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Technology

In this session, Session WP3, the discussion focuses on the following topics: Monitoring Physiological Variables With Membrane Probes; Real Time Confocal Laser Scanning Microscopy, Potential Applications in Space Medicine and Cell Biology; Optimum Versus Universal Planetary and Interplanetary Habitats; Application of Remote Sensing and Geographic Information System Technologies to the Prevention of Diarrheal Diseases in Nigeria; A Small G Loading Human Centrifuge for Space Station ERA; Use of the Bicycle Ergometer on the International Space Station and Its Influence On The Microgravity Environment; Munich Space Chair (MSC) - A Next Generation Body Restraint System for Astronauts; and Thermoelectric Human-Body Cooling Units Used By NASA Space Shuttle Astronauts.

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Effects of a Tantalum Addition on the Morphological and Compositional Evolutions of a Model Ni-AL-Cr Superalloy

The effects of a 2.0 at.% addition of Ta to a model Ni-Al-Cr superalloy aged at 1073 K are assessed using scanning electron microscopy and atom-probe tomography. The addition of Ta results in appreciable strengthening, and the morphology is found to evolve from a bimodal distribution of spheroidal precipitates, to cuboidal precipitates aligned along the elastically soft <001>-type directions. Tantalum is observed to partition preferentially to the gamma -precipitate phase and decreases the mobility of Ni in the gamma- matrix sufficiently to cause an accumulation of Ni on the gamma-matrix side of the gamma -precipitate/gamma-matrix heterophase interface.

Booth-Morrison, Christopher

Effects of Tantalum on the Temporal Evolution of a Model Ni-Al-Cr Superalloy During Phase Decomposition

The effects of a 2.0 at.% addition of Ta to a model Ni-10.0Al-8.5Cr (at.%) superalloy aged at 1073 K are assessed using scanning electron microscopy and atom-probe tomography. The gamma'(Ll2)-precipitate morphology that develops as a result of gamma-(fcc)matrix phase decomposition is found to evolve from a bimodal distribution of spheroidal precipitates, to {001}-faceted cuboids and parallelepipeds aligned along the elastically soft {001}-type directions. The phase compositions and the widths of the gamma'-precipitate/gamma-matrix heterophase interfaces evolve temporally as the Ni-Al-Cr-Ta alloy undergoes quasi-stationary state coarsening after 1 h of aging. Tantalum is observed to partition preferentially to the gamma'-precipitate phase, and suppresses the mobility of Ni in the gamma-matrix sufficiently to cause an accumulation of Ni on the gamma-matrix side of the gamma'/gamma interface. Additionally, computational modeling, employing Thermo-Calc, Dictra and PrecipiCalc, is employed to elucidate the kinetic pathways that lead to phase decomposition in this concentrated Ni-Al-Cr-Ta alloy.

Booth, Morrison, Christopher

Using BEEM To Probe Strains In Semiconductors

Ballistic-electron-emission microscopy (BEEM) useful in determining strains in semiconductors under some conditions. More specifically, BEEM is variant of scanning tunneling microscopy and sensitive to electronic structure of probed material. In present approach, BEEM used to obtain data on those aspects of variations in electronic structures related to variations in strains. Then by use of mathematical modeling of relationships between electronic structures and strains, variations in strains deduced from BEEM data.

Bell, L. Douglas

X-Ray Diffraction and Reflectance Spectroscopy of Murchison Powders (CM2) After Thermal Analysis Under Reducing Conditions to Final Temperatures Between 300 and 1300°c

The asteroids Ryugu and Bennu have spectral characteristics in common with CI/CM type carbonaceous chondrites and are target bodies for JAXA’s Hayabusa2 and NASA’s OSIRIS-Rex missions, respectively. Analog studies, based primarily on the Murchison CM2 chondrite, provide a pathway to separate spectral properties resulting space weathering from those inherent to parent-body, mineralogy, chemistry, and processes. Ryugu shares spectral properties with thermally metamorphosed and partly dehydrated CI/CM chondrites. We have undertaken a multidisciplinary study of the thermal decomposition of Murchison powder samples as an analog to metamorphic process that may have occurred on Ryugu. Bulk analyses include thermal And evolved gas analysis, X-ray diffraction (XRD), and VIS-NIR and Mössbauer spectroscopy; micro- to nanoscale analyses included scanning and transmission electron microscopy and electron probe micro analysisWe report here XRD and VIS-NIR analyses of pre- and post-heated Murchison powders, and in a companion paper report results from multiple electron beam techniques.

Morris, R. V.

Mechanisms and Consequences of Intra-Crystalline Enrichment of Ancient Radiogenic Pb in Detrital Hadean Zircons from the Jack Hills, Western Australia

The recent discovery of Pb* (radiogenic lead) -enriched domains (PEDs) in zircon using high-resolution scanning ion imaging, atom probe tomography and transmission electron microscopy indicates that the U-Pb isotopic system in zircon can be affected not only by Pb* loss but also by intra-crystalline Pb* enrichment. However, the formation mechanism of PEDs and the consequences for in-situ U-Pb dating remain elusive. To further understand these issues, scanning ion imaging and U-Pb dating were carried out on 51 Hadean detrital zircon grains from the Jack Hills, Western Australia. Of these, 8 grains were found to contain micrometer-scale PEDs with elevated Pb-207 and Pb-206 in the ion images. Isotope profiles across these PEDs confirm that they represent unsupported Pb* resulting from intra-grain mobilization and local enrichment of Pb* during ancient overprinting events. The PEDs are rare in most grains, with only 1 – 3 Pb* hotspots present in any ~70 μm × 70 μm imaged area, and are located either in dark-CL, high-U growth zones, or associated with bright-CL, low-Th recrystallized domains, suggesting that they were likely formed by local-scale processes. The PEDs located in dark-CL, high-U growth zones likely resulted from Pb* trapped in local, interconnected pathways produced by radiation damage during thermal overprinting events. Those associated with bright-CL, low-Th domains are interpreted as Pb* concentrated in nanoscale pores formed during fluid-present recrystallization of non-metamict zircon. Our interpretations therefore imply that intra-crystalline enrichment of Pb* in zircon can occur at various scales and through diverse mechanisms. Age calculations based on the ion images demonstrate that incorporation of PEDs in conventional in-situ SIMS spots produces spuriously old ages that are either reversely discordant or concordant, depending on the time of Pb* mobilization and the analytical precision. The implication is that careful investigation of intra-grain distribution of U-Th-Pb isotopes is required in order to better understand the U-Pb isotopic system and to obtain reliable crystallization ages for ancient zircons affected by complex Pb* mobilization and redistribution.

Unsupported radiogenic lead

Particle impact and optical property analysis of the surfaces of Surveyor 3 materials

As part of the investigation of Surveyor 3 materials, a study was conducted to determine the effect of the lunar environment on some of the painted and unpainted exterior surfaces. Examination of the camera parts and tube sections was conducted using three techniques: (1) optical and scanning electron microscopy, (2) energy dispersive X-ray probe analysis, and (3) spectral reflectance measurements.

Anderson, D. L.

Australian Red Dune Sand: A Potential Martian Regolith Analog

To demonstrate the potential scientific and technical merits of in situ microscopy on Mars, we analyzed a possible Martian regolith analog - an acolian red dune sand from the central Australian desert (near Mt. Olga). This sand was chosen for its ubiquitous red coating and the desert environment in which is it found. Grains of this sand were analyzed using a variety of microanalytical techniques. A database of detailed studies of such terrestrial analogs would assist the study of geological and astrobiological specimens in future missions to Mars. Potential instrument concepts for in situ deployment on Mars include local electrode atom probe nanoanalysis (LEAP), vertical scanning white light interferometry (VSWLI), scanning electron microscopies, energy dispersive x-ray microanalysis (EDX), atomic force microscopy (AFM) and X-ray diffraction (XRD). While in situ deployment of these techniques is many years away, ground-based studies using these analytical techniques extend our understanding of the data obtained from instruments to be flown in the near future.

Kuhlman, K. R.

Solar wind and micrometeorite alteration of the lunar regolith

Developments in the understanding of reduction processes which occur in the lunar regolith as a result of solar-wind bombardment and micrometeorite impacts are discussed. The mechanism is described by which water released during reduction is removed from the lunar surface, and the possible contribution of solar-wind sputtering to the reduction process is considered. It is shown that the overall reduction efficiency of incoming hydrogen ions may reach several per cent, which is sufficient to produce all the metallic iron observed in the regolith. Mossbauer spectroscopic data on the amount of metallic iron present as isolated atoms or small clusters in reduced grain surfaces are presented together with data on the metallic iron content of fines samples obtained by Mossbauer spectroscopy, ferromagnetic resonance, and scanning as well as transmission electron microscopy. A portable magnetic probe is described which has been designed for determining surface-exposure age profiles in intact lunar core and drive-tube samples.

Housley, R. M.

KLASS: Kennedy Launch Academy Simulation System

Software provides access to many sophisticated scientific instrumentation (Scanning Electron Microscope (SEM), a Light Microscope, a Scanning Probe Microscope (covering Scanning Tunneling, Atomic Force, and Magnetic Force microscopy), and an Energy Dispersive Spectrometer for the SEM). Flash animation videos explain how each of the instruments work. Videos on how they are used at NASA and the sample preparation. Measuring and labeling tools provided with each instrument. Hands on experience of controlling the virtual instrument to conduct investigations, much like the real scientists at NASA do. Very open architecture. Open source on SourceForge. Extensive use of XML Target audience is high school and entry-level college students. "Many beginning students never get closer to an electron microscope than the photos in their textbooks. But anyone can get a sense of what the instrument can do by downloading this simulator from NASA's Kennedy Space Center." Science Magazine, April 8th, 2005

Garner, Lesley C.

Ballistic-Electron-Emission Microscopy Techniques for Nanometer-scale Characterization of Interfaces

Semiconductor interface properties are among the most important phenomena in materials science and technology. The study of metal/semiconductor Schottky barrier interfaces has been the primary focus of a large research and development community for decades. Throughout the long history of interface investigation, the study of interface defect electronic properties have been seriously hindered by the fundamental experimental difficulty of probing subsurface structures. A new method, Ballistic-Electron-Emission Microscopy (BEEM), has been developed which not only enables spectroscopic probing of subsurface interface properties, but also, provides nanometer-resolution imaging capabilities. BEEM employs Scanning Tunneling Microscopy (STM) and a unique spatially localized ballistic electron spectroscopy method...

Bell, L. D.

Spray CVD for Making Solar-Cell Absorber Layers

Spray chemical vapor deposition (spray CVD) processes of a special type have been investigated for use in making CuInS2 absorber layers of thin-film solar photovoltaic cells from either of two subclasses of precursor compounds: [(PBu3) 2Cu(SEt)2In(SEt)2] or [(PPh3)2Cu(SEt)2 In(SEt)2]. The CuInS2 films produced in the experiments have been characterized by x-ray diffraction, scanning electron microscopy, energy-dispersive spectroscopy, and four-point-probe electrical tests.

Banger, Kulbinder K.

Resonant difference-frequency atomic force ultrasonic microscope

A scanning probe microscope and methodology called resonant difference-frequency atomic force ultrasonic microscopy (RDF-AFUM), employs an ultrasonic wave launched from the bottom of a sample while the cantilever of an atomic force microscope, driven at a frequency differing from the ultrasonic frequency by one of the contact resonance frequencies of the cantilever, engages the sample top surface. The nonlinear mixing of the oscillating cantilever and the ultrasonic wave in the region defined by the cantilever tip-sample surface interaction force generates difference-frequency oscillations at the cantilever contact resonance. The resonance-enhanced difference-frequency signals are used to create images of nanoscale near-surface and subsurface features.

Cantrell, John H.

Quantative Measurements of Trace Elements and Three-Dimensional Atomic Scale Characterisation of Presolar O-rich Oxides and Silicates: An Atom Probe Tomography Approach

Presolar grains are recordsof a single moment in stellar evolution which have survived nebula and parent body processingwithin our Solar System. These grains condensed within a range of stellar envi-ronments including asymptotic giant branch stars, red giant branch stars, nova, supernova (SN) and hydrogen burning electron capture supernova(ECSN)[1,2]. Iso-topic and chemical compositions can be used to unravel details about environmental conditions at the time of their condensation and physical and chemical processes occurring at the time. For example,nucleosynthesis, stellar evolution, physical properties of stellar atmos-pheres, mixing from inner core to outer envelope, galac-tic chemical evolution, interstellar medium and parent body processing.NanoSIMS enables detailed characterisation of iso-topic compositions and rapid in situidentification of O-rich presolar oxides and silicates using their character-istic 17O/16O and 18O/16O isotopic ratios.Spectroscopic techniques e.g., auger spectroscopyand transmission electron microscopy, have provided additional details on major and minor chemical signatures. However, due tospatial resolution limitations,interaction volumes and interferencesfrom surrounding grains for in situtech-niques, attaining quantative characterisation of trace el-ements,hasproved challenging[1,3]. As the most sensitive geochemical tracers of envi-ronmental changes, trace elements are essential to un-ravelling the geochemical record of their parent stellar environments and evolutionary pathways[4].We car-ried out correlated in situisotopic and chemical analyses of 13 presolar grains to better understand stellar evolu-tion. In this work, we achieved this using a custom ap-proach, coordinating NanoSIMS, Scanning Electron Microscopy Energy Dispersive X-Ray Spectroscopy (SEM-EDX)and Atom Probe Tomography(APT).Our objective was to develop an approach which could ena-ble precise targeting of presolar grains for atom probe tomography and successfully execute atomic scale anal-yses of presolar oxides and silicates, to achieve quantative analysis of their trace elements for the first time.We also aimed to test the capability for Atom Probe tomography to measure isotopic compositions and stoichiometries of presolar oxide and silicate grains.

N D Nevill

Spatially resolved ballistic electron spectroscopy of subsurface interfaces

Buried interfaces have traditionally been inaccessible to direct investigation by surface-sensitive techniques. A unique and novel electronic probe, which is sensitive to subsurface electronic structure, has been utilized to probe Schottky barrier interfaces. The method, ballistic electron emission microscopy (BEEM), is based on scanning tunnelling microscopy (STM) techniques. A theoretical treatment has been developed to describe the ballistic electron spectra obtained by BEEM and this treatment is applied to data obtained on the Au-Si Schottky barrier interface system. Excellent agreement between experiment and theory is obtained. In addition, the treatment predicts nanometer spatial resolution for interface imaging by BEEM.

Bell, L. D.

Scanning Tunneling Optical Resonance Microscopy

Scanning tunneling optical resonance microscopy (STORM) is a method, now undergoing development, for measuring optoelectronic properties of materials and devices on the nanoscale by means of a combination of (1) traditional scanning tunneling microscopy (STM) with (2) tunable laser spectroscopy. In STORM, an STM tip probing a semiconductor is illuminated with modulated light at a wavelength in the visible-to-near-infrared range and the resulting photoenhancement of the tunneling current is measured as a function of the illuminating wavelength. The photoenhancement of tunneling current occurs when the laser photon energy is sufficient to excite charge carriers into the conduction band of the semiconductor. Figure 1 schematically depicts a proposed STORM apparatus. The light for illuminating the semiconductor specimen at the STM would be generated by a ring laser that would be tunable across the wavelength range of interest. The laser beam would be chopped by an achromatic liquid-crystal modulator. A polarization-maintaining optical fiber would couple the light to the tip/sample junction of a commercial STM. An STM can be operated in one of two modes: constant height or constant current. A STORM apparatus would be operated in the constant-current mode, in which the height of the tip relative to the specimen would be varied in order to keep the tunneling current constant. In this mode, a feedback control circuit adjusts the voltage applied to a piezoelectric actuator in the STM that adjusts the height of the STM tip to keep the tunneling current constant. The exponential relationship between the tunneling current and tip-to-sample distance makes it relatively easy to implement this mode of operation. The choice of method by which the photoenhanced portion of the tunneling current would be measured depends on choice of the frequency at which the input illumination would be modulated (chopped). If the frequency of modulation were low enough (typically < 10 Hz) that the feedback circuit could respond, then the voltage applied to the piezoelectric tip-height actuator could be measured by use of a lock-in amplifier locked to the modulation (chopping) signal. However, at a high modulation frequency (typically in the kilohertz range or higher), the feedback circuit would be unable to respond. In this case, the photoenhanced portion of the tunneling current could be measured directly. For this purpose, the tunneling current would be passed through a precise resistor and the voltage drop would be measured by use of the lock-in amplifier.

Bailey, Sheila

Analysis of a Memory Device Failure

The recent failure of a vintage memory device presented a unique challenge to failure analysts. Normally device layouts, fabrication parameters and other technical information were available to assist the analyst in the analysis. However, this device was out of production for many years and the manufacturer was no longer in business, so the information was not available. To further complicate this analysis, the package leads were all but removed making additional electrical testing difficult. Under these conditions, new and innovative methods were used to analyze the failure. The external visual exam, radiography, PIND, and leak testing were performed with nominal results. Since electrical testing was precluded by the short lead lengths, the device was delidded to expose the internal structures for microscopic examination. No failure mechanism was identified. The available electrical data suggested an ESD or low level EOS type mechanism which left no visible surface damage. Due to parallel electrical paths, electrical probing on the chip failed to locate the failure site. Two non-destructive Scanning Electron Microscopy techniques, CIVA (Charge Induced Voltage Alteration) and EBIC (Electron Beam Induced Current), and a liquid crystal decoration technique which detects localized heating were employed to aid in the analysis. CIVA and EBIC isolated two faults in the input circuitry, and the liquid crystal technique further localized two hot spots in regions on two input gates. Removal of the glassivation and metallization revealed multiple failure sites located in the gate oxide of two input transistors suggesting machine (testing) induced damage.

Nicolas, David P.