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At least 379 records · Page 21

Microstructural characterization of the HRSI thermal protection system for space shuttle

Components of the space shuttle high temperature reusable surface insulation (HRSI) system were microscopically characterized, both separately and as a system, to obtain information needed for stress analysis models of the thermal protection system. A tension specimen of the HRSI system was loaded in steps and was microscopically observed at each load condition to demonstrate the tension failure mode associated with strain isolation pad (SIP) behavior. A local failure occurred which should be associated with transfer of load through transverse fibers in the SIP. Stress concentrations attributed to the SIP behavior necessitated strengthening of the HRSI by densification of the RSI at the bondline. An HRSI tile was microscopically characterized after the densification process. The densified surface layer blended into the RSI which caused a gradual change in density. The gradation in density does not appear to represent a sharp discontinuity in elastic modulus between the densified layer and the parent material.

Ransone, P. O.↗

Towards Autonomous Experiments by Connecting High Performance Microscopy with High Performance Computing

The digitization of controls, data, and analysis in microscopy is bringing the idea of autonomous microscopes closer to reality than ever before. Automated transmission electron microscopy (TEM) is already fairly routine for some experiments the only require simple repetitive tasks such as imaging biological macromolecules for single particle cryoEM [1], tilt series for electron tomography [2], and movies for crystallography [3]. The vast majority of TEM experiments are conducted completely by human operators who choose the regions of interest, optimize experimental parameters, and make decisions about data quality visually during an experiment. The field is still a long way from having completely autonomous TEMs that can adapt to sample difficulties and tune experimental parameters based on data quality and desired experimental outcomes. Part of the issue is the lack of capability for feeding information learned from on-line, live data analysis back into the on-going experiment [4]. Furthermore, this presentation will discuss current capabilities for large scale data reduction and analysis using high performance computing (i.e. supercomputing) and progress towards developing a true feed-back loop that places data analysis and theory in the experimental loop.

97 MATHEMATICS AND COMPUTING↗

Readying advanced composites for the microscope

Concerns related to the proper preparation of composite specimens for microstructural analysis are examined. Proper preparation will minimize the amount of surface and subsurface damage at each stage of the procedure so that the microstructural features of the final-polished specimen can be accurately determined as a function of the composite's response to processing, testing, or service conditions. This requires that an optimum combination of abrasive type, size, and bond be applied during each grinding, lapping, and polishing step. Machine settings, such as polishing speed, force, and relative polishing direction, are also important. Guidelines are given for each step of the six-stage specimen preparation process: sectioning, planar grinding, sample integrity, polishing, and etching.

Zipperian, Donald C.↗

Digital image processing of bone - Problems and potentials

The development of a digital image processing system for bone histomorphometry and fluorescent marker monitoring is discussed. The system in question is capable of making measurements of UV or light microscope features on a video screen with either video or computer-generated images, and comprises a microscope, low-light-level video camera, video digitizer and display terminal, color monitor, and PDP 11/34 computer. Capabilities demonstrated in the analysis of an undecalcified rat tibia include the measurement of perimeter and total bone area, and the generation of microscope images, false color images, digitized images and contoured images for further analysis. Software development will be based on an existing software library, specifically the mini-VICAR system developed at JPL. It is noted that the potentials of the system in terms of speed and reliability far exceed any problems associated with hardware and software development.

Morey, E. R.↗

The MSP 2001 Mars Environmental Compatibility Assessment (MECA)

A chemical analysis of soil-water mixtures and the first microscopic images of martian soil will be among the results to be returned by the Mars Environmental Compatibility Assessment (MECA) payload on the Mars Surveyor Program 2001 Lander. Sponsored by the Human Exploration and Development of Space (HEDS) enterprise, MECA's primary goal is to evaluate potential geochemical and environmental hazards that may confront future martian explorers, and to guide HEDS scientists in the development of high fidelity Mars soil simulants. As a survey of soil properties, the MECA data set will also be rich in information relevant to basic geology, paleoclimate, and exobiology. The integrated MECA payload contains a wet-chemistry laboratory, a microscopy station, an electrometer to characterize the electrostatics of the soil and its environment, and arrays of material patches to study the abrasive and adhesive properties of soil grains. MECA is allocated a mass of 10 kg and a peak power usage of 15 W within an enclosure of 35 x 25 x 15 cm. The Wet Chemistry Laboratory (WCL) consists of four identical cells that will accept samples from surface and subsurface regions accessible to the Lander's robotic arm, mix them with water, and perform extensive analysis of the solution. Ion-selective electrodes and related sensors will evaluate total dissolved solids, redox potential, pH, and the concentration of many soluble ions and gases. Cyclic voltammetry will address oxidants, and anodic stripping voltammetry will probe potentially hazardous trace metals. MECA's microscopy station combines optical and atomic-force microscopy (AFM) in a controlled illumination environment to image dust and soil particles from millimeters to nanometers in size. Careful selection of substrates and an abrasion tool allows experimental study of size distribution, adhesion, abrasion, hardness, color, shape, aggregation, magnetic and other properties. Mounted on the end of the robot arm, MECA's electrometer consists of four types of sensors: an electric field meter, several triboelectricity monitors, an ion gauge, and a thermometer. Tempered only by ultra-violet- light-induced ions and a low-voltage break-down threshold, the dry, cold, dusty martian environment presents an imposing electrostatic hazard to both robots and humans. In addition, the electrostatic environment is key to transport of dust and, consequently, martian meteorology. MECA will also observe natural dust accumulation on engineering materials. Viewed with the robot arm camera, the abrasion and adhesion plates are strategically placed to allow direct observation of the inter-action between materials and soils on a macroscopic scale. Materials of graded hardness are placed directly under the robot arm scoop to sense wear and soil hardness. A second array, placed on the lander deck, is deployed after the dust plume of landing has settled. It can be manipulated in a primitive fashion by the arm, first having dirt deposited on it from the scoop and subsequently shaken clean. Dust accumulation as a function of conductivity, magnetic field strength, and other parameters will be explored. The MECA instruments described above will assess potential hazards that the Martian soil might present to human explorers and their equipment. In addition, MECA will provide information on the composition of ancient surface water environments, observing microscopic evidence of geological (and biological?) processes, inferring soil and dust transport, comminution and weathering mechanisms, and characterizing soil horizons that might be encountered during excavation. Additional information is contained in the original extended abstract.

Hecht, M. H.↗

Suppression of Helium Induced Cracking in Laser Repair Welding of Highly Irradiated Stainless Steels

Welding repair of irradiated nuclear reactor materials such as austenitic stainless steels used for the reactor internals has been challenging due to irradiation generated helium in the material matrix over an extended period of time. In this study, improved laser welding techniques, including the novel Auxiliary Beam Stress Improved (ABSI) technique that proactively manages the stresses during laser repair welding is investigated to substantially reduce or avoid the occurrence of intergranular helium-induced cracking (HeIC). Here, laser weld cladding, with and without ABSI technique, was applied to deposit weld metal on irradiated stainless steel (Type 304 L) blocks with various helium concentrations up to approximately 20 atomic parts per million (appm). Welded samples were cross-sectioned and analyzed using optical and electron microscopes. It was found that, with the improved laser welding techniques, no macroscopic (millimeter-sized) cracks were observed in any of the samples. Microscopic (less than 50 μm) cracks were present in the heat affected zone. Statistical analysis on the sample with the highest helium concentration (~20 appm) reveals that the ABSI technique could effectively reduce the size and amounts of microscopic cracks.

36 MATERIALS SCIENCE↗

Correlative SIP-FISH-Raman-SEM-NanoSIMS links identity, morphology, biochemistry, and physiology of environmental microbes

Microscopic and spectroscopic techniques are commonly applied to study microbial cells but are typically used on separate samples, resulting in population-level datasets that are integrated across different cells with little spatial resolution. To address this shortcoming, we developed a workflow that correlates several microscopic and spectroscopic techniques to generate an in depth analysis of individual cells. By combining stable isotope probing (SIP), fluorescence in situ hybridization (FISH), scanning electron microscopy (SEM), confocal Raman microspectroscopy (Raman), and nano-scale secondary ion mass spectrometry (NanoSIMS), we illustrate how individual cells can be thoroughly interrogated to obtain information about their taxonomic identity, structure, physiology, and metabolic activity. Analysis of an artificial community demonstrated that our correlative approach was able to resolve the activity of single cells using heavy water SIP in conjunction with Raman and/or NanoSIMS and establish their taxonomy and morphology using FISH and SEM. We then applied this workflow to a sample of yet uncultured multicellular magnetotactic bacteria. In addition to establishing their identity and activity, backscatter electron microscopy (BSE), NanoSIMS, and energy-dispersive X-ray spectroscopy (EDS) were employed to characterize the magnetosomes within the cells. By integrating these techniques, we demonstrate a cohesive approach to thoroughly study environmental microbes at single cell resolution.

Schaible, George↗

Unit-density SU(3) Fermi-Hubbard model with spin-flavor imbalance

The advent of ultracold alkaline-earth atoms in optical lattices has established a platform for investigating correlated quantum matter with SU⁡(𝑁) symmetry, offering highly tunable model parameters that allow experiments to access phenomena that are unavailable in conventional materials. Understanding the ground-state physics of SU⁡(𝑁) Fermi-Hubbard models away from the Heisenberg limit and from the spin-flavor balanced setting is important, as examining the flavor imbalance reveals new physics in Fermi-Hubbard models and shows how SU⁡(𝑁) phases react to practical experimental imperfections in optical lattices. Here, in this study, mean-field phase diagrams are presented for the unit-density SU(3) Fermi-Hubbard model at two sets of flavor densities, ($\frac{1}{3}$ − 𝛿, $\frac{1}{3}$ + 𝛿, $\frac{1}{3}$) and ($\frac{1}{4}$ − 𝛿, $\frac{1}{4}$ +𝛿, $\frac{1}{2}$), with the flavor imbalance introduced as 𝛿. Novel phases are identified at moderate interaction strengths for both densities, and their robustness is investigated in the presence of flavor imbalance. Furthermore, we provide microscopic explanations of the phases found and their stability. Analysis of thermal ensembles of random mean-field solutions indicate that, at temperatures accessible in state-of-the-art cold atom experiments, some spin orders are hard for conventional scattering or local observable measurements to detect, but can be more accessible with quantum gas microscopy in optical lattice experiments. This work also shows that nesting and Mottness, intertwined in the usual SU(2) Hubbard model in stark contrast to generic materials, can be tuned in the SU(3) model and play distinct roles. The resulting phase diagrams not only deepen our understanding of SU⁡(𝑁) Fermi-Hubbard models but also inform future experimental search for new phases.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Slow ferromagnetic fluctuations in the kagome metal Sc 3 ⁢ Mn 3 ⁢Al 7 ⁢ Si 5 revealed by 27 Al NMR

Static and dynamical magnetic and electronic properties of the kagome metal Sc 3 ⁢Mn 3 ⁢ Al 7⁢ Si 5 have been investigated by 27 Al nuclear magnetic resonance (NMR) measurements. Two distinct 27 Al -NMR signals with two different values of quadrupolar frequencies of 𝜈 Q = 1.55(2) and 1.07(2) MHz are observed, which are assigned to Al(1) and Al(2), respectively. From the detailed NMR spectrum measurements under three different magnetic field directions and the density functional theory calculations, the principal axes of the electric field gradient for each Al site have been determined. The temperature dependence of Knight shift (𝐾) shows a similar temperature dependence of the DC magnetic susceptibility 𝜒 except for the low-temperature region below ∼50 K where 𝐾 is almost constant while 𝜒 keeps increasing, which suggests that the increase in 𝜒 at low temperatures is not intrinsic. 27 Al spin-lattice relaxation rate divided by temperature (1/𝑇 1 ⁢𝑇) is found to be constant, confirming the metallic state of Sc 3 ⁢Mn 3 ⁢ Al 7⁢ Si 5 from a microscopic point of view. Based on a Korringa ratio analysis using the 𝑇 1 and 𝐾 data, ferromagnetic fluctuations are found to dominate in Sc 3 ⁢Mn 3 ⁢ Al 7⁢ Si 5 . In conclusion, these fluctuations are suggested to be very slow with frequencies on the order of kilohertz or lower.

Ding, Qing-Ping [Ames Laboratory (AMES), Ames, IA ↗

Electronic surface reconstruction of TiO 2 nanocrystals revealed by resonant inelastic x-ray scattering

The identification of lattice multiphases in TiO 2 nanocrystals is studied by high resolution transmission electron microscope and electron diffraction patterns. Based on the spectroscopic analysis using soft x-ray absorption and resonant inelastic soft x-ray scattering, it is believed that the oxygen vacancies at the interface exhibit structural distortion of the TiO$^{8-}_6$ cluster around the defect site as for the multiphase lattice. We elucidate that the extra 3d electrons nearby induce the inelastic scattering features with the excitation energy dependence owing to different energy relaxation processes, a characteristic of the electron-phonon coupling or the nature of the electron-hole pair at the intermediate state. The manifold dd excitations driven by the strong interaction between Ti-3d and O-2p electrons are noticeably rich, coexisting on both Ti and O sites. Finally, this sophisticated experiment can advance the perspective of nanocomposite TiO 2 for various interactions of surface Ti 3+ in applications of future devices.

36 MATERIALS SCIENCE↗

Preliminary results from the noctilucent sampling from Kiruna in 1970.

On Aug. 8, 1970 at 0148 and 0354 local time, two Pandora sounding rocket payloads were launched from the ESRO range in Kiruna, Sweden, during a noctilucent cloud display. Large numbers of particles were collected, many of which appear to be micrometeorites coated with a low density material. Typical electron micrographs are shown, and numerical densities as a function of altitude are given. Particle composition information has been obtained by use of dispersive X-ray analysis equipment attached to our Philips EM 300 electron microscope.

Hallgren, D. S.↗

Tibial changes in experimental disuse osteoporosis in the monkey

The mechanical properties and structural changes in the monkey tibia with disuse osteoporosis and during subsequent recovery are investigated. Bone mending stiffness is evaluated in relation to microscopic changes in cortical bone and Norland bone mineral analysis. Restraint in the semireclined position is found to produce regional losses of bone most obviously in the anterior-proximal tibiae. After six months of restraint, the greatest losses of bone mineral in the proximal tibiae range from 23 percent to 31 percent; the largest changes in bone stiffness range from 36 percent to 40 percent. Approximately eight and one-half months of recovery are required to restore the normal bending properties. Even after 15 months of recovery, however, the bone mineral content does not necessarily return to normal levels. Histologically, resorption cavities in cortical bone are seen within one month of restraint; by two and one-half months of restraint there are large resorption cavities subperiosteally, endosteally, and intracortically. After 15 months of recovery, the cortex consists mainly of first-generation haversian systems. After 40 months, the cortex appears normal, with numerous secondary and tertiary generations of haversian systems.

Young, D. R.↗

Separating Peaks in X-Ray Spectra

Deconvolution algorithm assists in analysis of x-ray spectra from scanning electron microscopes, electron microprobe analyzers, x-ray fluorescence spectrometers, and like. New algorithm automatically deconvolves x-ray spectrum, identifies locations of spectral peaks, and selects chemical elements most likely producing peaks. Technique based on similarities between zero- and second-order terms of Taylor-series expansions of Gaussian distribution and of damped sinusoid. Principal advantage of algorithm: no requirement to adjust weighting factors or other parameters when analyzing general x-ray spectra.

Nicolas, David↗

The trace element chemistry of CaS in enstatite chondrites and some implications regarding its origin

The trace element distribution in oldhamite (CaS) extracted from enstatite chondrites was determined by INAA. Prior to extraction, the petrologic setting of the grains was studied microscopically, and their minor element contents determined by microprobe analysis; samples that displayed a wide range of minor element contents were selected for detailed elementary analysis. Those samples of CaS suspected to be more primitive on the basis of their minor element and petrologic siting contain the entire inventory of the host meteorite's light REE (LREE) and Eu, plus 30-50 percent of the heavy-REE inventory. In less primitive samples, the LREE are less enriched although Eu remains highly concentrated. Several other elements, including lithophiles and chalcophiles, are most enriched in the most primitive CaS. It is suggested that oldhamite played a key role in the redistribution of these elements during the metamorphism and evolution of enstatite-rich material.

Larimer, John W.↗

Chemical compatibility of cartridge materials

This twelve month progress report deals with the chemical compatibility of semiconductor crystals grown in zero gravity. Specifically, it studies the chemical compatibility between TZM, a molybdenum alloy containing titanium and zirconium, and WC 103, a titanium alloy containing Niobium and Hafnium, and Gallium arsenide (GaAs) and Cadmium Zinc Tellurite (CdZnTe). Due to the health hazards involved, three approaches were used to study the chemical compatibility between the semiconductor and cartridge materials: reaction retort, thermogravimetric analysis, and bulk cylindrical cartridge containers. A scanning electron microscope with an energy dispersive X-ray analyzer was used to examine all samples after testing. The first conclusion drawn is that reaction rates with TZM were not nearly as great as they were with WC 103. Second, the total reaction between GaAs and WC 103 was almost twice that with TZM. Therefore, even though WC 103 is easier to fabricate, at least half of the cartridge thickness will be degraded if contact is made with one of the semiconductor materials leading to a loss of strength properties.

Wilcox, Roy C.↗

Soot and Sulfuric Acid from Aircraft: Is There Enough to Cause Detrimental Environmental E-kCTSs?

Aerosol from aircraft can affect the environment in three ways: First, soot aerosol has been implicated to cause Icing-tern ozone depletion at mid-latitudes in the lower stratosphere at a rate of approx. 5% per decade. This effect is in addition and unrelated to the polar ozone holes which are strongly influenced by heterogeneous chemistry on polar stratospheric clouds. Second, the most obvious effect of jet aircraft is the formation of visible contrails in the upper troposphere. The Salt Lake City region experienced an 8% increase in cirrus cloud cover over a 15-year period which covariates with an increase in regional commercial air traffic. If soot particles act as freezing nuclei to cause contrail formation heterogeneously, they would be linked to a secondary effect to cloud modification that very likely is climatologically important. Third, a buildup of soot aerosol could reduce the single scatter albedo of stratospheric aerosol from 0.993+0.004 to 0.98, a critical value that has been postulated to separate stratospheric cooling from warming. Thus arises an important question: Do aircraft emit sufficient amounts of soot to have detrimental effects and warrant emission controls? During the 1996 SUCCESS field campaign, we sampled aerosols in the exhaust wake of a Boeing 757 aircraft and determined emission indices for sulfuric acid (EI(sub H2SO4) = 9.0E-2 and 5.0E-1 g/kg (sub FUEL) for 75 and 675 ppm fuel-sulfur, respectively) and soot aerosol (2.2E-3 less than EI(sub SOOT) = l.lE-2 g/kg (sub FUEL)). The soot particle analysis accounted for their fractal nature, determined electron-microscopically, which enhanced the surface area by a factor of 26 and the volume 11-fold over equivalent-volume spheres. The corresponding fuel-sulfur to H2SO4 conversion efficiency was 10% (for 675 ppmm fuel-S) and 37% (for 75 ppmm fuel-S). Applying the H2SO4 emission index to the 1990 fuel use by the worlds commercial fleets of 1.3E11 kg, a conversion efficiency of 30% of 500 ppmm fuel-S would have led to an annual contribution to the atmospheric sulfur budget by aircraft of 2.E7 kg H2SO4. This is about one part in 1.E4 of anthropogenic sulfate from other sources. The soot emission index given above yielded a 1990 injection of soot aerosol by aircraft of 1.E6 kg. Thus, soot amounts to only five percent of the aerosol generated by aircraft. Its reactivity with ozone would have to be 20 times that of sulfuric acid particles to make it chemically significant. Nevertheless, the findings, of stratospheric soot loadings commensurate with aircraft fuel consumption, based on the emission index given above and the assumption of stratospheric residence times of the order of one year implicate aircraft as stratospheric polluters. A trend similar to soot of H2SO4 aerosol loading could not be deciphered, neither from in situ measurements nor SAGE II satellite extinction, against the "noise" due to volcanic eruptions. Observation of soot particles at 20 km altitude which, if emitted by aircraft were generated at 10-12 km altitude, suggests a displacement of those particles against gravity. Because eddy mixing is virtually absent in the lower stratosphere and isentropic mixing explains lofting to only about 15 km, radiometric forces acting on morphologically and chemically asymmetric soot particles must be considered a possibility. The consequence could be an extended residence time of soot against that of sulfuric acid aerosol that would lower the single scatter albedo with time.

Pueschel, R. F.↗

Comprehensive Micromechanics-Analysis Code - Version 4.0

Version 4.0 of the Micromechanics Analysis Code With Generalized Method of Cells (MAC/GMC) has been developed as an improved means of computational simulation of advanced composite materials. The previous version of MAC/GMC was described in "Comprehensive Micromechanics-Analysis Code" (LEW-16870), NASA Tech Briefs, Vol. 24, No. 6 (June 2000), page 38. To recapitulate: MAC/GMC is a computer program that predicts the elastic and inelastic thermomechanical responses of continuous and discontinuous composite materials with arbitrary internal microstructures and reinforcement shapes. The predictive capability of MAC/GMC rests on a model known as the generalized method of cells (GMC) - a continuum-based model of micromechanics that provides closed-form expressions for the macroscopic response of a composite material in terms of the properties, sizes, shapes, and responses of the individual constituents or phases that make up the material. Enhancements in version 4.0 include a capability for modeling thermomechanically and electromagnetically coupled ("smart") materials; a more-accurate (high-fidelity) version of the GMC; a capability to simulate discontinuous plies within a laminate; additional constitutive models of materials; expanded yield-surface-analysis capabilities; and expanded failure-analysis and life-prediction capabilities on both the microscopic and macroscopic scales.

Arnold, S. M.↗

Method and system for near-field spectroscopy using targeted deposition of nanoparticles

There is provided in one embodiment of the invention a method for analyzing a sample material using surface enhanced spectroscopy. The method comprises the steps of imaging the sample material with an atomic force microscope (AFM) to select an area of interest for analysis, depositing nanoparticles onto the area of interest with an AFM tip, illuminating the deposited nanoparticles with a spectrometer excitation beam, and disengaging the AFM tip and acquiring a localized surface enhanced spectrum. The method may further comprise the step of using the AFM tip to modulate the spectrometer excitation beam above the deposited nanoparticles to obtain improved sensitivity data and higher spatial resolution data from the sample material. The invention further comprises in one embodiment a system for analyzing a sample material using surface enhanced spectroscopy.

Anderson, Mark S.↗