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The objective of this project is to determine the influence of vibration on the composition homogeneity and microstructure of alloy semiconductors solidified with the Vertical Bridgman-Stockbarger (VBS) technique. InSb-GaSb and InSb were directionally solidified in a VBS apparatus with axial vibration of the ampoule.
Caterpillar's approach to applying Thick Thermal Barrier Coatings (TTBC's) to diesel engine combustion chambers has been to use advanced modeling techniques to predict engine conditions and combine this information with fundamental property evaluation of TTBC systems to predict engine performance and TTBC stress states. Engine testing has been used to verify the predicted performance of the TTBC systems and provide information on failure mechanisms. The objective of Caterpillar's subcontract with ORNL is to advance the fundamental understanding of thick thermal barrier coating systems. Previous reviews of thermal barrier coating technology concluded that the current level of understanding of coating system behavior is inadequate and the lack of fundamental understanding may impede the application of TTBC's to diesel engines. Areas of TTBC technology being examined in this program include powder characteristics and chemistry; bond coat composition; coating design, microstructure, and thickness as they affect properties, durability, and reliability; and TTBC 'aging' effects (microstructural and property changes) under diesel engine operating conditions. Methods to evaluate the reliability and durability of TTBC's have been developed that attempt to understand the fundamental strength of TTBC's for particular stress states.
Caterpillar's approach to applying thick thermal barrier coatings (TTBC's) to diesel engine combustion chambers has been to use advanced modeling techniques to predict engine conditions and combine this information with fundamental property evaluation of TTBC systems to predict engine performance and TTBC stress states. Engine testing has been used to verify the predicted performance of the TTBC systems and provide information on failure mechanisms. The objective Caterpillar's program to date has been to advance the fundamental understanding of thick thermal barrier coating systems. Previous reviews of thermal barrier coating technology concluded that the current level of understanding of coating system behavior is inadequate and the lack of fundamental understanding may impeded the application of TTBC's to diesel engines. Areas of TTBC technology being examined in this program include powder characteristics and chemistry; bond coat composition; coating design, microstructure, and thickness as they affect properties, durability, and reliability; and TTBC 'aging' effects (microstructural and property changes) under diesel engine operating conditions. Methods to evaluate the reliability and durability of TTBC's have been developed that attempt to understand the fundamental strength of TTBC's for particular stress states.
Some day hydrogen may be used as a viable energy storage and transport medium within the United States. Hydrogen gas may be used to dilute and extend our present methane supply as a blend or may even be used in its pure elemental form as a primary fuel. Independent of the methods of production, storage, and distribution, the interaction of hydrogen with its containment material will play an integral role in the success of a hydrogen energy program. Presently, the selection of hydrogen containment materials can be made such that the material will remain reasonably free from environmental degradation; however, costly alloying additions are required. Unfortunately, high alloy steels are economically prohibitive when large-scale hydrogen energy storage, transmission, and conversion systems are desired. Therefore, in order to implement such hydrogen energy systems in the future, existing low-cost materials must be improved via mechanical, thermal, or thermo-mechanical processing methods or new low-cost materials which are compatible with hydrogen must be developed. Originally, low strength, low alloy steels at room temperature were thought to be immune to hydrogen gas embrittlement, since no sustained load crack growth is observed. However, results of Clark in HY8O and Nelson in SAE 1020 have shown that the fatigue crack growth rate can be greatly accelerated in the presence of hydrogen gas. In recent results reported by Louthan and Mucci, the smooth bar fatigue life of an A1068 pipeline steel was reduced up to a factor of ten when the tests were performed in a 13.8 MPa hydrogen environment. These results suggest that the selection of material for structures designed to operate in hydrogen under cyclic loads must include consideration of hydrogen/metal fatigue interaction. Although the hydrogen/metal fatigue interaction can be severe in low strength low alloy steels, the degree of degradation may be altered by the underlying ferrous microstructure. At present, no correlation between microstructure and degree of hydrogen susceptibility exists for low strength steels. However, in high strength steels, susceptibility to hydrogen embrittlement has been shown to be strongly sensitive to the metallurgical microstructure. In addition, compositional effects and grain size can 703 Some day hydrogen may be used as a viable energy storage and transport medium within the United States. Hydrogen gas may be used to dilute and extend our present methane supply as a blend or may even be used in its pure elemental form as a primary fuel. Independent of the methods of production, storage, and distribution, the interaction of hydrogen with its containment material will play an integral role in the success of a hydrogen energy program. Presently, the selection of hydrogen containment materials can be made such that the material will remain reasonably free from environmental degradation; however, costly alloying additions are required. Unfortunately, high alloy steels are economically prohibitive when large-scale hydrogen energy storage, transmission, and conversion systems are desired. Therefore, in order to implement such hydrogen energy systems in the future, existing low-cost materials must be improved via mechanical, thermal, or thermo-mechanical processing methods or new low-cost materials which are compatible with hydrogen must be developed.
Microorganisms preserved within the permafrost, glaciers, and polar ice sheets of planet Earth provide analogs for microbial life forms that may be encountered in ice or permafrost of Mars, Europa, Callisto, Ganymede, asteroids, comets or other frozen worlds in the Cosmos. The psychrophilic and psychrotolerant microbes of the terrestrial cryosphere help establish the thermal and temporal limitations of life on Earth and provide clues to where and how we should search for evidence of life elsewhere in the Universe. For this reason, the cold-loving microorganisms are directly relevant to Astrobiology. Cryo-preserved microorganisms can remain viable (in deep anabiosis) in permafrost and ice for millions of years. Permafrost, ice wedges, pingos, glaciers, and polar ice sheets may contain intact ancient DNA, lipids, enzymes, proteins, genes, and even frozen and yet viable ancient microbiota. Some microorganisms carry out metabolic processes in water films and brine, acidic, or alkaline channels in permafrost or ice at temperatures far below 0 T. Complex microbial communities live in snow, ice-bubbles, cryoconite holes on glaciers and ancient microbial ecosystems are cryopreserved within the permafrost, glaciers, and polar caps. In the Astrobiology group of the NASA Marshall Space Flight Center and the University of Alabama at Huntsville, we have employed advanced techniques for the isolation, culture, and phylogenetic analysis of many types of microbial extremophiles. We have also used the Environmental Scanning Electron Microscope to study the morphology, ultra-microstructure and chemical composition of microorganisms in ancient permafrost and ice. We discuss several interesting and novel anaerobic microorganisms that we have isolated and cultured from the Pleistocene ice of the Fox Tunnel of Alaska, guano of the Magellanic Penguin, deep sea sediments from the vicinity of the Rainbow Hydrothermal Vent and enrichment cultures from ice of the Patriot Hills of Antarctica. The microbial extremophiles recovered from permafrost, ice, cold pools and deep sea sediments may provide information relevant to the question of how and where we should search for evidence of extant or extinct microbial life elsewhere in the Cosmos.
Microorganisms preserved within the permafrost, glaciers, and polar ice sheets of planet Earth provide analogs for microbial life forms that may be encountered in ice or permafrost of Mars, Europa, Callisto, Ganymede, asteroids, comets or other frozen worlds in the Cosmos. The psychrophilic and psychrotolerant microbes of the terrestrial cryosphere help establish the thermal and temporal limitations of life on Earth and provide clues to where and how we should search for evidence of life elsewhere in the Universe. For this reason, the cold-loving microorganisms are directly relevant to Astrobiology. Cryopreserved microorganisms can remain viable (in deep anabiosis) in permafrost and ice for millions of years. Permafrost, ice wedges, pingos, glaciers, and polar ice sheets may contain intact ancient DNA, lipids, enzymes, proteins, genes, and even frozen and yet viable ancient microbiota. Some microorganisms carry out metabolic processes in water films and brine, acidic, or alkaline channels in permafrost or ice at temperatures far below 0 C. Complex microbial communities live in snow, ice-bubbles, cryoconite holes on glaciers and ancient microbial ecosystems are cryopreserved within the permafrost, glaciers, and polar caps. In the Astrobiology group of the NASA Marshall Space Flight Center and the University of Alabama at Huntsville, we have employed advanced techniques for the isolation, culture, and phylogenetic analysis of many types of microbial extremophiles. We have also used the Environmental Scanning Electron Microscope to study the morphology, ultra-microstructure and chemical composition of microorganisms in ancient permafrost and ice. We discuss several interesting and novel anaerobic microorganisms that we have isolated and cultured from the Pleistocene ice of the Fox Tunnel of Alaska, guano of the Magellanic Penguin, deep-sea sediments from the vicinity of the Rainbow Hydrothermal Vent and enrichment cultures from ice of the Patriot Hills of Antarctica. The microbial extremophiles recovered from permafrost, ice, cold pools and deep-sea sediments may provide information relevant to the question of how and where we should search for evidence of extant or extinct microbial life elsewhere in the Cosmos.
Crystallization kinetics of a barium calcium aluminosilicate glass (BCAS), a sealant material for planar solid oxide fuel cells, have been investigated by differential thermal analysis (DTA). From variation of DTA peak maximum temperature with heating rate, the activation energy for glass crystallization was calculated to be 259 kJ/mol. Development of crystalline phases on thermal treatments of the glass at various temperatures has been followed by powder x-ray diffraction. Microstructure and chemical composition of the crystalline phases were investigated by scanning electron microscopy and energy dispersive spectroscopic (EDS) analysis. BaSiO3 and hexacelsian (BaAl2Si2O8) were the primary crystalline phases whereas monoclinic celsian (BaAl2Si2O8) and (Ba(x), Ca(y))SiO4 were also detected as minor phases. Needle-shaped BaSiO3 crystals are formed first, followed by the formation of other phases at longer times of heat treatments. The glass does not fully crystallize even after long term heat treatments at 750 to 900 C.
Individual aerosol particles in smoke plumes from biomass fires and in regional hazes in southern Africa were studied using analytical transmission electron microscopy (TEM), which allowed detailed characterization of carbonaceous particle types in smoke and determination of changes in particle properties and concentrations during smoke aging. Based on composition, morphology, and microstructure, three distinct types of carbonaceous particles were present in the smoke: organic particles with inorganic (K-salt) inclusions, tar ball particles, and soot. The relative number concentrations of organic particles were largest in young smoke, whereas tar balls were dominant in a slightly aged (1 hour) smoke from a smoldering fire. Flaming fires emitted relatively more soot particles than smoldering fires, but soot was a minor constituent of all studied plumes. Further aging caused the accumulation of sulfate on organic and soot particles, as indicated by the large number of internally mixed organic/sulfate and soot/sulfate particles in the regional haze. Externally mixed ammonium sulfate particles dominated in the boundary layer hazes, whereas organic/sulfate particles were the most abundant type in the upper hazes. Apparently, elevated haze layers were more strongly affected by biomass smoke than those within the boundary layer. Based on size distributions and the observed patterns of internal mixing, we hypothesize that organic and soot particles are the cloud-nucleating constituents of biomass smoke aerosols. Sea-salt particles dominated in the samples taken in stratus clouds over the Atlantic Ocean, off the coast of Namibia, whereas a distinct haze layer above the clouds consisted of aged biomass smoke particles.
Microfossils of large filamentous trichomic prokaryotes have been detected during in-situ investigations of carbonaceous meteorites. This research has been carried out using the Field Emission Scanning Electron Microscope (FESEM) to examine freshly fractured interior surfaces of the meteorites. The images obtained reveal that many of these remains are embedded in the meteorite rock matrix. Energy Dispersive X-Ray Spectroscopy (EDS) studies establish that the filamentous microstructures have elemental compositions consistent with the meteorite matrix, but are often encased within carbon-rich electron transparent sheath-like structures infilled with magnesium sulfate. This is consistent with the taphonomic modes of fossilization of cyanobacteria and sulphur bacteria, since the life habits and processes of these microorganisms frequently result in distinctive chemical biosignatures associated with the properties of their cell-walls, trichomes, and the extracellular polymeric substances (EPS) of the sheath. In this paper the evidence for biogenicity presented includes detailed morphological and morphometric data consistent with known characteristics of uniseriate and multiseriate cyanobacteria. Evidence for indigeneity includes the embedded nature of the fossils and elemental compositions inconsistent with modern biocontaminants.
NASA has an ongoing program of collecting interplanetary dust particles (IDPs) in the stratosphere using high altitude research aircraft. The collected IDPs are derived from asteroids and comets and here we report studies of a subset of hydrated IDPs rich in carbonaceous matter that are proposed to have a cometary origin. Our studies are aimed at understanding the evolution of oxygen reservoirs in the Solar System and their interaction with cometary minerals and organic matter. The small size (<20 μm) and fragility of these IDPs present a number of analytical challenges. We have pioneered techniques for performing chemical, mineralogical, isotopic, and spectroscopic measurements on the same sample in a carefully coordinated sequence. Coordinated analyses of nanogram-size samples is made possible by several delicate sample preparation techniques. To avoid organic contamination, we embed IDPs in elemental sulfur and use ultramicrotomy to partly section the particles (the first few micrometers). Multiple thin sections (50-70 nm thick) are placed on different substrates depending on the analysis technique. We use a JEOL 2500SE scanning, transmission electron microscope (STEM) to determine the mineralogy, microstructure, and elemental compositions of constituent minerals in the thin sections through a combination of high resolution imaging, electron diffraction, quantitative energy-dispersive x-ray mapping, and electron energy-loss spectroscopy. Following the STEM analyses, we use a NanoSIMS 50L for high spatial resolution isotopic measurements of H, C, N, and O to search for presolar grains and to understand the origin of the indigenous organic matter. The isotopic analyses are performed on the same sections analyzed in the STEM in order to correlate isotopic properties with the elemental and mineralogical data. We reserve other thin sections for non-destructive analyses utilizing synchrotron-based techniques including Fourier-transform infrared (FTIR) micro-spectroscopy and X-ray absorption near-edge structure (XANES) analyses, especially for functional group analysis of organic matter in the particles. The remainder of the IDP is extracted from the sulfur bead that was used for microtomy and is pressed into Au foil for quantitative analysis (including light elements) using a JEOL 8530F field emission electron probe microanalyzer (EPMA). After the EPMA measurements, high precision oxygen isotopic analyses are obtained using Cameca IMS1270/1290 instruments at UCLA. The hydrated IDPs in this study are dominated by saponitic clays, with minor magnetite, carbonate and abundant organic matter. The remarkable oxygen isotopic compositions, high carbon contents, and the abundance of isotopically anomalous organic matter, together suggest that the high carbon, hydrated IDPs are derived from primitive sources not yet represented in meteorite collections such as outer main belt P- and D-type asteroids or comets.
Hibonite is a primary ultra-refractory mineral occurring in many Ca-Al-rich inclusions (CAIs) and is predicted to condense as the second major phase from a cooling gas of solar composition. Our previous microstructural studies of hibonite in carbonaceous chondrites revealed its unique microstructures consisting of numerous defects that contain Mg-enriched, wider spinel blocks in stoichiometric hibonite. Han, J. et al. [2 items] demonstrated experimentally that defect-structured hibonites can grow easily in the presence of minor Mg and are kinetically more stable than equilibrium assemblages predicted by thermodynamic calculations. However, a thermo-dynamic vs. structural stability of defect-structured hibonite relative to other early-condensed Al-rich phases such as corundum, grossite, and spinel remains poorly constrained. Here, we present the results of atomic resolution TEM (Transmission Electron Microscopy) imaging of hibonite in a compact Type A CAI in the Allende CV3 chondrite in order to better understand the crystal structure and chemistry of defect-structured hibonite and its associated Al-rich phases, especially non-stoichiometric, Al-rich spinel, in the context of the formation of first refractory solids in the early solar nebula.
Imagine entering Earth’s atmosphere after returning from the outer solar system. A heat shield less than 2 inches thick protects you from temperatures up to 2,900° Celsius (5,252° Fahrenheit). Such conditions were experienced by NASA’s Stardust capsule during reentry in 2006. The only materials capable of providing the necessary protection are composites with complex microstructures. Evaluating these materials is difficult, requiring precise knowledge of their properties. To this end, NASA scientists are developing research codes to compute material properties and simulate ablation at the microscale using agency supercomputers. Utilizing these tools, along with experiments, researchers are working to push the limits of spaceflight, allowing for greater flexibility in future space missions.
Historically, several grades of hot pressed hexagonal boron nitride have been used for space electric propulsion applications. This study investigates the material properties of a selection of commercially available boron nitride grades including HP, M26, M, BNXX, and Shapal Hi-M. This work complements data which was presented at JANNAF 2018. The grades selected for this study are of interest because their available billet size is sufficient for space electric propulsion. This research investigates a range of material properties, tailored and focused on enhancing performance, reliability, and economics of electric propulsion thrusters. This work builds upon previous efforts by studying lot-to-lot variability of some of the properties of interest. Coefficient of friction, moisture absorption, moisture sensitivity, hot press directionality, flexural strength, compression strength, elastic modulus, thermal conductivity, thermal emissivity, thermal expansion, density, X-ray diffraction phase, microstructure, and chemical composition were all investigated across two lots of materials to help guide the selection of advanced ceramics. Variability between lots is the critical concern of the study.
Coordinated microanalyses of Wark-Lovering (WL) rims are needed to best understand their origin and to decipher their subsequent evolution both in the nebular and parent body settings. Here we present the mineralogy, petrology, microstructures, O isotopic compositions, and Al-Mg systematics of a WL rim on a Type B CAI, ‘‘Big Guy”, from the reduced CV3 chondrite Vigarano [1]. Our SEM and TEM study reveals seven distinct mineral layers in the WL rim that include: (1) gehlenite with rare grossite, (2) hibonite, (3) spinel with minor hibonite and perovskite, (4) zoned melilite (Åk(sub ~0-10)), (5) anorthite, (6) zoned diopside grading outwards from Al,Ti-rich to Al,Tipoor, and (7) forsterite intergrown with diopside. We infer a two-stage history in which WL rim formation was initiated by flash melting and extensive evaporation of the original inclusion edge, followed by subsequent condensation under highly dynamic conditions. The outermost edge of the CAI mantle is mineralogically and texturally distinct compared to the underlying mantle that is composed of coarse, zoned melilite (Åk(sub ~10-60)) grains. The mantle edge contains finegrained gehlenite with hibonite and rare grossite that likely formed by rapid crystallization from a Ca,Al-rich melt produced during a flash vaporization event [2]. These gehlenite and hibonite layers are surrounded by successive layers of spinel, melilite, diopside, and forsterite, indicating their sequential gas-solid reactions onto hibonite. Anorthite occurs as a discontinuous layer that corrodes adjacent melilite and Al-diopside, and appears to have replaced them [3,4], probably even later than the forsterite layer formation. All the WL rim minerals analyzed using the JSC NanoSIMS 50L are 16O-rich (Δ17O ≈ −23‰), indicating their formation in an 16O-rich gas reservoir. Our data are in contrast with many CV CAIs that show heterogeneous Δ 17O values across their WL rims [5]. Our Al-Mg data obtained using the UCLA ims-1290 ion microprobe of the CAI interior and the WL rim define a well-correlated isochron with (26Al/27Al)(sub 0) = 4.94 × 10(exp −5), indicating their synchronous formation ≤5 × 10(exp 4) years after the canonical CAI value. In contrast, no 26Mg excesses are observed in the WL rim anorthite, which suggests its later formation or later isotopic resetting in an 16O-rich gas reservoir, after 26Al had decayed.
Soft magnetic metal amorphous nanocomposite alloys are produced through rapid solidification and thermal annealing yielding nanocrystals embedded within an amorphous precursor. Similar free energies in Co-rich and FeNi-based alloy systems result in multiple nanocrystalline phases being formed during devitrification. Studies of multi-phase crystallization processes have been reported for Co-rich alloys but relatively few have investigated FeNi-based systems. A detailed characterization of compositional partitioning and microstructure of an optimally annealed FeNi-based MANC (Fe70Ni30)80Nb4Si2B14 alloy is presented through complementary high-resolution transmission electron microscopy (HRTEM) and atom probe tomography (APT). HRTEM demonstrates orientation relationships between FCC and BCC nanocrystals, suggesting heterogeneous nucleation of nanocrystals in the amorphous matrix or a cooperative mechanism of nucleation between BCC and FCC nanocrystallites. APT results show evidence for (i) the segregation of Fe and Ni between nanocrystals of different phases, (ii) B partitioning to the amorphous phase, and (iii) an Nb-enriched shell surrounding nanocrystals.
Fiber reinforced composites are desirable in applications where low weight and high strength are needed, but are susceptible to variability and flaws during manufacturing, making failure predictions difficult. These flaws may occur at the microscale where mechanical properties vary locally due to regions of fiber clusters and matrix pockets. In this study, a multiscale approach was taken to model 3-point bend, 4-point bend, and tensile experiments of a unidirectional composite from only having microstructure scans of these samples and constituent properties from literature. These scans were sampled with different sized windows, and statistically equivalent microstructures were generated, then simulated for stiffness, strength, and fracture toughness using a reduced order micromechanical model and NASA’s Multiscale Analysis Tool (NASMAT). Mesoscale models were created with equivalent element sizes to microstructures and properties sampled from microscale simulation results. Results showed how microscale size affects certain mechanical properties. Also shown is how well mesoscale models agree to experiments when using stochastic element properties and varying element size.
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.
Results of multiscale modeling simulations of the nonlinear response of SiC/SiC ceramic matrix composites are reported, wherein the microstructure of the ceramic matrix is captured. This micro scale architecture, which contains free Si material as well as the SiC ceramic, is responsible for residual stresses that play an important role in the subsequent thermo-mechanical behavior of the SiC/SiC composite. Using the novel Multiscale Generalized Method of Cells recursive micromechanics theory, the microstructure of the matrix, as well as the microstructure of the composite (fiber and matrix) can be captured.