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NASA NTRS2001

Carbonate Globules from Spitsbergen, Norway: Terrestrial Analogs of the Carbonates in Martian Meteorite ALH84001?

Pleistocene volcanic centers in NW Spitsbergen, Norway host one of the world's richest occurrences of mantle xenoliths. The xenoliths comprise varieties of spinel lherzolites and pyroxenites. Some of these xenoliths (and their host basalts) contain 10-100 micrometer globules of ankedtic-magnesitic carbonates (AMC). In composition, mineralogy and petrology the AMC globules from Spitsbergen are strikingly similar to the carbonate globules in ALH84001. The AMC globules occur within interstitial quenched glass and as fracture fillings, although we have not seen replacement fabrics analogous to carbonate rosettes replacing glass in ALH84001. Siderite/ankerite forms the core of these concentrically zoned globules while rims are predominantly magnesite. Clay minerals can occasionally be found within and around the globules. Aside from the clay minerals, the principal mineralogical difference between the AMCs and the ALH84001 carbonate rosettes is the presence of concentrated zones of nanophase magnetite in the rosettes, notably absent in the AMCs. However, carbonate globules containing nanophase magnetite have been produced inorganically by hydrothermal precipitation of carbonates and subsequent heating. We heated Spitsbergen AMC at 585 C in a reducing atmosphere to determine whether magnetite could be produced. Optical micrographs of the heated Spitsbergen AMC show dark concentric zones within the AMC. High resolution SEM images of those areas reveal 150-200 nm euhedral crystals that exhibit various morphologies including octahedra and elongated prisms. EDS analyses of areas where the crystals occur contain Fe, O, and minor Si, and P. However, the probe integrates over volumes of material, which also include the surrounding matrix. We have begun TEM observations of both the heated and unheated Spitsbergen AMC to characterize the microstructures of the carbonates, establish the presence/absence of magnetite and determine the relationship of the clay minerals to the carbonates and host rock.

De, Subarnarek↗

NASA NTRS2003

Thermo-Mechanical Processing in Friction Stir Welds

Friction stir welding is a solid-phase joining, or welding process that was invented in 1991 at The Welding Institute (TWI). The process is potentially capable of joining a wide variety of aluminum alloys that are traditionally difficult to fusion weld. The friction stir welding (FSW) process produces welds by moving a non-consumable rotating pin tool along a seam between work pieces that are firmly clamped to an anvil. At the start of the process, the rotating pin is plunged into the material to a pre-determined load. The required heat is produced by a combination of frictional and deformation heating. The shape of the tool shoulder and supporting anvil promotes a high hydrostatic pressure along the joint line as the tool shears and literally stirs the metal together. To produce a defect free weld, process variables (RPM, transverse speed, and downward force) and tool pin design must be chosen carefully. An accurate model of the material flow during the process is necessary to guide process variable selection. At MSFC a plastic slip line model of the process has been synthesized based on macroscopic images of the resulting weld material. Although this model appears to have captured the main features of the process, material specific interactions are not understood. The objective of the present research was to develop a basic understanding of the evolution of the microstructure to be able to relate it to the deformation process variables of strain, strain rate, and temperature.

Schneider, Judy↗

NASA NTRS2003

Correlation of Radiation Dosage With Mechanical Properties of Thin Films

The objective of this investigation was to examine the relationship between irradiation level (proton dose), microstructure, and stress levels in chemical vapor deposited diamond and polysilicon film using crosssectioned specimens. However, the emphasis was placed on the diamond specimen because diamond holds much promise for use in advanced technologies. The use of protons allows not only the study of the charged particle that may cause the most microstructural damage in Earth-orbit microelectromechanical systems (MEMS) devices, but also allows the study of relatively deeply buried damage inside the diamond material. Using protons allows these studies without having to resort to megaelectronvolt implant energies that may create extensive damage due to the high energy that is needed for the implantation process. Since 1 MEMS devices operating in space will not have an opportunity to reverse radiation damage via annealing, only nonannealed specimens were investigated. The following three high spatial resolution techniques were used to examine these relationships: (I) Scanning electron microscopy, (2) micro-Raman spectroscopy, and (3) micro x-ray diffraction.

Newton, R. L.↗

NASA NTRS2004

Development of Ceramic Matrix Composites For High Temperature Applications

The microstructure and mechanical properties of carbon fiber reinforced silicon carbide (C/SiC) composites that incorporated molecular-level oxidation inhibitors designed to increase the material s high temperature durability were characterized. The viability of a fiber-level inhibitor incorporated as part of a layered interface system as well as a molecularly-integrated matrix-level oxidation inhibitor that is co-deposited with the SiC matrix during Chemical Vapor Infiltration (CVI) was determined. It was expected that the inhibitor would act as a glass former that will getter the oxygen and form a crack sealant to reduce further ingress of oxygen into the composite. Three composites were examined. Composite A was a baseline C(sub f)/SiC(sub m) composite that incorporated a approx. 0.4 micron pyrolytic carbon (PyC) fiber coating to promote strength and toughness, and a CVI-derived SiC matrix. Composite B was a C(sub f)/SiC(sub m) composite incorporating a approx 0.4 micron pyrolytic carbon (PyC) fiber coating to promote strength and toughness, a approx. 0.6 micron B4C fiber-level oxidation barrier coating, and a CVI-derived SiC matrix. Composite C was a C(sub f) /SiC(sub m) composite that incorporated a approx. 0.4 micron pyrolytic carbon (PyC) fiber coating to promote strength and toughness, a approx. 0.6 micron B4C fiber-level oxidation barrier coating, and a BxC-SiC oxidation-inhibited matrix produced by CVI co-deposition. All composites were reinforced with 10 plies of T-300 balanced plain weave carbon fabric with 3K tows at 12.5 ends per inch.

Heimann, Paula↗

NASA NTRS2001

Highlights of NASA's Role in Developing State-of-the-Art Nondestructive Evaluation for Composites

Since the 1970's, when the promise of composites was being pursued for aeronautics applications, NASA has had programs that addressed the development of NDE methods for composites. These efforts included both microscopic and macroscopic NDE. At the microscopic level, NDE investigations interrogated composites at the submicron to micron level to understand a composite's microstructure. A novel microfocus CT system was developed as well as the science underlying applications of acoustic microscopy to a composite's component material properties. On the macroscopic scale NDE techniques were developed that advanced the capabilities to be faster and more quantitative. Techniques such as stiffness imaging, ultrasonic arrays, laser based ultrasound, advanced acoustic emission, thermography, and novel health monitoring systems were researched. Underlying these methods has been a strong modeling capability that has aided in method development.

Source record↗

NASA NTRS2018

Fatigue Characteristics of Additively Manufactured Aerospace Materials

This presentation documents the fatigue properties of three additive manufactured (AM) metallic systems (Ti-6-4, GRC op-84, and Alloy 718) used by NASA in various aerospace applications. These alloys were produced using the powder bed method, with the titanium alloy using an electron beam melting (EBM) and the other two alloys using selective laser melting systems (SLM). For each material a large matrix of fatigue tests were conducted and the fatigue characteristics compared to their conventionally manufactured counterparts. Build orientations and resulting microstructures are discussed with respect to the tested mechanical properties.

Lerch, Brad↗

NASA NTRSDate not supplied

Convolution-Based Numerical Solutions of Transient Temperature Fields during Powder Bed Fusion Additive Manufacturing: Theory, Accuracy, and Computational Cost

Powder bed fusion (PBF) additive manufacturing has found numerous applications in the aerospace domain. However, components fabricated via PBF have a complex time-temperature history that significantly impacts subsequent mechanical performance. This study examines convolution-based numerical solutions of transient temperature fields that support simulations involving arbitrary beam shapes and paths during PBF. The convolutional approach is verified through comparisons with analytical solutions of the temperature field. The computational speed and accuracy of the method are assessed through comparisons with other explicit and implicit numerical techniques. In addition, the straightforward translation of the approach from a CPU to a GPU implementation and the resultant performance improvement are presented. The role of the technique in predicting microstructure evolution during PBF (for a greater process-structure-property-performance framework) is also demonstrated. This work supports the development of computational materials methods for understanding and controlling the time-temperature history during PBF.

powder bed fusion↗

NASA NTRS1989

Evaluation, development, and characterization of superconducting materials for space application

Results are reported of low magnetic field studies of dc magnetic susceptibility and ac magnetic susceptibility of bulk samples and powders. These data are analyzed and compared with the microstructures and compositions of the samples as determined by scanning electron microscopic micrographs, X-ray and chemical analysis. Particular emphasis is given to the interpretation of the ac magnetic susceptibility data which were obtained as function of the magnitude and frequency of the ac measuring field, and low values of an applied dc magnetic field. Two general conclusions are given and briefly discussed.

Thorpe, A. N.↗

NASA NTRS2015

Compositional and Microstructural Evolution of Olivine During Pulsed Laser Irradiation: Insights Based on a FIB/Field-Emission TEM Study

Introduction: The use of pulsed laser irradiation to simulate the short duration, high-energy conditions characteristic of micrometeorite impacts is now an established approach in experimental space weathering studies. The laser generates both melt and vapor deposits that contain nanophase metallic Fe (npFe(sup 0)) grains with size distributions and optical properties similar to those in natural impact-generated melt and vapor deposits. There remains uncertainty, however, about how well lasers simulate the mechanical work and internal (thermal) energy partitioning that occurs in actual impacts. We are currently engaged in making a direct comparison between the products of laser irradiation and experimental/natural hypervelocity impacts. An initial step reported here is to use analytical TEM is to attain a better understanding of how the microstructure and composition of laser deposits evolve over multiple cycles of pulsed laser irradiation. Experimental Methods: We irradiated pressed-powder pellets of San Carlos olivine (Fo(sub 90)) with up to 99 rastered pulses of a GAM ArF excimer laser. The irradiated surface of the sample were characterized by SEM imaging and areas were selected for FIB cross sectioning for TEM study using an FEI Quanta dual-beam electron/focused ion beam instrument. FIB sections were characterized using a JEOL2500SE analytical field-emission scanning transmission electron microscope (FE-STEM) optimized for quantitative element mapping at less than 10 nm spatial resolutions. Results: In the SEM the 99 pulse pressed pellet sample shows a complex, inhomogeneous, distribution of laser-generated material, largely concentrated in narrow gaps and larger depressions between grains. Local concentrations of npFe0 spherules 0.1 to 1 micrometers in size are visible within these deposits in SEM back-scatter images. Fig. 1 shows bright-field STEM images of a FIB cross-section of a one of these deposits that continuously covers the top and sloping side of an olivine grain. The deposit has 3 microstructurally distinct sub-layers composed of silicate glass with varying modal fractions and size distributions of npFe( sup 0) spherules, along with nanocrystalline silicate material. A relatively thin (50-300 nm) topmost surface layer has a high-concentration of npFe0 spherules 5-20 nm in size. Element mapping shows the layer to be enriched in Fe by a factor of 2.5 relative to the olivine substrate, with Mg and Si depleted by 20% and 10% respectively. This is compositionally complementary to the underlying, middle layer of the deposit that is depleted in Fe, enriched in Mg and has a much lower npFe0 concentration. A third layer of nanocrystalline olivine occurs at the substrate interface. Discussion: The FE-STEM results suggest the topmost layer is a vapor deposit, underlain by a thicker microstructurally complex melt-generated layer. The compositional relations suggest the melt layer was partially vaporized, preferentially losing more volatile elements (e.g., Fe). The vaporized material re-condensed to form the thin, npFe(sup 0)-rich surface deposit during or immediately after the scan cycle. Nanocrystalline olivine that grew within the melt layer as it formed and cooled is similar in volume and microstructure to what we have observed in the impact melt lining of a micrometeorite impact crater in olivine. This suggest the time-temperature relations attained in the laser sample may not be too different from a micrometeorite impact. Our TEM observations, however, do not show evidence for the same level of mechanical dam-age (e.g., fracturing) seen around the natural micrometeorite crater.

Christoffersen, R.↗

NASA NTRS1971

Test and evaluation of Apollo 14 composite casting demonstration specimens 6, 9, and 12, phase 1

Flight and control specimens 6, 9, and 12 from the Apollo 14 composite casting demonstration were evaluated with respect to the degree of dispersion achieved for mixtures of immiscible materials under one-gravity and low gravity environments. The flight and control capsules 6, 9, and 12 contained paraffin and sodium acetate; paraffin, sodium acetate and argon; and paraffin, sodium acetate and 100 micrometer diameter tungsten microspheres, respectively. The evaluation and documentation utilized photographic and microstructure examinations, density measurements, and droplet size and distribution determinations. In addition, theoretical analyses were performed in order to aid in the understanding of the fluid behavior of the specimens during processing and subsequent solidification. A comparison of evaluated data with the theoretical analyses reveals that although the immiscible materials were uniquely dispersed in a low gravity environment, nonuniform dispersions were obtained primarily due to insufficient initial mixing and an essentially unidirectional thermal gradient during cooldown.

Reger, J. L.↗

NASA NTRS1992

Combustion synthesis of advanced materials

The combustion synthesis of ceramic-metal composites using an in-situ liquid infiltration technique is described. The effect of varying the reactants and their stoichiometry to provide a range of reactant and product species i.e. solids, liquids and gases, with varying physical properties e.g. thermal conductivity, on the microstructure and morphology of synthesized products is also described. Alternatively, conducting the combustion synthesis reaction in a reactive gas environment is also discussed, in which advantages can be gained from the synergistic effects of combustion synthesis and vapor phase transport. In each case, the effect of the presence or absence of gravity (density) driven fluid flow and vapor transport is discussed as is the potential for producing new and perhaps unique materials by conducting these SHS reactions under microgravity conditions.

Moore, J. J.↗

NASA NTRS1974

Research study on materials processing in space, M566 experiment

Specimens of the aluminum-33 wt% copper eutectic partially melted and resolidified in the low effective gravity of the orbiting Skylab were examined and characterized with respect to microstructural defects and thermal conductivity values. The results obtained were compared with similar evaluations of ground-based simulation melt-resolidification experiments and as-prepared unidirectionally solidified specimens. Thermal conductivity data and electrical resistivity data at temperatures from 25 C to 400 C did not show significant differences between ground and space processed specimens. A methology of evaluating the defects in the Al-Al2Cu structure was implemented. A specimen from Skylab 3 showed signs of instability in growth and several grains were found in the ingot. The specimen from Skylab 4 did not show such marked instability in growth and was found to contain fewer defects than the ground-processed specimens. This agrees with data from Georgia Institute of Technology which showed that there were fewer defects in both their Skylab 3 and 4 specimens than in ground processed specimens.

Douglas, F. C.↗

NASA NTRS2008

Microstructural Evolution in Friction Stir Welding of Ti-6Al-4V

Friction stir welding (FSW) is a thermo-mechanical process that utilizes a nonconsumable rotating pin tool to consolidate a weld joint. In the conventional FSW process, the pin tool is responsible for generating both the heat required to soften the material and the forces necessary to deform and combine the weld seam. As such, the geometry of the pin tool is important to the quality of the weld and the process parameters required to produce the weld. Because the geometry of the pin tool is limitless, a reduced set of pin tools was formed to systematically study their effect on the weldment with respect to mechanical properties and resultant microstructure. In this study 0deg, 15deg, 30deg, 45deg, and 60deg tapered, microwave sintered, tungsten carbide (WC) pin tools were used to FSW Ti-6Al-4V. Transverse sections of the weld were used to test for mechanical properties and to document the microstructure using optical microscopy. X-ray diffraction (XRD) was also used to characterize the microstructure in the welds. FSW results for the 45deg and 60deg pin tools are reported in this paper.

Rubisoff, H.↗

NASA NTRS1983

The effect of microstructure on the fatigue behavior of Ni base superalloys

Nickel-base superalloys are used in jet engine components such as disks, turbine blades, and vanes. Improvements in the fatigue behavior will allow the life to be extended or the payloads to be increased. The first part of the present investigation deals primarily with the effects of microstructural variations on the fatigue crack propagation (FCP) behavior of nickel-base alloys, while the second part is concerned with low-cycle fatigue (LCF) behavior of Ni base systems. Waspaloy at low temperature is considered, taking into account material heat treatment and test procedures, a composite plot of Waspaloy FCP data, Paris law fatigue crack propagation constants, monotonic tensile data, and overload FCP test results for Waspaloy. It is found that the FCP and overload behavior of nickel-base alloys may be markedly improved by heat treating. Attention is given to effects of cyclic deformation on microstructure and substructure, environmental damage, and an environmental/deformation model of high temperature LCF.

Antolovich, S. D.↗

NASA NTRS1984

Space Environment Effects on Spacecraft Materials (M0003)

The immediate objectives of this experiment are to understand changes in the properties and structure of materials after exposure to the space environment and to compare these changes with predictions based on laboratory experiments. The experiment consists of 19 subexperiments involving a number of DOD laboratories and contractor organizations. In general, the experimental approach with each of the subexperiments will involve comparison of preflight and postflight analyses. Typical analyses will include the measurement of optical properties (reflectance, transmittance, and refractive index), and macrophysical properties. In addition to measuring changes in the macroscopic properties of the returned specimens, microstructural properties will also be examined. Thus, it may be possible to increase our understanding of the changes induced by the environment. This increased understanding can then be used to predict the performance of materials based on knowledge of the space environment and the results of laboratory tests. This experiment will be a coopperative effort and will provide an opportunity for DOD space programs and laboratories to evaluate materials and components after long exposures to the space environment.

Paul Schall↗

NASA NTRS1976

Creep resistance

High-temperature structural applications usually require creep resistance because some average stress is maintained for prolonged periods. Alloy and microstructural design guidelines for creep resistance are presented through established knowledge on creep behavior and its functional dependences on alloy microstructure. Important considerations related to creep resistance of alloys as well as those that are harmful to high-temperature properties are examined. Although most of the creep models do not predict observed creep behavior quantitatively, they are sophisticated enough to provide alloy or microstructural design guidelines. It is shown that creep-resistant microstructures are usually in conflict with microstructures that improve such other properties as stress rupture ductility. Greater understanding of the effects of environments on creep and stress rupture behavior of materials is necessary before one can optimally design alloys for applications in different environments.

Tien, J. K.↗

NASA NTRS1985

Fracture characteristics of angleplied laminates fabricated from overaged graphite/epoxy prepreg

A series of angleplied graphite/epoxy laminates was fabricated from overaged prepreg and tested in tension to investigate the effects of overaged or advanced cure material on the degradation of laminate strength. Results, which include fracture stresses, indicate a severe degradation in strength. In addition, the fracture surfaces and microstructural characteristics are distinctly unlike any features observed in previous tests of this prepreg and laminate configuration. Photographs of the surfaces and microstructures reveal flat morphologies consisting of alternate rows of fibers and hackles. These fracture surface characteristics are independent of the laminate configurations. The photomicrographs are presented and compared with data from similar studies to show the unique characteristics produced by the overage prepreg. Analytical studies produced results which agreed with those from the experimental investigations.

Ginty, C. A.↗

NASA NTRS1987

Fracture characteristics of angleplied laminates fabricated from overaged graphite/epoxy prepreg

Ginty, Carol A.↗