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NASA NTRS2009

Electron Backscatter Diffraction (EBSD) Analysis and U-Pb Geochronology of the Oldest Lunar Zircon: Constraining Early Lunar Differentiation and Dating Impact-Related Deformation

The evolution of the early moon was dominated by two processes (i) crystallization of the Lunar Magma Ocean (LMO) and differentiation of potassium-rare earth element-phosphorous-rich residual magma reservoir referred to as KREEP, and (ii) an intense meteorite bombardment referred to as lunar cataclysm . The exact timing of these processes is disputed, and resolution relies on collection and interpretation of precise age data. This study examines the microstructure and geochronology of zircon from lunar impact breccias collected during the Apollo 17 mission. A large zircon clast within lunar breccia 72215,195 shows sector zoning in optical microscopy, cathodoluminescence (CL) imaging and Raman mapping, and indicates that it was a relict fragment of a much larger magmatic grain. Sensitive high resolution ion microprobe (SHRIMP) U-Pb analysis of the zircon shows that U and Th concentration correlate with sector zoning, with darkest CL domains corresponding with high-U and Th (approx.150 and approx.100 ppm respectively), and the brightest-CL sectors containing approx.30-50 ppm U and approx.10-20 ppm Th. This indicates that variations in optical CL and Raman properties correspond to differential accumulation of alpha-radiation damage in each sector. Electron backscatter diffraction (EBSD) mapping shows that the quality of electron backscatter patterns (band contrast) varies with sector zoning, with the poorest quality patterns obtained from high-U and Th, dark-CL zones. EBSD mapping also reveals a deformation microstructure that is cryptic in optical, CL and Raman imaging. Two orthogonal sets of straight discrete and gradational low-angle boundaries accommodate approx.12 misorientation across the grain. The deformation bands are parallel to the crystallographic {a}-planes of the zircon, have misorientation axes parallel to the c-axis, and are geometrically consistent with formation by dislocation creep associated with <100>{010} slip. The deformation bands are unlike curved morphology of crystal-plastic microstructures in tectonically deformed terrestrial zircon, and geometrically similar to dislocation microstructures reported in experimentally shocked zircon. We interpret these crystal-plastic deformation microstructures to have resulted from a significant impact, either directly from impact shock, or during ductile flow directly following the impact. The deformation bands appear to continue undeflected through the non-indexed, radiation-damaged areas of the grain, which suggests that the orientation variation predates any significant mechanical weakening from radiation damage in the grain, and therefore occurred early in its history.

Timms, Nick↗

NASA NTRS1976

Effect of polymer properties and adherend surfaces on adhesion

High temperature polymer surface characteristics associated with joint strength were evaluated. Selected samples represented composite adherends, aluminum filler and fiber glass carrier cloth. Detailed analysis of fractured joint surfaces revealed unique characteristics typical of the specific adhesive formulations and test conditions. A fracture mechanism model was developed for correlating macroscopic shear strength and microstructure of fracture surfaces. Applications were made to unpublished data on polyimides and fluoropolymers.

Dwight, D. W.↗

NASA NTRS1989

Time dependent reliability model incorporating continuum damage mechanics for high-temperature ceramics

Presently there are many opportunities for the application of ceramic materials at elevated temperatures. In the near future ceramic materials are expected to supplant high temperature metal alloys in a number of applications. It thus becomes essential to develop a capability to predict the time-dependent response of these materials. The creep rupture phenomenon is discussed, and a time-dependent reliability model is outlined that integrates continuum damage mechanics principles and Weibull analysis. Several features of the model are presented in a qualitative fashion, including predictions of both reliability and hazard rate. In addition, a comparison of the continuum and the microstructural kinetic equations highlights a strong resemblance in the two approaches.

Duffy, Stephen F.↗

NASA NTRS2018

Multi-Scale Modeling of Low-Density Carbon-Phenolic Ablators

Protecting a spacecraft during atmospheric entry is one of highest risk factors that needs to be mitigated during design of a space exploration mission. At entry speeds from space, air turns into high-temperature plasma, and spacecraft Thermal Protection Systems (TPS) are needed to protect the vehicle payload. Modern successful material architectures of spacecraft shields use a porous carbon fiber substrate impregnated with phenolic as an ablator material. In the lecture, efforts to build a Predictive Material Modeling framework for porous ablators from micro-scale to macro-scale will be presented. Several numerical methods and techniques will be summarized that use voxelized images to compute geometrical properties of the porous substrate. These computed properties include porosity, specific surface area and tortuosity that are otherwise indirectly measured through experimental techniques. Direct simulation Monte Carlo (DSMC), a particle-based method for approximating the Boltzmann equation, is used to compute the permeability coefficient of the porous substrate based on its digitized representation. The method computes the flow within the microstructure, where the size of the pores may approach the mean-free-path of the flow. Finally, a high-fidelity model implemented in PATO (Porous-material Analysis Toolbox) is discussed, and some examples of ablative material response are presented, including for the first time 3D simulations of the full tiled heat shield for the Mars Science Laboratory (MSL) capsule.

Ablators↗

NASA NTRS1996

Fatigue response of perforated titanium for application in laminar flow control

The room temperature tensile and fatigue response of non-perforated and perforated titanium for laminar flow control application was investigated both experimentally and analytically. Results showed that multiple perforations did not affect the tensile response, but did reduce the fatigue life. A two dimensional finite element stress analysis was used to determine that the stress fields from adjacent perforations did not influence one another. The stress fields around the holes did not overlap one another, allowing the materials to be modeled as a plate with a center hole. Fatigue life was predicted using an equivalent MW flow size approach to relate the experimental results to microstructural features of the titanium. Predictions using flaw sizes ranging from 1 to 15 microns correlated within a factor of 2 with the experimental results by using a flow stress of 260 MPa. By using two different flow stresses in the crack closure model and correcting for plasticity, the experimental results were bounded by the predictions for high applied stresses. Further analysis of the complex geometry of the perforations and the local material chemistry is needed to further understand the fatigue behavior of the perforated titanium.

Johnson, W. Steven↗

NASA NTRS2005

The Space Shuttle Columbia Accident Investigation and Reconstruction: Two Years Later

The Space Shuttle Columbia was lost during re-entry over two years ago. Since the release of the official materials-related findings in August of 2003, additional testing and analysis of select pieces of debris has continued. Microanalytical techniques, including EMPA, ESCA, and x-ray elemental dot mapping, were employed during the initial investigation; the results related the microstructural characteristics of deposit layers to the breach location in the leading edge of the left wing. Such characteristics included deposition order, composition, and distribution. Subsequent to the original efforts, new analytical data and information, not available at the time of the primary investigation, has been generated. This data was obtained via a low-vacuum SEM, fitted not only with a light-element EDS detector, but an XRF tube as well. Essentially, for elements up to sodium, classic EDS was utilized; above sodium, XRF was used. Predominantly, the elements of interest were aluminum, titanium, chromium, iron, nickel, and copper. The findings of both old and new data are compared, and their application to the overall accident investigation detailed.

McDanels, Steven J.↗

NASA NTRS2012

ISS-Experiments of Columnar-to-Equiaxed Transition in Solidification Processing

The main topic of the research project CETSOL in the framework of the Microgravity Application Promotion (MAP) programme of the European Space Agency (ESA) is the investigation of the transition from columnar to equiaxed grain growth during solidification. Microgravity environment allows for suppression of buoyancy-driven melt flow and for growth of equiaxed grains free of sedimentation and buoyancy effects. This contribution will present first experimental results obtained in microgravity using hypo-eutectic AlSi alloys in the Materials Science Laboratory (MSL) on-board the International Space Station (ISS). The analysis of the experiments confirms the existence of a columnar to equiaxed transition, especially in the refined alloy. Temperature evolution and grain structure analysis provide critical values for the position, the temperature gradient and the solidification velocity at the columnar to equiaxed transition. These data will be used to improve modeling of solidification microstructures and grain structure on different lengths scales.

Sturz, Laszlo↗

NASA NTRS2019

Modeling of the Influence of a Damaged Thermally Grown Oxide (TGO) Layer in an Environmental Barrier Coating System

Environmental barrier coatings (EBC) are an enabling technology for the successful application of ceramic matrix composites (CMCs) in air-breathing gas turbine engines. EBCs are susceptible to a number of failure modes including oxidation/delamination, recessions, chemical attack and dissolution, thermomechanical degradation, erosion, and foreign object impact damage in a combustion environment. Spallation of environmental barrier coating (EBC), induced by a thermally grown oxide (TGO) layer, is a key EBC failure mode. The TGO layer, resulting from steam oxidation, grows either from a silicon bond coat layer (if present) or from a silicon carbide (SiC) based substrate itself. The TGO layer evolves (i.e., thickness increases with time) as water vapor and oxygen gradually diffuse through the EBC, and the EBC spalls off once the TGO layer reaches some critical thickness. The critical thickness of the TGO layer for failure is in the range of 20-30 microns, but it can vary due to exposure temperature, microstructure etc. Current work at NASA Glenn Research Center, under the Revolutionary Tools and Methods (RTM) subproject is aimed at addressing associated failure modes in EBC systems and developing robust analysis tools to aid in the design/analysis of these systems. The objective of the current work is to conduct a sensitivity study to examine the influence of uniformly and non-uniformly grown oxide layers on the associated driving forces leading to spallation of the EBC when subjected to isothermal loading. The effect of damage in the TGO layer on the resulting stress states is also assessed both in uniform and non-uniform TGO layers.

Mital, Subodh K.↗

NASA NTRS2020

Influence of Thermally-Grown Oxide (TGO) Layer on the Driving Forces Associated with Failure in Environmental Barrier Coating (EBC) Systems

Environmental barrier coatings (EBC) is an enabling technology for the successful application of ceramic matrix composites (CMCs) in air-breathing gas turbine engines. Spallation of environmental barrier coating (EBC) induced by thermally grown oxide (TGO) layer is a key EBC failure mode. The TGO layer, resulting from steam oxidation, grows either from a silicon bond coat layer (if present) or from the silicon carbide (SiC) based substrate itself. Critical thickness of the TGO layer for failure is in the range of 20-30 microns but it can vary due to exposure temperature, microstructure etc. Current work at NASA Glenn Research Center, under the Revolutionary Tools and Methods (RTM) project is aimed at addressing associated failure modes in EBC systems and developing robust analysis tools to aid in the design/analysis of these systems. The objective of the current work is to conduct a sensitivity study to examine the influence of uniformly and non-uniformly grown oxide layers with or without damage on the associated driving forces leading to spallation of the EBC when subjected to isothermal loading. Initial results indicate that the presence of damage (vertical cracks caused by in-plane stresses) enhances the stresses that are present due to non-uniformity. However, the presence of non-uniformity itself is still the main factor influencing the magnitude of peel and shear stresses in the TGO layer.

Mital, Subodh K.↗

NASA NTRSDate not supplied

A Convolutional Neural Network for Multiscale Modeling of Composite Materials

An artificial convolutional neural network was created to efficiently mimic a micromechanics model, the High Fidelity Generalized Method of Cells, for use in multi-scale structural finite element analysis. The network was found to quickly and accurately replicate the stiffness predicted by the micromechanics model using a 2D image of an idealized representative volume element of a fiber/matrix microstructure. The long-term goal of this work is to efficiently apply multi-scale methods for predicting the damage progression of a composite structure.

Composites↗

NASA NTRS2021

Modeling of the Influence of Thermally Grown Oxide (TGO) Layers on the Driving Forces in Environmental Barrier Coating Systems

Environmental barrier coatings (EBC) are an enabling technology for the successful application of ceramic matrix composites (CMCs) in air-breathing gas turbine engines. EBCs are susceptible to several failure modes including oxidation/delamination, recession, chemical attack and dissolution, thermomechanical degradation, erosion, and foreign object impact damage in a combustion environment. Spallation of environmental barrier coating (EBC), induced by a thermally grown oxide (TGO) layer, is a key EBC failure mode. The TGO layer, resulting from steam oxidation, grows either from a silicon bond coat layer (if present) or from a silicon carbide (SiC) based substrate itself. The TGO layer evolves (i.e., thickness increases with time) as water vapor and oxygen gradually diffuse through the EBC, and the EBC spalls off once the TGO layer reaches some critical thickness. The critical thickness of the TGO layer for failure is in the range of 20-30 microns, with the actual value depending upon exposure temperature, microstructure, etc. Current work at NASA Glenn Research Center, under the Transformative Tools and Technology (TTT) subproject is aimed at addressing associated failure modes in EBC systems and developing robust analysis tools to aid in the design/analysis of these systems. The objective of the current work is to conduct a sensitivity study to examine the influence of uniformly and non-uniformly grown oxide layers on the associated driving forces leading to spallation of the EBC when subjected to isothermal loading. The effect of damage in the TGO layer on the resulting stress states is also assessed both in uniform and non-uniform TGO layers.

Coatings↗

NASA NTRS1998

Analysis of Phase Separation in Czochralski Grown Single Crystal Ilmenite

Ilmenite (FeTiOs) is a wide bandgap semiconductor with an energy gap of 2.58 eV. Ilmenite has properties suited for radiation tolerant applications, as well as a variety of other electronic applications. Single crystal ilmenite has been grown from the melt using the Czochralski method. Growth conditions have a profound effect on the microstructure of the samples. Here we present data from a variety of analytical techniques which indicate that some grown crystals exhibit distinct phase separation during growth. This phase separation is apparent for both post-growth annealed and unannealed samples. Under optical microscopy, there appear two distinct areas forming a matrix with an array of dots on order of 5 pm diameter. While appearing bright in the optical micrograph, atomic force microscope (AFM) shows the dots to be shallow pits on the surface. Magnetic force microscope (MFM) shows the dots to be magnetic. Phase identification via electron microprobe analysis (EMPA) indicates two major phases in the unannealed samples and four in the annealed samples, where the dots appear to be almost pure iron. This is consistent with micrographs taken with a scanning probe microscope used in the magnetic force mode. Samples that do not exhibit the phase separation have little or no discernible magnetic structure detectable by the MFM.

Wilkins, R.↗

NASA NTRS1992

Influence of convection on microstructure

The primary motivation for this research has been to determine the cause for space processing altering the microstructure of some eutectics, especially the MnBi-Bi eutectic. Prior experimental research at Grumman and here showed that the microstructure of MnBi-Bi eutectic is twice as fine when solidified in space or in a magnetic field, is uninfluenced by interfacial temperature gradient, adjusts very quickly to changes in freezing rate, and becomes coarser when spin-up/spin-down (accelerated crucible rotation technique) is used during solidification. Theoretical work at Clarkson predicted that buoyancy driven convection on earth could not account for the two fold change in fiber spacing caused by solidification in space. However, a lamellar structure with a planar interface was assumed, and the Soret effect was not included in the analysis. Experimental work at Clarkson showed that the interface is not planar, and that MnBi fibers project out in front of the Bi matrix on the order of one fiber diameter. Originally four primary hypotheses were to be tested under this current grant: (1) a fibrous microstructure is much more sensitive to convection than a lamellar microstructure, which was assumed in our prior theoretical treatment; (2) an interface with one phase projecting out into the melt is much more sensitive to convection than a planar interface, which was assumed in our prior theoretical treatment; (3) the Soret effect is much more important in the absence of convection and has a sufficiently large influence on microstructure that its action can explain the flight results; and (4) the microstructure is much more sensitive to convection when the composition of the bulk melt is off eutectic. As reported previously, we have learned that while a fibrous microstructure and a non-planar interface are more sensitive to convection than a lamellar microstructure with a planar interface, the influence of convection remains too small to explain the flight and magnetic field results. Similarly addition of the Soret effect does not explain the flight and magnetic field results.

Wilcox, William R.↗

NASA NTRS1981

Fracture and failure: Analyses, mechanisms and applications; Proceedings of the Symposium, Los Angeles, CA, March 17-20, 1980

Papers are presented on the application of fracture mechanics to spacecraft design, fracture control applications on the Space Shuttle reaction control thrusters, and an assessment of fatigue crack growth rate relationships for metallic airframe materials. Also considered are fracture mechanisms and microstructural relationships in Ni-base alloy systems, the use of surface deformation markings to determine crack propagation directions, case histories of metallurgical failures in the electronics industry, and a failure analysis of silica phenolic nozzle liners.

Tung, P. P.↗

NASA NTRS2000

PSIDD3: Post-Scan Ultrasonic Data Display System for the Windows-Based PC Including Fuzzy Logic Analysis

Post-Scan Interactive Data Display (PSIDD) III is a user-oriented Windows-based system that facilitates the display and comparison of ultrasonic contact data. The system is optimized to compare ultrasonic measurements made at different locations within a material or at different stages of material degradation. PSIDD III provides complete analysis of the primary wave forms in the time and frequency domains along with the calculation of several frequency dependent properties including Phase Velocity and Attenuation Coefficient and several frequency independent properties, like the Cross Correlation Velocity. The system allows image generation on all of the frequency dependent properties at any available frequency (limited by the bandwidth used in the scans) and on any of the frequency independent properties. From ultrasonic contact scans, areas of interest on an image can be studied with regard to underlying raw waveforms and derived ultrasonic properties by simply selecting the point on the image. The system offers various modes of in-depth comparison between scan points. Up to five scan points can be selected for comparative analysis at once. The system was developed with Borland Delphi software (Visual Pascal) and is based on a SQL database. It is ideal for classification of material properties, or location of microstructure variations in materials.

Lovelace, Jeffrey J.↗

NASA NTRS2005

Experiments and Models for Polymeric Microsphere Foams

The current project was performed under the direction of Dr. Byron Pipes as its lead investigator from January 2001 to August 2004. With the permission of the NASA, the project was transferred to Dr. Thein Kyu as the principle investigator for the period of September 2004 - June 2005. There were two major thrust areas in the original proposal; (1) experimental characterization and kinematics of foam structure formation and (2) determination of the mechanical, physical, and thermal properties, although these thrust areas were further sub- divided into 7 tasks. The present project has been directed primarily to elucidate kinematics of micro-foam formation (tasks 1 and 3) and to characterize micro-foam structures, since the control of the micro-structure of these foams is of paramount importance in determining their physical, mechanical and thermal properties. The first thrust area was accomplished in a timely manner; however, the second thrust area of foam properties (tasks 2,4-7) has yet to be completed because the area of kinematics of foam structure formation turned out to be extremely complex and thus consumed more time than what have been anticipated. As will be reported in what follows, the present studies have greatly enhances the in-depth understanding of mechanisms and kinematics of the micro-foam formation from solid powders. However, in order to implement all objectives of the second thrust areas regarding investigations of mechanical, physical, and thermal properties and establishment of the correlation of structure - properties of the foams, the project needs additional time and resources. The technical highlights of the accomplishment are summarized as follows. The present study represents a first approach to understanding the complexities that act together in the powder foaming process to achieve the successful inflation of polyimide microstructures. This type of study is novel as no prior work had dissected the fundamentals that govern the inflation process in this type of systems. The systematic approach to each of the different phenomena (i.e. morphological, diffusive, kinetic and dynamic) brings into context each of them in a way that allows separate understanding and analysis. Of the different phenomena studied, probably the one that gives a higher level of control over the inflation process has been shown to be the morphological aspects of the precursor particles. It is a major contribution of the present work to isolate and identify this phenomenon and highlight the features that with careful control during the synthesis of the precursor material can lead to a highly optimized and specialized final product (neat foam or microstructure). Some of these accomplishments have been presented in various national meetings and some of which are either published in refereed journals or still in various stages of publications. One of the presentations was selected for "Best of ANTEC 2004" Online Presentation Series of the Society of Plastics Engineers (SPE) (September 2004)

Pipes, R. Byrona↗

NASA NTRS1998

Evidence for Microfossils in Ancient Rocks and Meteorites

The McKay et all. detection of chemical biomarkers and possible microfossils in an ancient meteorite from Mars (ALH84001) stimulated research in several areas of importance to the newly emerging field of Astrobiology. Their report resulted in a search for additional evidence of microfossils in ancient terrestrial rocks and meteorites. These studies of ancient rocks and meteorites were conducted independently (and later collaboratively) in the United States and Russia using the SEM, Environmental Scanning Electron Microscope (ESEM), and Field Emission Scanning Electron Microscope (FESEM). We have encountered in-situ in freshly broken carbonaceous chondrites a large number of complex microstructures that appear to be lithified microbial forms. The meteoritic microstructures have characteristics similar to the lithified remains of filamentous cyanobacteria and bacterial microfossils we have found in ancient phosphorites, ancient graphites and oil shales. Energy Dispersive Spectroscopy (EDS) and Link microprobe analysis shows the possible microfossils have a distribution of chemical elements characteristic of the meteorite rock matrix, although many exhibit a superimposed carbon enhancement. We have concluded that the mineralized bodies encountered embedded in the rock matrix of freshly fractured meteoritic surfaces can not be dismissed as recent surface contaminants. Many of the forms found in-situ in the Murchison, Efremovka, and Orgueil carbonaceous meteorites are strikingly similar to microfossils of coccoid bacteria, cyanobacteria and fungi such as we have found in the Cambrian phosphorites of Khubsugul, Mongolia and high carbon Phanerozoic and Precambrian rocks of the Siberian and Russian Platforms.

Hoover, Richard B.↗

NASA NTRS1994

Analysis of the Erosion of Cubic Centered and Face Centered Metallic Materials [Analyse de L'erosion de Matereaux Metalliques de Structures Cubiques Centree et Face Centree]

A generalized law of erosion, in nondimensional form, is proposed. The aforementioned explicitly gives an account of the nature and the microstructure of the material impacted, the angle of impact of the particles, and their hardness. The erosion behavior of various steels, pig iron, and cast iron is examined as well as the behavior of new ordered intermetallic materials, Fe-25% Al-(Zr, Cr, B). The concern of such alloys in an erosion-corrosion environment is shown. --- Une loi généralisée d'usure par érosion, sous forme non dimensionnelle, est proposée. Celle-ci rend compte explicitement de la nature et de la microstructure du matériau impacté, de l'angle d'impact des particules, de leur acuité at de leur durete. Le comportement à l'érosion de divers aciers et fontes est examiné ainsi que la tenue de nouveaux matériaux intermétalliques ordonnés Fe-25% Al - (Zr, Cr, B). L'interet de tels alliages dans des environnements agressifs du type érosion-corrosion est montré. Mots clés: usure, érosion, modèle, matériaux métalliques, intermétalliques Fe-Al.

A Magnée↗