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NASA NTRS1992

Applications of the Analytical Electron Microscope to Materials Science

In the last 20 years, the analytical electron microscope (AEM) as allowed investigators to obtain chemical and structural information from less than 50 nanometer diameter regions in thin samples of materials and to explore problems where reactions occur at boundaries and interfaces or within small particles or phases in bulk samples. Examples of the application of the AEM to materials science problems are presented in this paper and demonstrate the usefulness and the future potential of this instrument.

Goldstein, J. I.↗

NASA NTRS1995

Technologies and Designs for Electronic Nanocomputers

Diverse space-related applications have been proposed for microscopic and sub-microscopic structures, mechanisms, and 'organisms'. To govern their functions, many of these tiny systems will require even smaller, nanometer-scale programmable computers, i.e. 'nanocomputers' on-board. This paper provides an overview of the results of a nearly two-year study of the technologies and designs that presently are in development for electronic nanocomputers. Strengths and weaknesses of the various technologies and designs are discussed, as well as promising directions for remedying some of the present research issues in this area. The presentation is a synopsis of a longer MITRE review article on the same subject.

Montemerlo, Michael S.↗

NASA NTRS1995

Laser Material Processing for Microengineering Applications

The processing of materials via laser irradiation is presented in a brief survey. Various techniques currently used in laser processing are outlined and the significance to the development of space qualified microinstrumentation are identified. In general the laser processing technique permits the transferring of patterns (i.e. lithography), machining (i.e. with nanometer precision), material deposition (e.g., metals, dielectrics), the removal of contaminants/debris/passivation layers and the ability to provide process control through spectroscopy.

Helvajian, H.↗

NASA NTRS1996

Application of Phase Shifted, Laser Feedback Interferometry to Fluid Physics

We have combined the principles of phase-shifting interferometry (PSI) and laser-feedback interferometry (LFI) to produce a new instrument that can measure both optical path length (OPL) changes and discern sample reflectivity variations. In LFI, coherent feedback of the incident light either reflected directly from a surface or reflected after transmission through a region of interest will modulate the output intensity of the laser. LFI can yield a high signal-to-noise ratio even for low reflectivity samples. By combining PSI and LFI, we have produced a robust instrument, based upon a HeNe laser, with high dynamic range that can be used to measure either static (dc) or oscillatory changes along the optical path. As with other forms of interferometry, large changes in OPL require phase unwrapping. Conversely, small phase changes are limited by the fraction of a fringe that can be measured. We introduce the phase shifts with an electro-optic modulator (EOM) and use either the Carre or Hariharan algorithms to determine the phase and visibility. We have determined the accuracy and precision of our technique by measuring both the bending of a cantilevered piezoelectric bimorph and linear ramps to the EOM. Using PSI, sub-nanometer displacements can be measured. We have combined our interferometer with a commercial microscope and scanning piezoelectric stage and have measured the variation in OPL and visibility for drops of PDMS (silicone oil) on coated single crystal silicon. Our measurement of the static contact angle agrees with the value of 68 deg stated in the literature.

Ovryn, Ben↗

NASA NTRS1997

Combustion of PTFE: The Effects of Gravity and Pigmentation on Ultrafine Particle Generation

Ultrafine particles generated during polymer thermodegradation are a major health hazard, owing to their unique pathway of processing in the lung. This hazard in manned spacecraft is poorly understood, because the particulate products of polymer thermodegradation are generated under low gravity conditions. Particulate generated from the degradation of PolyTetraFluoroEthylene (PTFE), insulation coating for 20 AWG copper wire (representative of spacecraft application) under intense ohmic heating were studied in terrestrial gravity and microgravity. Microgravity tests were done in a 1.2-second drop tower at the Colorado School of Mines (CSM). Thermophoretic sampling was used for particulate collection. Transmission Electron Microscopy (TEM) and Scanning Transmission Electron Microscopy (STEM) were used to examine the smoke particulates. Image software was used to calculate particle size distribution. In addition to gravity, the color of PTFE insulation has an overwhelming effect on size, shape and morphology of the particulate. Nanometer-sized primary particles were found in all cases, and aggregation and size distribution was dependent on both color and gravity; higher aggregation occurred in low gravity. Particulates from white, black, red and yellow colored PTFE insulations were studied. Elemental analysis of the particulates shows the presence of inorganic pigments.

McKinnon, J. Thomas↗

NASA NTRS1997

Space Environmental Effects on Thermal Control Coatings

The study of long term near ultra-violet (NUV) effects in a vacuum atmosphere, is a crucial element for space applications. NUV radiation causes significant changes in the reflectance of many coatings and types of materials. An ultra high vacuum NUV system was assembled in order to investigate various coatings and materials in this hostile environment. The vacuum is an ion pump that maintains a minimum vacuum in the mid 10(exp -9) range. The system has a base pressure of 10(exp -9) torr and this base pressure is maintained with the ion pump. The NUV exposure was maintained at 2-3 suns which allows accelerated NUV exposure without overheating the samples. The goal of this test was to maintain an intensity of 3.4 x 10(exp -2) Watts/cm(exp 2) which equals 2.9 NUV suns. An NUV sun is defined as 1.16 Watts/cm(exp 2) integrated over wavelength of 200-400 nanometers.

OBrien, Susan K.↗

NASA NTRS1998

New AFM Techniques for Investigating Molecular Growth Mechanisms of Protein Crystals

Atomic Force Microscopy (AFM) has emerged as a powerful technique for investigating protein crystal growth. Earlier AFM studies were among the first to demonstrate that these crystals grew by dislocation and 2D nucleation growth mechanisms [1]. These investigations were restricted to the micron range where only surface features, such as dislocation hillocks and 2D islands are visible. Most AFM instruments can scan at higher resolutions and have the potential to resolve individual protein molecules at nanometer ranges. Such scans are essential for determining the molecular packing arrangements on crystal faces and for probing the growth process at the molecular level. However, at this resolution the AFM tip influences the image produced, with the resulting image being a convolution of the tip shape and the surface morphology [2]. In most studies this problem is resolved by deconvoluting the image to obtain the true surface morphology. Although deconvolution routines work reasonably well for simple one- dimensional shapes, for complex surfaces this approach does not produce accurate results. In this study we devised a new approach which takes advantage of the precise molecular order of crystal surfaces, combined with the knowledge of individual molecular shapes from the crystallographic data of the protein and the AFM tip shape. This information is used to construct expected theoretical AFM images by convoluting the tip shape with the constructed crystal surface shape for a given surface packing arrangement. By comparing the images from actual AFM scans with the constructed ones for different possible surface packing arrangements, the correct packing arrangement can be conclusively determined. This approach was used in this study to determine the correct one from two possible packing arrangements on (I 10) faces of tetragonal lysozyme crystals. Another novel AFM technique was also devised to measure the dimension of individual growth units of the crystal faces. Measuring these units was not attempted before and most studies have assumed that the growth unit consisted of individual protein molecules. The linescan mode of AFM instruments allows the crystal surface to be scanned along a single line. By scanning across a growth step an image showing the motion of the step is obtained. Normally such an image shows a straight line for continuous and constant step velocity. In this study by increasing the scan rate and by decreasing the step velocity (by decreasing the supersaturation), we were able to capture images of individual growth events, shown by jump discontinuities in the step line. By suitable integration of the image the growth unit dimension in the scanned direction can be obtained. Since multiple units can be involved in the growth process it is necessary to collect a statistically relevant sample before drawing conclusions about the growth mechanism. This technique was successfully employed to obtain the dimensions of growth units for the (110) face, showing that they consisted of various aggregates corresponding to the 43 helices in the crystal structure.

Li, Huayu↗

NASA NTRS1989

Control Structures Interaction (CSI) Technology

Control Structures Interaction (CSI) technology for control of space structures is being developed cooperatively by JPL, LaRC and MSFC for NASA OAST/RM. The mid-'90s goal of JPL's CSI program is to demonstrate with analysis, ground and flight tests, the super quiet structures needed for large diffraction-limited instruments such as optical stellar interferometers and large advanced successors to the Hubble Space Telescope. Microprecision CSI technology is intended as a new "building block" for use by the designers of large optical systems. The thrust of the microprecision CSI technology effort is to achieve nanometer-levels of space structure stability/accuracy with designs which employ otherwise conventional spacecraft technologies. JPL design experiences have indicated the following CSI technology development areas are especially applicable to large optical system projects: (1) Active structural members; (2) Control/structures design methods; (3) Microdynamic effects characterization; and (4) Ground and flight test validation of CSI methods.

Layman, W. E.↗

NASA NTRS1996

Stress Determination of Micromembranes Using Laser Vibrometry

A laser vibrometry based dynamic technique for biaxial residual stress determination in micromembranes is reported. Layered, low pressure chemical vapor deposition grown, rectangular shaped micromembranes are ultrasonically excited. The resulting micromembrane displacement, as a function of frequency and position, is recorded to yield resonance frequencies and associated vibrational mode numbers. The stress is determined from this information. Vibrations forced from ultrasonic pressure (-25 Pa) resulted in peak displacements of tens of nanometers at resonance. For the sample set studied, the (3,1) mode resonance peak displayed the least damping in atmospheric testing and was used to establish stress levels approximately 10(exp 8)N/m2 . A trend for this stress showing an overall decrease by approximately 40% as a result of thermomechanical cycling was identified.

Biswas, Abhijit↗

NASA NTRS1998

Biomarkers in Carbonate Thermal Springs: Implications for Mars

Evidence of possible relict biogenic activity has been reported in carbonate inclusions within martian meteorite ALH 84001. The initial evidence included ovoid and elongated forms 50 - 500 nanometers in length, morphologically similar to but significantly smaller than many terrestrial microbes. More recently, thin structures resembling the remains of organic biofilms have been reported in the same meteorite. Carbonates have also been discussed in the context of Mars sample return missions. Thermal spring deposits have often been cited as prime locations for exobiological exploration. By analogy to Earth, specialized microbes may have existed in the heated, mineralized waters, and precipitates of carbonate and/or silica from these waters may have trapped and preserved evidence of life. Since the geological interactions that produce thermal springs can be recognized in orbital imagery, directed searches for microfossils in such deposits are deemed possible. We are engaged in a study of the signatures produced by contemporary biogenic activity (biomarkers) in carbonate thermal springs. We are examining the microbes that live in such environments and the preservation of microbial forms, biofilms, and petrographic fabrics indicative of life in thermal spring mineral deposits. This work is part of a much more extensive study to refine the appropriate tools, techniques, and approaches to seek evidence of life in a range of planetary samples. A deeper understanding of biological signatures will prepare us for the detailed search for life on Mars and eventually on other planets. Overall. the study of biomarkers in rocks and soils will provide insight into the evolution of life because such signatures are a record of how life interacts with its environment, how it adapts to changing conditions, and how life can influence geology and climate.

Allen, C. C.↗

NASA NTRS1999

Ozone Depletion, UVB and Atmospheric Chemistry

The primary constituents of the Earth's atmosphere are molecular nitrogen and molecular oxygen. Ozone is created when ultraviolet light from the sun photodissociates molecular oxygen into two oxygen atoms. The oxygen atoms undergo many collisions but eventually combine with a molecular oxygen to form ozone (O3). The ozone molecules absorb ultraviolet solar radiation, primarily in the wavelength region between 200 and 300 nanometers, resulting in the dissociation of ozone back into atomic oxygen and molecular oxygen. The oxygen atom reattaches to an O2 molecule, reforming ozone which can then absorb another ultraviolet photon. This sequence goes back and forth between atomic oxygen and ozone, each time absorbing a uv photon, until the oxygen atom collides with and ozone molecule to reform two oxygen molecules.

Stolarski, Richard S.↗

NASA NTRS1999

Ozone Depletion, UVB and Atmospheric Chemistry

Stolarski, Richard S.↗

NASA NTRS1996

Solar Electromagnetic Radiation Study for Solar Cycle 22: Solar Ultraviolet Irradiance, 120 to 300 NM: Report of Working Groups 2 and 3 of SOLERS 22

This report summarizes the activities of Working Group 2 and Working Group 3 of the SOLax Electromagnetic Radiation Study for Solar Cycle 22 (SOLERS22) Program. The international (SOLERS22) is Project 1.2 of the Solar-Terrestrial Energy Program (STEP) sponsored by SCOSTEP, a committee of the International Council of Scientific Unions). SOLERS22 is comprised of five Working Groups, each concentrating on a specific wave-length range: WG-1 - visible and infrared, WG-2 - mid-ultraviolet (200 < A < 300 nm), WG-3 - Far-ultraviolet (lambda greater than 100 and lambda less than 200 nanometers), WG-4 - extreme-ultraviolet (lambda greater than 10 and lambda less than 100 nm), and WG-5 - X-ray (lambda greater than 1 and lambda less than 10 nano meters). The overarching goals of SOLERS22 are to: 1) establish daily solar irradiance values in the specified wavelength ranges, 2) consider the evolving solar structures as the cause of temporal variations, and 3) understand the underlying physical processes driving these changes.

Rottman, G. J.↗

NASA NTRS1998

Estimates of Spectral UV Irradiance from Earth Probe TOMS: Comparisons with Ground-Based Measurements

Estimates of the spectral UV flux incident on the Earth's surface are calculated based on total column ozone and cloud optical thickness determined from the Earth Probe Total Ozone Mapping Spectrometer (TOMS) satellite data. Spectral fluxes are calculated between 300 and 325 nanometers using a weighting function similar to the measured function of the Brewer Spectrophotometer. Comparisons of the TOMS-derived values with ground-based Brewer Spectrophotometer measurements at 3 locations from the Canadian Brewer network (Toronto, Saskatoon and Saturna Island) and 3 locations from the United States EPA network (Boston, Gaithersburg, and Boulder) show reasonably good agreement over a variety of clear and cloudy conditions. Some systematic differences are apparent, particularly when snow/ice is present and the TOMS instrument cannot distinguish between clouds and snow covered ground, thus leading to an underestimation of UV flux. The presence of absorbing aerosols near the ground or sub-pixel clouds can also lead to significant errors. There are also possible errors in the Brewer data due to radiometric calibration uncertainties and uncorrected cosine response.

Labow, G. J.↗

NASA NTRS1999

Monte Carlo Simulation of Nanoparticle Encapsulation in Flames

Gas-phase combustion (flame) synthesis has been an essential industrial process for producing large quantities of powder materials such as carbon black, titanium dioxide, and silicon dioxide. Flames typically produce simple oxides, with carbon black being the noted exception because the oxides of carbon are gaseous and are easily separated from the particulate matter that is formed during fuel pyrolysis. Furthermore, the powders produced in flames are usually agglomerated, nanometer-sized particles (nanoparticles). This composition and morphology is acceptable for many applications. However, the present interest in nanoparticles for advanced materials application has led to efforts to employ flames for the synthesis of unagglomerated nanoparticles (2 to 100 nm) of metals and non-oxide ceramics. Sodium-halide chemistry has proven to be viable for producing metals and non-oxide ceramics in flames. Materials that have been produced to date include Si (Calcote and Felder, 1993), TiN, TiB2, TiC, TiSi2, SiC, B4C (Glassman et al, 1993) Al, W, Ti, TiB2, AlN, and W-Ti and Al-AlN composites (DuFaux and Axelbaum, 1995, Axelbaum et al 1996,1997). Many more materials are possible. The main challenge that faces application of flame synthesis for advanced materials is overcoming formation of agglomerates in flames (Brezinsky, 1997). The high temperatures and high number densities in the flame environment favor the formation of agglomerates. Agglomerates must be avoided for many reasons. For example, when nanopowders are consolidated, agglomerates have a deleterious effect on compaction density, leading to voids in the final part. Efforts to avoid agglomeration in flames without substantially reducing particle number density and, consequently, production rate, have had limited success. Another critical challenge that faces all synthesis routes for nanopowders is ensuring that the powders are high purity and that the process is scaleable. Though the containerless, high temperature environment of a flame is excellent for producing high-purity simple compounds, ultrafine metals and non-oxide ceramic powders are inherently reactive in the presence of oxygen and/or moisture. Thus, the handling of these powders after synthesis poses a challenging problem. Impurities acquired during handling of nanoparticles have plagued the advancement of nanostructured materials technology.

Sun, Z.↗

NASA NTRS1999

The Mars Environmental Compatibility Assessment (MECA)

Meloy, Thomas P.↗

NASA NTRS1999

Mars Environmental Compatibility Assessment (MECA): Identifying the Hazards of the Martian Soil

Sometime in the next decade NASA will decide whether to send a human expedition to explore the planet Mars. The Mars Environmental Compatibility Assessment (MECA) has been selected by NASA to evaluate the Martian environment for soil and dust hazards to human exploration. The integrated MECA payload contains three elements: a wet-chemistry laboratory, a microscopy station, and enhancements to a lander robot-arm system incorporating arrays of material patches and an electrometer to identify triboelectric charging during soil excavation. The wet-chemistry laboratory will evaluate samples of Martian soil in water to determine the total dissolved solids, redox potential, pH, and quantify the concentration of many soluble ions using ion-selective electrodes. These electrodes can detect potentially dangerous heavy-metal ions, emitted pathogenic gases, and the soil's corrosive potential. MECA's microscopy station combines optical and atomic-force microscopy with a robot-arm camera to provide imaging over nine orders of magnitude, from meters to nanometers. Soil particle properties including size, shape, color, hardness, adhesive potential (electrostatic and magnetic), will be determined on the microscope stage using an ar-ray of sample receptacles and collection substrates, and an abrasion tool,. The simple, rugged atomic-force microscope will image in the submicron size range and has the capability of performing a particle-by-particle analysis of the dust and soil. Although selected by NASA's Human Exploration and Development of Space Enterprise, the MECA instrument suite also has the capability to address basic geology, paleoclimate, and exobiology issues. To understand both contemporaneous and ancient processes on Mars, the mineralogical, petrological, and reactivity of Martian surface materials should be constrained: the NMCA experiment will shed light on these quantities through its combination of chemistry and microscopy. On Earth, the earliest forms of life are preserved as microfossils. The atomic-force microscope will have the required resolution to image down to the scale of terrestrial microfossils and beyond.

Meloy, T. P.↗

NASA NTRS1999

The MSP 2001 Mars Environmental Compatibility Assessment (MECA)

The Mars Environmental Compatibility Assessment (MECA) will evaluate the Martian environment for soil and dust-related hazards to human exploration as part of the Mars Surveyor Program 2001 Lander. Sponsored by the Human Exploration and Development of Space (HEDS) enterprise, MECA's 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. 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. The instrument will acquire soil samples with a robotic arm equipped with a camera. MECA will examine surface and subsurface soil and dust in order to characterize particle size, shape, hardness, and also physical characteristics that may provide clues to mineralogy. MECA will characterize soil/water mixtures with respect to pH, redox potential, total dissolved ions, and trace toxins. MECA will determine the nature of electrostatic charging associated with excavation of soil, and the influence of ionizing radiation on material properties. It will also observe natural dust accumulation on engineering materials. To accomplish these objectives, MECA is allocated a mass of 10 kg 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 in wet Martian soil. These electrodes can detect potentially dangerous heavy-metal ions, emitted pathogenic gases, and the soil's corrosive potential. Experiments will include cyclic voltammetry and anodic stripping voltammetry. Complementary to the Viking experiments, the chemical laboratory will characterize the water-soil solution rather than emitted gases. Nonetheless, through analysis of dissolved gases it will be able to replicate many of the Viking observations related to oxidants. MECA's microscopy station combines optical and atomic-force microscopy (AFM) in an actively focused, controlled illumination environment to image particles from millimeters to nanometers in size. Careful selection of substrates allows controlled experiments in adhesion, abrasion, hardness, aggregation, magnetic and other properties. Special tools allow primitive manipulation (brushing and scraping) of samples. Soil particle properties including size, shape, color, hardness, adhesive potential (electrostatic and magnetic), will be determined using an array of sample receptacles and collection substrates. The simple, rugged atomic-force microscope will image in the submicron size range and has the capability of performing a particle-by-particle analysis of the dust and soil. On Earth, the earliest forms of life are preserved as microfossils. The atomic-force microscope will have the required resolution to image down to the scale of terrestrial microfossils and beyond. Mounted on the end of the robot arm, MECA's electrometer actually consists of four types of sensors: an electric field meter, several triboelectricity monitors, an ion gauge, and a thermometer. Tempered only by ultraviolet-light-induced ions and a low-voltage breakdown threshold, the dry, cold, dusty martian environment presents an imposing electrostatic hazard to both robots and humans. The field meter will measure the ambient field on nearby objects while the triboelectric sensors, using identical circuitry, will measure the charge accumulated on test substances as they are dragged through the soil by the arm. The ion chamber, open to the environment, will sense both charged dust and free ions in the air. Over and above the potential threat to electronics, the electrostatic environment holds one of the keys to transport of dust and, consequently, Martian meteorology. Viewed with the robot arm camera, the abrasion and adhesion plates are strategically placed to allow direct observation of the interaction 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. A third array will passively collect dust from the atmosphere. In addition to objectives related to human exploration, the MECA data set will be rich in information relevant to basic geology, paleoclimate, and exobiology issues. To understand both contemporaneous and ancient processes on Mars, the mineralogy, petrology, and reactivity of Martian surface materials should be constrained. The MECA experiment will shed light on these quantities through its combination of chemistry and microscopy. MECA will be capable of measuring 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.

Hecht, M. H.↗