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NASA NTRS1995

Atomic oxygen interactions with protected organic materials on the Long Duration Exposure Facility (LDEF)

The Long Duration Exposure Facility (LDEF) has provided an excellent opportunity to understand the nature of directed atomic oxygen interactions with protected polymers and composites. Although there were relatively few samples of materials with protective coatings on their external surfaces on LDEF which were exposed to a high atomic oxygen fluence, analysis of such samples has enabled an examination of the shape of atomic oxygen undercut cavities at defect sites in the protective coatings. Samples of front-surface aluminized (Kapton) polyimide were inspected by scanning electron microscopy to identify and measure crack defects in the aluminum protective coatings. After chemical removal of the aluminum coating, measurements were also made of the width of the oxidized undercut cavities below the crack defects. The LDEF flight undercut cavity geometries were then compared with Monte Carlo computational model undercut cavity predictions. The comparison of the LDEF results and computational modeling indicates agreement in specific undercut cavity geometries for atomic oxygen reaction probabilities dependent upon the 0.68 to 3.0 power of the energy. However, no single energy dependency was adequate to replicate flight results over a variety of aluminum crack widths.

Banks, Bruce A.↗

NASA NTRS2000

Thermographic Nondestructive Evaluation of the Space Shuttle Main Engine Nozzle

The methods and results presented in this summary address the thermographic identification of interstitial leaks in the Space Shuttle Main Engine nozzles. A highly sensitive digital infrared camera is used to record the minute cooling effects associated with a leak source, such as a crack or pinhole, hidden within the nozzle wall by observing the inner "hot wall" surface as the nozzle is pressurized. These images are enhanced by digitally subtracting a thermal reference image taken before pressurization, greatly diminishing background noise. The method provides a nonintrusive way of localizing the tube that is leaking and the exact leak source position to within a very small axial distance. Many of the factors that influence the inspectability of the nozzle are addressed; including pressure rate, peak pressure, gas type, ambient temperature and surface preparation.

Walker, James L.↗

NASA NTRS2001

Thermographic/Nondestructive Evaluation of the Space Shuttle Main Engine Nozzle

The methods and results presented in this summary address the thermographic identification of interstitial leaks in the Space Shuttle Main Engine nozzles. A highly sensitive digital infrared camera is used to record the minute cooling effects associated with a leak source, such as a crack or pinhole, hidden within the nozzle wall by observing the inner 'hot wall' surface as the nozzle is pressurized. These images are enhanced by digitally subtracting a thermal reference image taken before pressurization, greatly diminishing background noise. The method provides a nonintrusive way of localizing the tube that is leaking and the exact leak source position to within a very small axial distance. Many of the factors that influence the inspectability of the nozzle are addressed; including pressure rate, peak pressure, gas type, ambient temperature and surface preparation.

Walker, J. L.↗

NASA NTRS2001

Evaluation of Ti-48Al-2Cr-2Nb Under Fretting Conditions

The fretting behavior of Ti-48Al-2Cr-2Nb (y-TiAl) in contact with the nickel-base superalloy 718 was examined in air at temperatures from 296 to 823 K (23 to 550 C). The interfacial adhesive bonds between Ti-48Al-2Cr-2Nb and superalloy 718 were generally stronger than the cohesive bonds within Ti-48Al-2Cr-2Nb. The failed Ti-48Al-2Cr-2Nb debris subsequently transferred to the superalloy 718. In reference experiments conducted with Ti-6Al-4V against superalloy 718 under identical fretting conditions, the degree of transfer was greater for Ti-6A1-4V than for Ti-48Al-2Cr-2Nb. Wear of Ti-48Al-2Cr-2Nb generally decreased with increasing fretting frequency. The increasing rate of oxidation at elevated temperatures led to a drop in wear at 473 K. However, fretting wear increased as the temperature was increased from 473 to 823 K. At 723 and 823 K, oxide film disruption generated cracks, loose wear debris, and pits on the Ti-48Al-2Cr-2Nb wear surface. Both increasing slip amplitude and increasing load tended to produce more metallic wear debris, causing severe abrasive wear in the contacting metals.

Miyoshi, Kazuhisa↗

NASA NTRS2003

Blind Leak Detection for Closed Systems

The current inspection technique for locating interstitial leaking in the Space Shuttle Main Engine nozzles is the application of a liquid leak check solution in the openings where the interstitials space between the tubing and the structural jacket vent out the aft end of the nozzle, while its cooling tubes are pressurized to 25 psig with Helium. When a leak is found, it is classified, and if the leak is severe enough the suspect tube is cut open so that a boroscope can be inserted to find the leak point. Since the boroscope can only cover a finite tube length and since it is impossible to identify which tube (to the right or left of the identified interstitial) is leaking, many extra and undesired repairs have been made to fix just one leak. In certain instances when the interstitials are interlinked by poor braze bonding, many interstitials will show indications of leaking from a single source. What is desired is a technique that can identify the leak source so that a single repair can be performed. Dr, Samuel Russell and James Walker, both with NASA/MSFC have developed a thermographic inspection system that addresses a single repair approach. They have teamed with Boeing/Rocketdyne to repackage the inspection processes to be suitable to address full scale Shuttle development and flight hardware and implement the process at NASA centers. The methods and results presented address the thermographic identification of interstitial leaks in the Space Shuttle Main Engine nozzles. A highly sensitive digital infrared camera (capable of detecting a delta temperature difference of 0.025 C) is used to record the cooling effects associated with a leak source, such as a crack or pinhole, hidden within the nozzle wall by observing the inner hot wall surface as the nozzle is pressurized, These images are enhanced by digitally subtracting a thermal reference image taken before pressurization. The method provides a non-intrusive way of locating the tube that is leaking and the exact leak source position to within a very small axial distance. Many of the factors that influence the inspectability of the nozzle are addressed; including pressure rate, peak pressure, gas type, ambient temperature and surface preparation. Other applications for this thermographic inspection system are the Reinforced-Carbon-Carbon (RCC) leading edge of the Space Shuttle orbiter and braze joint integrity.

Oelgoetz, Peter↗

NASA NTRS1995

Effect of microgravity and hypergravity on embryo axis alignment during postencystment embryogenesis in Artemia franciscana (Anostraca)

Cysts of brine shrimp attached with a liquid adhesive to 12-mm diameter glass coverslips in a syringe-type fluid processing apparatus were flown aboard the NASA space shuttle Discovery, flight STS-60, from 3-11 February 1994, and were allowed to undergo postencystment embryogenesis and to hatch in microgravity. The shuttle flight and the ground-based control coverslips with attached cysts were parallel to the earth's surface during incubation in salt water. Based on the position of the cyst shell crack in the attached cyst population, the ground-control nauplii emerged mostly upward. On the shuttle in microgravity, although our method of detection of orientation would not reveal emergence toward the coverslip, the ratio of the position of the cyst shell crack in the population after hatching best fit the predicted values of a random direction for nauplii emergence. Centrifugation on earth was then used to create hypergravity forces of up to 73 g during postencystment embryogenesis and hatching. The upward orientation of emerging nauplii showed a high degree of correlation (r(2) =98.8%) with a linear relationship to the log of g, with 78.2% of the total hatching upward at 1 g and 91.0% hatching upward at 73 g.

NASA Program NSCORT↗

NASA NTRS2009

Simulation of RCC Crack Growth Due to Carbon Oxidation in High-Temperature Gas Environments

The carbon wall oxidation technique coupled with a CFD technique was employed to study the flow in the expanding crack channel caused by the oxidation of the channel carbon walls. The recessing 3D surface morphing procedure was developed and tested in comparison with the arcjet experimental results. The multi-block structured adaptive meshing was used to model the computational domain changes due to the wall recession. Wall regression rates for a reinforced carbon-carbon (RCC) samples, that were tested in a high enthalpy arcjet environment, were computationally obtained and used to assess the channel expansion. The test geometry and flow conditions render the flow regime as the transitional to continuum, therefore Navier-Stokes gas dynamic approach with the temperature jump and velocity slip correction to the boundary conditions was used. The modeled mechanism for wall material loss was atomic oxygen reaction with bare carbon. The predicted channel growth was found to agree with arcjet observations. Local gas flow field results were found to affect the oxidation rate in a manner that cannot be predicted by previous mass loss correlations. The method holds promise for future modeling of materials gas-dynamic interactions for hypersonic flight.

Titov, E. V.↗

DOE OSTI2022

Understanding the Origin of the Nonpassivating Behavior of Si-Based Anodes during the Initial Cycles

In this contribution, we combined electrochemical cycling and X-ray photoelectron spectroscopy (XPS) to understand the nonpassivating behavior of the solid electrolyte interphase (SEI) on Si anodes during the first cycles. Based on galvanostatic measurements, we show that the irreversible capacity loss is reduced after the first cycle, and it stays almost constant from the second cycle onwards. XPS was used to determine the root causes of the Coulombic inefficiency, showing that the rate of decomposition of the organic solvents strongly decreased after the first cycle, whereas the rate of salt decomposition is almost unchanged between cycles. We determine that the inhibition of the decomposition reaction of the organic solvent is responsible for the lower Coulombic loss during the second electrochemical cycle in comparison to the first, whereas the nonpassivating behavior toward the salt decomposition is one of the main causes of capacity loss upon cycling. Here, we further revisit the role of cracking in contributing to capacity loss. Whereas high volumetric expansion remains an issue plaguing the performance of Si anodes, our chronoamperometry studies reveal that the SEI formed on Si anodes does not passivate even when the electrode is fully expanded, and no additional surface is exposed. Overall, our work establishes the need to address the chemical and electrochemical instability of the SEI on the Si anode in addition to the more notorious issue of cracking.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2012

Surface Textures and Features Indicative of Endogenous Growth at the McCartys Flow Field, NM, as an Analog to Martian Volcanic Plains

Basaltic lavas typically form channels or tubes, which are recognized on the Earth and Mars. Although largely unrecognized in the planetary community, terrestrial inflated sheet flows also display morphologies that share many commonalities with lava plains on Mars. The McCartys lava flow field is among the youngest (approx.3000 yrs) basaltic flows in the continental United States. The southwest sections of the flow displays smooth, flat-topped plateaus with irregularly shaped pits and hummocky inter-plateau units that form a polygonal surface. Plateaus are typically elongate in map view, up to 20 m high and display lineations within the glassy crust. Lineated surfaces occasionally display small < 1m diameter lava coils. Lineations are generally straight and parallel each other, sometimes for over 100 meters. The boundaries between plateaus and depressions are also lineated and tilted to angles sometimes approaching vertical. Plateau-parallel cracks, sometimes containing squeeze-ups, mark the boundary between tilted crust and plateau. Some plateau depressions display level floors with hummocky surfaces, while some are bowl shaped with floors covered in broken lava slabs. The lower walls of pits sometimes display lateral, sagged lava wedges. Infrequently, pit floors display the upper portion of a tumulus from an older flow. In some places the surface crust has been disrupted forming a slabby texture. Slabs are typically on the scale of a meter or less across and no less than 7-10 cm thick. The slabs preserve the lineated textures of the undisturbed plateau crust. It appears that this style of terrain represents the emplacement of an extensive sheet that experiences inflation episodes within preferred regions where lateral spreading of the sheet is inhibited, thereby forming plateaus. Rough surfaces represent inflation-related disruption of pahoehoe lava and not a a lava. Depressions are often the result of non-inflation and can be clearly identified by lateral squeeze-outs along the pit walls that form when the rising crust exposes the still liquid core of the sheet. The plains of Tharsis and Elysium, Mars, display many analogous features

Bleacher, Jacob E.↗

DOE OSTI2025

SEM/EBSD Characterization of Baffle-Former Bolts Designated for High Energy X-ray Microscopy Studies at the Advanced Photon Source

This report documents the microstructural and surface characterization of two high-fluence baffle-former bolts (BFBs) harvested from a commercial pressurized water reactor (PWR) after nearly four decades of service. These bolts experienced extreme conditions including high neutron fluence, elevated temperatures, corrosive primary water, and sustained mechanical loads, all of which contribute to degradation mechanisms such as irradiation-assisted stress corrosion cracking (IASCC). Using scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD), the study assessed bulk and near-surface microstructures, grain boundary characteristics, and in-service oxide layers. The results revealed significant differences between bolts exposed to 41 dpa and 29 dpa, including differences in recrystallization extent, deformation structures, and oxidation morphology. These findings establish critical baseline data for integration with advanced synchrotron-based high-energy X-ray microscopy (HEXM) and computational crystal plasticity models. Ultimately, the work supports improved mechanistic understanding and predictive capability regarding the long-term performance of reactor core internal components.

Lach, Tim [Oak Ridge National Laboratory (ORNL), O↗

NASA NTRS1974

The detection of fatigue cracks by nondestructive testing methods

X-radiographic penetrant, ultrasonic, eddy current, holographic, and acoustic emission techniques were optimized and applied to the evaluation of 2219-T87 aluminum alloy test specimens. One hundred eighteen specimens containing a total of 328 fatigue cracks were evaluated. The cracks ranged in length from 0.500 inch (1.27 cm) to 0.007 inch (0.018 cm) and in depth from 0.178 inch (0.451 cm) and 0.001 inch (0.003 cm). Specimen thicknesses were nominally 0.060 inch (0.152 cm) and 0.210 inch (0.532 cm) and surface finishes were nominally 32 and 125 rms and 64 and 200 rms respectively. Specimens were evaluated in the as-milled surface condition, in the chemically milled surface condition and, after proof loading, in a randomized inspection sequence. Results of the nondestructive test (NDT) evaluations were compared with actual crack size obtained by measurement of the fractured specimens. Inspection data was then analyzed to provide a statistical basis for determinating the threshold crack detection sensitivity (the largest crack size that would be missed) for each of the inspection techniques at a 95% probability and 95% confidence level.

Rummel, W. D.↗

DOE OSTI2023

Effects of Accident Thermal Loading on In-Plane Shear Behavior of Steel-Plate Composite Walls

Structural walls in safety-related nuclear facilities are required to be designed for seismic and accident thermal (due to postulated high-energy pipe break events) loading combination. Current U.S. and international codes provide limited guidance for analysis and design of walls for this loading combination. This paper describes the experimental results and observations from tests conducted on a laboratory-scale (1:4 to 1:5) test unit representing steel-plate composite (SC) walls subjected to combined in-plane (seismic) and accident thermal loading. The test unit was subjected to surface temperatures of up to 450°F in combination with cyclic in-plane loading. Results of similar experiments recently conducted in Japan are also summarized (with surface temperatures up to 570°F). Surface heating combined with the low thermal conductivity and high specific heat of concrete resulted in nonlinear thermal gradients through the thickness of the specimens. These nonlinear thermal gradients and the associated self- or internal restraint led to extensive concrete cracking. This concrete cracking reduced the initial and secant stiffness of the specimens. The initial stiffness of the heated specimens reduced to 30 to 40% of the initial stiffness of the control (unheated) specimen. The secant stiffness of the heated specimens reduced up to 50% of the secant stiffness of the control (unheated) specimen. However, the in-plane shear strength of the heated SC specimens was still approximately 10 to 30% greater than the nominal in-plane shear strength calculated, for the limit state of steel plate von Mises yielding, using AISC N690 equations and measured material properties. Evaluation of the experimental results and observations suggests that the in-plane shear strength of SC walls subjected to typical accident surface temperatures (up to 570°F) can be estimated conservatively using the current provisions of AISC N690. The stiffness for accident thermal loading combinations can be considered to reduce from cracked composite stiffness at ambient temperature to fully cracked—that is, steel-only stiffness as the surface temperature increases up to typical accident value.

Construction & Building Technology↗

DOE OSTI2023

Effect of free surfaces on localized plastic deformation in single-crystal nickel containing helium bubbles and radiation-induced self-interstitial atom clusters

This paper presents molecular dynamics (MD) simulations of plastic deformation in single-crystal Ni models containing internal distributions of helium (He) bubbles and self-interstitial atom (SIA) clusters corresponding to experimental characterization of ex-service Inconel X-750 components. Here, we simulate single crystals with and without free surfaces at room temperature and 588K, the latter temperature corresponding to the Inconel X-750 service conditions. Both models are deformed under multiple slip to a maximum deviatoric strain of ~10 %. A dislocation slip band forms in the model without free surfaces, but not in the model with free surfaces. However, the latter exhibits nano-twin nucleation from surfaces. Helium (He) bubbles that overlap with a slip band or a nano-twinned region deform more severely than other bubbles in the model. Nevertheless, the bubbles do not link up and do not form configurations that resemble incipient cracks.

36 MATERIALS SCIENCE↗

NASA NTRS2013

Castable Amorphous Metal Mirrors and Mirror Assemblies

A revolutionary way to produce a mirror and mirror assembly is to cast the entire part at once from a metal alloy that combines all of the desired features into the final part: optical smoothness, curvature, flexures, tabs, isogrids, low CTE, and toughness. In this work, it has been demonstrated that castable mirrors are possible using bulk metallic glasses (BMGs, also called amorphous metals) and BMG matrix composites (BMGMCs). These novel alloys have all of the desired mechanical and thermal properties to fabricate an entire mirror assembly without machining, bonding, brazing, welding, or epoxy. BMGs are multi-component metal alloys that have been cooled in such a manner as to avoid crystallization leading to an amorphous (non-crystalline) microstructure. This lack of crystal structure and the fact that these alloys are glasses, leads to a wide assortment of mechanical and thermal properties that are unlike those observed in crystalline metals. Among these are high yield strength, carbide-like hardness, low melting temperatures (making them castable like aluminum), a thermoplastic processing region (for improving smoothness), low stiffness, high strength-to-weight ratios, relatively low CTE, density similar to titanium alloys, high elasticity and ultra-smooth cast parts (as low as 0.2-nm surface roughness has been demonstrated in cast BMGs). BMGMCs are composite alloys that consist of a BMG matrix with crystalline dendrites embedded throughout. BMGMCs are used to overcome the typically brittle failure observed in monolithic BMGs by adding a soft phase that arrests the formation of cracks in the BMG matrix. In some cases, BMGMCs offer superior castability, toughness, and fatigue resistance, if not as good a surface finish as BMGs. This work has demonstrated that BMGs and BMGMCs can be cast into prototype mirrors and mirror assemblies without difficulty.

Hofmann, Douglas C.↗

NASA NTRS2004

Improved BN Coatings on SiC Fibers in SiC Matrices

Modifications of BN-based coatings that are used as interfacial layers between the fibers and matrices of SiCfiber/SiC-matrix composite materials have been investigated to improve the thermomechanical properties of these materials. Such interfacial coating layers, which are also known as interphases (not to be confused with interphase in the biological sense), contribute to strength and fracture toughness of a fiber/matrix composite material by providing for limited amounts of fiber/matrix debonding and sliding to absorb some of the energy that would otherwise contribute to the propagation of cracks. Heretofore, the debonding and sliding have been of a type called inside debonding because they have taken place predominantly on the inside surfaces of the BN layers that is, at the interfaces between the SiC fibers and the interphases. The modifications cause the debonding and sliding to include more of a type, called outside debonding, that takes place at the outside surfaces of the BN layers that is, at the interfaces between the interphases and the matrix (see figure). One of the expected advantages of outside debonding is that unlike in inside debonding, the interphases would remain on the crack-bridging fibers. The interphases thus remaining should afford additional protection against oxidation at high temperature and should delay undesired fiber/fiber fusion and embrittlement of the composite material. A secondary benefit of outside debonding is that the interphase/matrix interfaces could be made more compliant than are the fiber/interphase interfaces, which necessarily incorporate the roughness of the SiC fibers. By properly engineering BN interphase layers to favor outside debonding, it should be possible, not only to delay embrittlement at intermediate temperatures, but also to reduce the effective interfacial shear strength and increase the failure strain and toughness of the composite material. Two techniques have been proposed and partially experimentally verified as candidate means to promote outside debonding in state-of-the-art SiC/SiC composites.

Morscher, Gregory N.↗

NASA NTRS1981

The generation and morphology of single-crystal silicon carbide wear particles under adhesive conditions

Sliding friction experiments were performed in vacuum at room temperature on a plane-type SiC surface in contact with iron-based binary alloys. Multiangular and spherical wear particles were found to form as a result of multipass sliding. The multiangular particles were produced by primary and secondary cracking of the 0001, 10(-)10, and 11(-)20 plane-type cleavage planes under the Hertzian stress field or local inelastic deformation zone. When alloy surfaces are in contact with silicon carbide under a load of 0.2 N, the alloy around the contact area is subjected to stresses that are close to the elastic limit in the elastic deformation region and/or exceed it. It was also found that spherical wear particles may be produced by two mechanisms: a penny-shaped fracture along the circular stress trajectories under the local inelastic deformation zone, and the attrition and fatigue of wear particles.

Miyoshi, K.↗

NASA NTRS2010

A Geometric Approach to Modeling Microstructurally Small Fatigue Crack Formation: Simulation and Prediction of Crack Nucleation in AA 7075-T651 - 2

The objective of this paper is to develop further a framework for computationally modeling microstructurally small fatigue crack growth in AA 7075-T651 [1]. The focus is on the nucleation event, when a crack extends from within a second-phase particle into a surrounding grain, since this has been observed to be an initiating mechanism for fatigue crack growth in this alloy. It is hypothesized that nucleation can be predicted by computing a non-local nucleation metric near the crack front. The hypothesis is tested by employing a combination of experimentation and nite element modeling in which various slip-based and energy-based nucleation metrics are tested for validity, where each metric is derived from a continuum crystal plasticity formulation. To investigate each metric, a non-local procedure is developed for the calculation of nucleation metrics in the neighborhood of a crack front. Initially, an idealized baseline model consisting of a single grain containing a semi-ellipsoidal surface particle is studied to investigate the dependence of each nucleation metric on lattice orientation, number of load cycles, and non-local regularization method. This is followed by a comparison of experimental observations and computational results for microstructural models constructed by replicating the observed microstructural geometry near second-phase particles in fatigue specimens. It is found that orientation strongly influences the direction of slip localization and, as a result, in uences the nucleation mechanism. Also, the baseline models, replication models, and past experimental observation consistently suggest that a set of particular grain orientations is most likely to nucleate fatigue cracks. It is found that a continuum crystal plasticity model and a non-local nucleation metric can be used to predict the nucleation event in AA 7075-T651. However, nucleation metric threshold values that correspond to various nucleation governing mechanisms must be calibrated.

Hochhalter, Jake D.↗

NASA NTRS1994

The effects of pitting on fatigue crack nucleation in 7075-T6 aluminum alloy

A high-strength aluminum alloy, 7075-T6, was studied to quantitatively evaluate chemical pitting effects of its corrosion fatigue life. The study focused on pit nucleation, pit growth, and fatigue crack nucleation. Pitting corrosion fatigue experiments were conducted in 3.5 percent NaCl aqueous solution under constant amplitude sinusoidal loading at two frequencies, 5 and 20 Hz. Smooth and unnotched specimens were used in this investigation. A video recording system was developed to allow in situ observation of the surface changes of the specimens during testing. The results indicated that pitting corrosion considerably reduces the fatigue strength by accelerating fatigue crack nucleation. A metallographic examination was conducted on the specimens to evaluate the nature of corrosion pits. First, the actual shapes of the corrosion pits were evaluated by cross-sectioning the pits. Secondly, the relation between corrosion pits and microstructure was also investigated. Finally, the possibility of another corrosion mechanism that might be involved in pitting was explored in this investigation. The fractography of the tested specimens showed that corner corrosion pits were responsible for fatigue crack nucleation in the material due to the associated stress concentration. The pits exhibited variance of morphology. Fatigue life for the experimental conditions appeared to be strongly dependent on pitting kinetics and the crack nucleation stage.

Ma, LI↗