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Transmission Electron Microscopy of Single Wall Carbon Nanotube/Polymer Nanocomposites: A First-Principles Study
The physics of HRTEM image formation and electron diffraction of SWCNT in a polymer matrix were investigated theoretically on the basis of the multislice method, and the optics of a FEG Super TWIN Philips CM 200 TEM operated at 80 kV. The effect of nanocomposite thickness on both image contrast and typical electron diffraction reflections of nanofillers were explored. The implications of the results on the experimental applicability to study dispersion, chirality and diameter of nanofillers are discussed.
Cooling History of Almahata Sitta Ureilite as Inferred from Transmission Electron Microscopy of Iron Metal
Almahata Sitta (AS) is a polymict breccia mainly composed of various ureilite lithologies with lesser chondritic lithologies [1]. In the ureilite lithologies, Fe metal is a common accessory phase present either as large grain boundary grains or small particles formed by reduction of olivine and pyroxene. In our earlier studies on grain boundary metals in one of AS fragments (#44) we found unique features never seen in other ureilites [2,3]. In order to further characterize these metal grains, we performed a detailed TEM study on a FIB section prepared from one of AS #44 grain boundary metals and here discuss its thermal history.
Transmission Electron Microscopy of Plagioclase-Rich Itokawa Grains: Space Weathering Effects and Solar Flare Track Exposure Ages
Limited samples are available for the study of space weathering effects on airless bodies. The grains returned by the Hayabusa mission to asteroid 25143 Itokawa provide the only samples currently available to study space weathering of ordinary chondrite regolith. We have previously studied olivine-rich Itokawa grains and documented their surface alteration and exposure ages based on the observed density of solar flare particle tracks. Here we focus on the rarer Itokawa plagioclase grains, in order to allow comparisons between Itokawa and lunar soil plagioclase grains for which an extensive data set exists.
Nucleation, growth, and strain relaxation of lattice-mismatched 3-5 semiconductor epitaxial layers
We have investigated the early stages of evolution of highly strained 2-D InAs layers and 3-D InAs islands grown by metal-organic chemical vapor deposition (MOCVD) on (100) and (111)B GaAs substrates. The InAs epilayer/GaAs substrate combination has been chosen because the lattice-mismatch is severe (approximately 7.2 percent), yet these materials are otherwise very similar. By examining InAs-on-GaAs composites instead of the more common In(x)Ga(1-x)As alloy we remove an additional degree of freedom (x) and thereby simplify data interpretation. A matrix of experiments is described in which the MOCVD growth parameters - susceptor temperature, Thin flux, and AsH3 flux - have been varied over a wide range. Scanning electron microscopy, atomic force microscopy, transmission electron microscopy, and electron microprobe analysis have been employed to observe the thin film surface morphology. In the case of 3-D growth, we have extracted activation energies and power-dependent exponents that characterize the nucleation process. As a consequence, optimized growth conditions have been identified for depositing approximately 250 A thick (100) and (111)B oriented InAs layers with relatively smooth surfaces. Together with preliminary data on the strain relaxation of these layers, the above results on the evolution of thin InAs films indicate that the (111)B orientation is particularly promising for yielding lattice-mismatched films that are fully relaxed with only misfit dislocations at the epilayer/substrate interface.
Nucleation, Growth, and Strain Relaxation of Lattice-Mismatched III-V Semiconductor Epitaxial Layers
We have investigated the early stages of evolution of highly strained 2-D InAs layers and 3-D InAs islands grown by metal-organic chemical vapor deposition (MOCVD) on (100) and (111) B GaAs substrates. The InAs epilayer / GaAs substrate combination has been chosen because the lattice-mismatch is severe (approx. 7.20%), yet these materials are otherwise very similar. By examining InAs-on-GaAs composites Instead of the more common In(x)Ga(1-x)As alloy, we remove an additional degree of freedom (x) and thereby simplify data interpretation. A matrix of experiments is described in which the MOCVD growth parameters -- susceptor temperature, TMIn flux, and AsH3 flux -- have been varied over a wide range. Scanning electron microscopy, atomic force microscopy, transmission electron microscopy, and electron microprobe analysis have been employed to observe the thin film surface morphology. In the case of 3-D growth, we have extracted activation energies and power-dependent exponents that characterize the nucleation process. As a consequence, optimized growth conditions have been identified for depositing approx. 250 A thick (100) and (111)B oriented InAs layers with relatively smooth surfaces. Together with preliminary data on the strain relaxation of these layers, the above results on the evolution of thin InAs films indicate that the (111)B orientation is particularly promising for yielding lattice-mismatched films that are fully relaxed with only misfit dislocations at the epilayer / substrate interface.
Indigenous Carbonaceous Matter in the Nakhla Mars Meteorite
Detailed microanalysis of the Martian meteorite Nakhla has shown there are morphologically distinct carbonaceous features spatially associated with low-T aqueous alteration phases including salts and id-dingsite. A comprehensive suite of analytical instrumentation including optical microscopy, field emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX) spectroscopy, focused ion beam (FIB) microscopy, transmission electron microscopy (TEM), two-step laser mass spectrometry (mu-L(sup 2)MS), laser mu-Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), and nanoscale secondary ion mass spectrometry (NanoSIMS) are being used to characterize the carbonaceous matter and host mineralogy. The search for carbonaceous matter on Mars has proved challenging. Viking Landers failed to unambiguously detect simple organics at either of the two landing sites although the Martian surface is estimated to have acquired at least 10(exp15) kg of C as a consequence of meteoritic accretion over the last several Ga. The dearth of organics at the Martian surface has been attributed to various oxidative processes including UV photolysis and peroxide activity. Consequently, investigations of Martian organics need to be focused on the sub-surface regolith where such surface processes are either severely attenuated or absent. Fortuitously since Martian meteorites are derived from buried regolith materials they provide a unique opportunity to study Martian organic geochemistry.
Investigation of high temperature fracture of T-111 and ASTAR-811C
The high temperature deformation and fracture behavior of T-111 and ASTAR-811C were studied over the temperature range 982 to 2205 C (1800 to 4000 F). As-cast and wrought-recrystallized material as well as GTA welds in sheet and plate were evaluated using conventional tensile and creep tests. Post test examinations were performed using optical metallography, scanning electron microscopy and transmission electron microscopy. A high temperature region of reduced ductility, in terms of tensile elongation, was identified for both alloys. The reduction in tensile elongation became more severe with increase in grain size, being near catastrophic for the as-cast specimens. Optical and electron metallography indicated that even for failures at very low total strain, considerable deformation of a very localized nature had occurred prior to fracture.
Avoidance of stress corrosion susceptibility in high strength aluminum alloys by control of grain boundary and matrix microstructure
The relation of microstructure to the mechanical strength and stress corrosion resistance of highest strength and overaged tempers of BAR and 7050 aluminum alloys was investigated. Comparison is made with previously studied 7075 aluminum alloy. Optical microscopy, transmission electron microscopy, and differential scanning calorimetry were used to characterize the grain morphology, matrix microstructure, and grain boundary microstructure of these tempers. Grain boundary interparticle spacing was significant to stress corrosion crack propagation for all three alloys; increasing interparticle spacing led to increased resistance to crack propagation. In addition, the fire grain size in Bar and 7050 appears to enhance crack propagation. The highest strength temper of 7050 has a comparatively high resistance to crack initiation. Overall stress corrosion behavior is dependent on environment pH, and evaluation over a range of pH is recommended.
Microstructure and mechanical properties of bulk and plasma-sprayed y2O3-partially stabilized zirconia
Bulk 8.0 weight percent yttria partially stabilied zirconia (PSZ) was studied by light microscopy, transmission electron microscopy, X-ray analysis, microhardness testing, and fracture toughness testing. The as received PSZ contained spheroidal and grain boundary precipitates up to 4 micrometers in size. Spheroids up to 1.26 micrometers were metastable tetragonal; large spheroids were monoclinic. Grinding the PSZ into powder did not cause a significant amount of tetragonal to transform to monoclinic. This indicates that transformation toughness is not a significant mechanism in PSZ. Aging the PSZ at 1500 C caused the fine tetragonal precipitates to grow from 0.06 to 0.12 micrometers, in 250 minutes. A peak hardness of 1400 kg/sq mm was attained after 50 minutes. Solution annealing and quenching the as received PSZ eliminated the large precipitates, but fine tetragonal precipitates reformed on quenching. Aging at 1500 C caused the fine 0.02 micrometers tetragonal precipitates to grow into plates about 0.10 by 0.50 micrometers. A peak hardness of 1517 kg/sq mm was obtained after 250 minutes. On further aging, monoclinic percipitates formed along grain boundaries. The fracture toughness of the aged and unaged solution annealed and quenched PSZ was found to be between 2 and 3 MN /square root of m cubed. This range of fracture toughness is consistent with PSZ's that do not undergo transformation toughening.
Coaxial carbon plasma gun deposition of amorphous carbon films
A unique plasma gun employing coaxial carbon electrodes was used in an attempt to deposit thin films of amorphous diamond-like carbon. A number of different structural, compositional, and electrical characterization techniques were used to characterize these films. These included scanning electron microscopy, scanning transmission electron microscopy, X ray diffraction and absorption, spectrographic analysis, energy dispersive spectroscopy, and selected area electron diffraction. Optical absorption and electrical resistivity measurements were also performed. The films were determined to be primarily amorphous, with poor adhesion to fused silica substrates. Many inclusions of particulates were found to be present as well. Analysis of these particulates revealed the presence of trace impurities, such as Fe and Cu, which were also found in the graphite electrode material. The electrodes were the source of these impurities. No evidence of diamond-like crystallite structure was found in any of the film samples. Details of the apparatus, experimental procedure, and film characteristics are presented.
Sliding wear of self-mated Al2O3-SiC whisker reinforced composites at 23-1200 C
Microstructural changes occurring during sliding wear of self-mated Al2O3-SiC whisker reinforced composites were studied using optical, scanning electron microscopy, and transmission electron microscopy. Pin-on-disk specimens were slid in air at 2.7 m/sec sliding velocity under a 26.5 N load for 1 hr. Wear tests were conducted at 23, 600, 800, and 1200 C. Mild wear with a wear factor of 2.4 times 10(exp -7) to 1.5 times 10(exp -6) cu mm/Nm was experienced at all test temperatures. The composite shows evidence of wear by fatigue mechanisms at 800 C and below. Tribochemical reaction (SiC oxidation and reaction of SiO2 and Al2O3) leads to intergranular failure at 1200 C. Distinct microstructural differences existing at each test temperature are reported.
Mineralogy of an unusual Cr-rich inclusion in the Los Martinez (L6) chrondritic breccia
During the petrological study of the L6 chondritic breccia, Los Martinez, we discovered a large, highly unusual Cr-rich inclusion whose mineralogy appears to be unique in both terrestrial and extraterrestrial occurrences. We carried out electron microprobe, scanning electron microscopy, and transmission electron microscopy investigations of this inclusion in order to determine its composition and mineralogy in detail and to establish its origin and possible relationship to other Cr-rich objects in chondritic meteorites. Details of the chemical composition, origin, and thermal history are given.
Sliding wear of self-mated Al2O3-SiC whisker-reinforced composites at 23-1200 C
Microstructural changes occurring during sliding wear of self-mated Al2O3 SiC whisker-reinforced composites were studied using optical, scanning electron microscopy and transmission electron microscopy. Pin-on-disc specimens were slid in air at 2.7 m/s sliding velocity under a 26.5 N load for 1 h. Wear tests were conducted at 23, 600, 800 and 1200 C. Mild wear with a wear factor of 2.4 x 10 exp -7 - 1.5 x 10 exp -6 cu mm /N per m was experienced at all test temperatures. The composite showed evidence of wear by fatigue mechanisms at 800 C and below. Tribochemical reaction (SiC oxidation and reaction of SiO2 and Al2O3) leads to intergranular failure at 1200 C. Distinct microstructural differences existing at each test temperature are reported.
Tensile Strength and Microstructural Characterization of Uncoated and Coated HPZ Ceramic Fibers
Tensile strengths of as-received HPZ fiber and those surface coated with BN, BN/SiC, and BN/Si3N4 have been determined at room temperature using a two-parameter Weibull distribution. Nominally approx. 0.4 micron BN and 0.2 micron SiC or Si3N4 coatings were deposited on the fibers by chemical vapor deposition using a continuous reactor. The average tensile strength of uncoated HPZ fiber was 2.0 +/- 0.56 GPa (290 +/- 81 ksi) with a Weibull modulus of 4.1. For the BN coated fibers, the average strength and the Weibull modulus increased to 2.39 +/- 0.44 GPa (346 +/- 64 ksi) and 6.5, respectively. The HPZ/BN/SiC fibers showed an average strength of 2.0 +/- 0.32 GPa (290 +/- 47 ksi) and Weibull modulus of 7.3. Average strength of the fibers having a dual BN/Si3N4 surface coating degraded to 1.15 +/- 0.26 GPa (166 +/- 38 ksi) with a Weibull modulus of 5.3. The chemical composition and thickness of the fiber coatings were determined using scanning Auger analysis. Microstructural analysis of the fibers and the coatings was carried out by scanning electron microscopy and transmission electron microscopy. A microporous silica-rich layer approx. 200 nm thick is present on the as-received HPZ fiber surface. The BN coatings on the fibers are amorphous to partly turbostratic and contaminated with carbon and oxygen. Silicon carbide coating was crystalline whereas the silicon nitride coating was amorphous. The silicon carbide and silicon nitride coatings are non-stoichiometric, non-uniform, and granular. Within a fiber tow, the fibers on the outside had thicker and more granular coatings than those on the inside.
Microgravity effects during fertilization, cell division, development, and calcium metabolism in sea urchins
The overall objectives of this project are to explore the role of microgravity during fertilization, early development, cytoskeletal organization, and skeletal calcium deposition in a model development system: the sea urchin eggs and embryos. While pursuing these objectives, we have also helped to develop, test, and fly the Aquatic Research Facility (ARF) system. Cells were fixed at preselected time points to preserve the structures and organelles of interest with regards to cell biology events during development. The protocols used for the analysis of the results had been developed during the earlier part of this research and were applied for post-flight analysis using light and (immuno)fluorescence microscopy, scanning electron microscopy, and transmission electron microscopy. The structures of interest are: microtubules during fertilization, cell division, and cilia movement; microfilaments during cell surface restructuring and cell division; centrosomes and centrioles during cell division, cell differentiation, and cilia formation and movement; membranes, Golgi, endoplasmic reticulum, mitochondria, and chromosomes at all stages of development; and calcium deposits during spicule formation in late-stage embryos. In addition to further explore aspects important or living in space, several aspects of this research are also aimed at understanding diseases that affect humans on Earth which may be accelerated in space.
Effects of HF Treatments on Tensile Strength of Hi-Nicalon Fibers
Tensile strengths of as-received Hi-Nicalon fibers and those having a dual BN/SiC surface coating, deposited by chemical vapor deposition, have been measured at room temperature. These fibers were also treated with HF for 24 h followed by tensile strength measurements. Strengths of uncoated and BN/SiC coated Hi-Nicalon fibers extracted from celsian matrix composites, by dissolving away the matrix in HF for 24 h, were also determined. The average tensile strength of uncoated Hi-Nicalon was 3.19 +/- 0.73 GPa with a Weibull modulus of 5.41. The Hi-Nicalon/BN/SiC fibers showed an average strength of 3.04 q 0.53 GPa and Weibull modulus of 6.66. After HF treatments, the average strengths of the uncoated and BN/SiC coated Hi-Nicalon fibers were 2.69 +/- 0.67 GPa and 2.80 +/- 0.53 GPa and the Weibull moduli were 4.93 and 5.96, respectively. The BN/SiC coated fibers extracted from the celsian matrix composite exhibited a strength of 2.38 +/- 0.40 GPa and a Weibull modulus of 7.15. The strength of the uncoated Hi-Nicalon fibers in the composite was so severely degraded that they disintegrated into small fragments during extraction with HF. The uncoated fibers probably undergo mechanical surface damage during hot pressing of the composites. Also, the BN layer on the coated fibers acts as a compliant layer which protects the fibers from mechanical damage during composite processing. The elemental composition and thickness of the fiber coatings were deten-nined using scanning Auger analysis. Microstructural analyses of the fibers and the coatings were done by scanning electron microscopy and transmission electron microscopy. Strengths of fibers calculated using average and measured fiber diameters were in good agreement. Thus, the strength of fibers can be evaluated using an average fiber diameter instead of the measured diameter of each filament.
Microstructural, Chemical and Mechanical Characterization of Polymer-Derived Hi-Nicalon Fibers with Surface Coatings
Room temperature tensile strengths of as-received Hi-Nicalon fibers and those having BN/SiC, p-BN/SiC, and p-B(Si)N/SiC surface coatings, deposited by chemical vapor deposition, were measured using an average fiber diameter of 13.5 microns. The Weibull statistical parameters were determined for each fiber. The average tensile strength of uncoated Hi-Nicalon on was 3.19 +/- 0.73 GPa with a Weibull modulus of 5.41. Strength of fibers coated with BN/SiC did not change. However, coat with p-BN/SiC and p-B(Si)N/SiC surface layers showed strength loss of approx. 10 and 35 percent, respectively, compared with as-received fibers. The elemental compositions of the fibers and the coatings were analyzed using scanning Auger microprobe and energy dispersive x-ray spectroscopy. The BN coating was contaminated with a large concentration of carbon and some oxygen. In contrast, p-BN, p-B(Si)N, and SiC coatings did not show any contamination. Microstructural analyses of the fibers and the coatings were done by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction. Hi-Nicalon fiber consists of the P-SIC nanocrystals ranging in size from 1 to 30 nm embedded in an amorphous matrix. TEM analysis of the BN coating revealed four distinct layers with turbostatic structure. The p-BN layer was turbostratic and showed considerable preferred orientation. The p-B(Si)N was glassy and the silicon and boron were uniformly distributed. The silicon carbide coating was polycrystalline with a columnar structure along the growth direction. The p-B(Si)N/SiC coatings were more uniform, less defective and of better quality than the BN/SiC or the p-BN/SiC coatings.