SHM solutions.

42 ENGINEERING↗

DOE OSTI2022

Assessing Long-Term Cycling Stability of Single-Crystal Versus Polycrystalline Nickel-Rich NCM in Pouch Cells with 6 mAh cm -2 Electrodes

Lithium-ion batteries based on single-crystal LiNi1-x-yCoxMnyO2 (NCM, 1-x-y ≥ 0.6) cathode materials are gaining increasing attention due to their improved structural stability resulting in superior cycle life compared to batteries based on polycrystalline NCM. However, an in-depth understanding of the less pronounced degradation mechanism of single-crystal NCM is still lacking. Here, a detailed postmortem study is presented, comparing pouch cells with single-crystal versus polycrystalline LiNi 0.60 Co 0.20 Mn 0.20 O 2 (NCM622) cathodes after 1375 dis-/charge cycles against graphite anodes. The thickness of the cation-disordered layer forming in the near-surface region of the cathode particles does not differ significantly between single-crystal and polycrystalline particles, while cracking is pronounced for polycrystalline particles, but practically absent for single-crystal particles. Transition metal dissolution as quantified by time-of-flight mass spectrometry on the surface of the cycled graphite anode is much reduced for single-crystal NCM622. Similarly, CO 2 gas evolution during the first two cycles as quantified by electrochemical mass spectrometry is much reduced for single-crystal NCM622. Benefitting from these advantages, graphite/single-crystal NMC622 pouch cells are demonstrated with a cathode areal capacity of 6 mAh cm -2 with an excellent capacity retention of 83% after 3000 cycles to 4.2 V, emphasizing the potential of single-crystalline NCM622 as cathode material for next-generation lithium-ion batteries.

36 MATERIALS SCIENCE↗

NASA NTRS1989

Evaluation of the split cantilever beam for Mode 3 delamination testing

A test rig for testing a thick split cantilever beam for scissoring delamination (mode 3) fracture toughness was developed. A 3-D finite element analysis was conducted on the test specimen to determine the strain energy release rate, G, distribution along the delamination front. The virtual crack closure technique was used to calculate the G components resulting from interlaminar tension, GI, interlaminar sliding shear, GII, and interlaminar tearing shear, GIII. The finite element analysis showed that at the delamination front no GI component existed, but a GII component was present in addition to a GIII component. Furthermore, near the free edges, the GII component was significantly higher than the GIII component. The GII/GIII ratio was found to increase with delamination length but was insensitive to the beam depth. The presence of GII at the delamination front was verified experimentally by examination of the failure surfaces. At the center of the beam, where the failure was in mode 3, there was significant fiber bridging. However, at the edges of the beam where the failure was in mode 3, there was no fiber bridging and mode 2 shear hackles were observed. Therefore, it was concluded that the split cantilever beam configuration does not represent a pure mode 3 test. The experimental work showed that the mode 2 fracture toughness, GIIc, must be less than the mode 3 fracture toughness, GIIIc. Therefore, a conservative approach to characterizing mode 3 delamination is to equate GIIIc to GIIc.

Martin, Roderick H.↗

NASA NTRS1991

Evaluation of the split cantilever beam for mode III delamination testing

Martin, Roderick, H.↗

DOE OSTI2022

Microstructure-Sensitive modeling of surface roughness and notch effects on extreme value fatigue response

Fatigue life knockdown due to surface roughness induces local stress concentrations. Physical fatigue experiments are crucial to qualify materials for use but are limited in their capability to examine the mechanisms underlying the fatigue crack formation driving force due to these stress concentrations. Microstructure-sensitive computational models can aid in this regard and are employed in this work to examine the effects of surface roughness in Al 7075-T6. Digital microstructure models are subjected to crystal plasticity finite element method (CPFEM) simulations to examine the combined effects of microstructure and grain scale asperities on the driving force for fatigue crack formation. Following elastic–plastic shakedown, mesoscale volume-averaged fatigue indicator parameters (FIPs) are computed within fatigue damage process zones of grains. An increase in the intensity of realistic surface roughness profiles corresponds accordingly to larger FIPs but it is difficult to precisely interpret the mechanisms and effects of this intensification. We thus parametrically investigate surface asperities that couple with microstructure and lack of constraint on slip at the free surface to describe microstructure-sensitive surface roughness knockdown effects on fatigue resistance. The depth of a single valley (i.e., notch) due to surface roughness is found to be more detrimental to fatigue resistance than the radius (i.e., notch width, not to be confused with notch acuity). Finally, we also find that different crystallographic textures, grain morphologies, and number of sampled grains have a limited effect on the depth of influence of these notches.

36 MATERIALS SCIENCE↗

NASA NTRS2003

Mars Exploration Rovers as Virtual Instruments for Determination of Terrain Roughness and Physical Properties

The two 2003 Mars Exploration Rovers (MERs), in combination with the Athena Payload, will be used as virtual instrument systems to infer terrain properties during traverses, in addition to using the rover wheels to excavate trenches, exposing subsurface materials for remote and in-situ observations. The MERs are being modeled using finite element-based rover system transfer functions that utilize the distribution of masses associated with the vehicle, together with suspension and wheel dynamics, to infer surface roughness and mechanical properties from traverse time series data containing vehicle yaw, pitch, roll, encoder counts, and motor currents. These analyses will be supplemented with imaging and other Athena Payload measurements. The approach is being validated using Sojourner data, the FIDO rover, and experiments with MER testbed vehicles. In addition to conducting traverse science and associated analyses, trenches will be excavated by the MERs to depths of approximately 10-20 cm by locking all but one of the front wheels and rotating that wheel backwards so that the excavated material is piled up on the side of the trench away from the vehicle. Soil cohesion and angle of internal friction will be determined from the trench telemetry data. Emission spectroscopy and in-situ observations will be made using the Athena payload before and after imaging. Trenching and observational protocols have been developed using Sojourner results; data from the FIDO rover, including trenches dug into sand, mud cracks, and weakly indurated bedrock; and experiments with MER testbed rovers. Particular attention will be focused on Mini-TES measurements designed to determine the abundance and state of subsurface water (e.g. hydrated, in zeolites, residual pore ice?) predicted to be present from Odyssey GRS/NS/HEND data.

R E Arvidson↗

NASA NTRS2012

Oxidation and the Effects of High Temperature Exposures on Notched Fatigue Life of an Advanced Powder Metallurgy Disk Superalloy

Oxidation and the effects of high temperature exposures on notched fatigue life were considered for a powder metallurgy processed supersolvus heat-treated ME3 disk superalloy. The isothermal static oxidation response at 704 C, 760 C, and 815 C was consistent with other chromia forming nickel-based superalloys: a TiO2-Cr2O3 external oxide formed with a branched Al2O3 internal subscale that extended into a recrystallized - dissolution layer. These surface changes can potentially impact disk durability, making layer growth rates important. Growth of the external scales and dissolution layers followed a cubic rate law, while Al2O3 subscales followed a parabolic rate law. Cr- rich M23C6 carbides at the grain boundaries dissolved to help sustain Cr2O3 growth to depths about 12 times thicker than the scale. The effect of prior exposures was examined through notched low cycle fatigue tests performed to failure in air at 704 C. Prior exposures led to pronounced debits of up to 99 % in fatigue life, where fatigue life decreased inversely with exposure time. Exposures that produced roughly equivalent 1 m thick external scales at the various isotherms showed statistically equivalent fatigue lives, establishing that surface damage drives fatigue debit, not exposure temperature. Fractographic evaluation indicated the failure mode for the pre-exposed specimens involved surface crack initiations that shifted with exposure from predominately single intergranular initiations with transgranular propagation to multi-initiations from the cracked external oxide with intergranular propagation. Weakened grain boundaries at the surface resulting from the M23C6 carbide dissolution are partially responsible for the intergranular cracking. Removing the scale and subscale while leaving a layer where M23C6 carbides were dissolved did not lead to a significant fatigue life improvement, however, also removing the M23C6 carbide dissolution layer led to nearly full recovery of life, with a transgranular initiation typical to that observed in unexposed specimens.

Sudbrack, Chantal K.↗

NASA NTRS1985

Fault Offsets and Lateral Crustal Movement on Europa

Structural evidence is presented for tension cracking associated with strike slip faulting and crustal movement in the bright ice covered Galilean satellite Europa. The structure and morphology of wedge shaped bands argues that they formed as a result of the rotation and lateral displacement of crustal units bounded by near vertical faults penetrating through the brittle crustal layer. The significant rotation and lateral motion of crustal blocks near the anti-jove point on Europa, without graben formation, also argues that the lithosphere in the fractured area is mechanically decoupled from the solid silicate interior, by either warm ice at depth or liquid water. Ice at depth and at a large fraction of its melting temperature is expected to behave as a fluid over geologically short time intervals due to its extremely low viscosity relative to the cold, brittle ice near the surface. One proposed convection mechanism is thus considered unlikely as it would be difficult to transmit internal stress through a decoupling layer to the surface.

Schenk, P. M.↗

NASA NTRS2001

Research on High Temperature Ceramic Insulation for Electrical Conductors

Three methods for applying ceramic coatings to wires were examined in depth and a fourth (chemical vapor deposition) was studied briefly. CVD coatings were not reported in the thesis because it was realized early in the study that the deposition rate of the coatings was too slow to be used in a commercial process. Of the methods reported in the thesis, slurry coating was the most promising. This method consists of slowly drawing a platinum wire through a thixotropic slurry of alumina in a vehicle composed of polyvinyl butyral, methyl ethyl ketone, and toluene. The coatings produced by this method were continuous and free of cracks after sintering. The sintered coatings crack when the wire is bent around sharp corners, but most of the coating remains in place and still provides electrical insulation between the wire and any metallic structure to which the wire may be attached. The coating thickness was 0.61 mm (16 micrometers). The electrical resistivity of the intact coating was 340 M-Ohm-cm at 800 C and 23 M-Ohm-cm at 1050 C. Therefore, these coatings more than meet the electrical requirements for use in turbine engines. Although adherence of the coating to the wire was generally excellent, a problem was noted in localized areas where the coating flaked off. Further work will be needed to obtain good coating adherence along the entire length of the wire. The next most promising coatings were made by electrophoretic deposition (EPD) of Al2O3 onto platinum wires, using mixtures of ethanol and acetone as the suspending liquid. These EPD coatings were made only on short lengths of wire because the coating is too fragile to allow spooling of the wire. The worst coatings were those made by electrophoretic deposition from aqueous suspensions. Continuous slurry coating of wire was achieved, but due to lack of suitable equipment, the wire had to be cut into short lengths for sintering.

Kreidler, Eric R.↗

DOE OSTI2021

In–Depth Analysis of the Degradation Mechanisms of High–Nickel, Low/No–Cobalt Layered Oxide Cathodes for Lithium–Ion Batteries

A rational compositional design of high-nickel, cobalt-free layered oxide materials for high-energy and low-cost lithium-ion batteries would be expected to further propel the widespread adoption of electric vehicles (EVs), yet a composition with satisfactory electrochemical properties has yet to emerge. The previous work has demonstrated a promising LiNi 0.883 Mn 0.056 Al 0.061 O 2 (NMA-89) composition that outperformed high-nickel, cobalt-containing analogs in cycling stability and maintained a comparable rate performance and thermal stability. Herein, the capacity fading mechanism of NMA-89 in a pouch full cell with a 4.2 V cutoff is compared to that of its cobalt-containing analogs. The results reveal that particle cracking in LiNi 0.89 Mn 0.055 Co 0.055 O 2 (NMC-89) and LiNi 0.883 Co 0.053 Al 0.064 O 2 (NCA-89) leads to a loss of active material and an increase in surface area, thereby exacerbating structural and surface instabilities, accelerating impedance and polarization growth, and ultimately reducing their capacity retentions. LiNi 0.89 Mn 0.044 Co 0.042 Al 0.013 Mg 0.011 O 2 (NMCAM-89) and NMA-89 experience subdued surface reactions and maintain spherical particle structures, both of which are conducive to their capacity retentions during long-term cycling. Furthermore, this investigation offers insights into how specific transition-metal ions dictate the electrochemical stability of high-Ni layered oxide cathode materials, highlights the benefit of Mn-Al combination in NMA-89, and presents potential strategies to further enhance the performance of this novel class of cathode materials.

degradation mechanisms↗