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At least 127 records · Page 7

An e.s.c.a. study of atomic oxygen interactions with phosphazene-coated polyimide films

Metallic as well as most nonmetallic materials experience oxidation and mass loss via surface erosion in low earth orbit as shown in previous Space Shuttle flights. This study is an evaluation of select polyphosphazene polymers and their resistance to atomic oxygen attack. Electron spectroscopy for chemical analysis examinations of the surfaces of polyphosphazene coatings were monitored for microstructural changes induced during exposures to atomic oxygen. Sample exposures in oxygen plasmas and O(3P) beam were compared as to their effect on surface compositional changes in the polyphosphazene coating. High resolution line scans revealed rearrangements in the polymer backbone and scissioning reactions involving fluorocarbon units of long chain fluoroalkoxy pendant groups. Atom percents and peak areas of all species provided a detailed profile of the microstructural changes induced in phosphazene polymers as a result of exposures to atomic oxygen.

Fewell, Larry L.↗

Hot tensile properties and deformation response of a gamma/Ni/-gamma prime/Ni3Al/-delta/Ni3Nb/ eutectic composite

Three distinct regions of tensile, deformation and fracture behavior were observed in a 2.5 wt. per cent Al gamma/gamma prime-delta eutectic alloy as the testing temperature was varied. The major finding was an extraordinary ductility maximum at about 550 C. It was shown that this phenomenon is caused by the deflection of transverse cracks at the eutectic grain boundaries when yielding occurs. This delamination between eutectics grains caused by fracture of a gamma prime eutectic grain boundary film leads to a distinctly different 'wood-like' fracture surface morphology. Above 690 C to 926 C, yield and tensile strength values decrease while ductility increase slightly. Cooperative twinning of both phases develops giving rise to block-like deformation of the microstructure quite in parallel to the behavior observed previously in the gamma-delta system.

Bertorello, H. R.↗

Surface topography-connections between lubrication and failure initiation

The characteristics of the initial surface topography is intimately connected to the machining process by which it is produced. Both processes create a near surface region of residual stresses, microstructure and hardness that is different from the bulk. The material properties in this rather undefined region can significantly influence the mode of failure, such as wear, scuffing or fatigue, as well as the degree of failure resistance for a given material. Under full film elastohydrodynamic (EHD) conditions, where shear is accomodated within a relatively thick lubricant film, the normal and shear stresses are distributed uniformly over the near surface region, and the surface topography has little influence on the lubrication or failure process. Under more typical conditions where surface roughness and lubricant film thickness are of the same order of magnitude, the surface topography not only emerges as an important parameter in failure initiation, but it also becomes intimately involved in the lubrication process itself.

Wedeven, L. D.↗

Reactions of SiC with H2/H2O/Ar mixtures at 1300 C

Thermochemical modeling anticipates the existence of three reaction regions for the case of a sintered alpha-SiC with 5 percent H2/H2O/Ar at 1300 C, depending on the initial water vapor or, equivalently, oxygen, content of the gas stream. While a high oxygen content leads to SiC-protecting SiO2 surface film formation and limits consumption of the SiC through passive oxidation, intermediate oxygen contents lead to SiO and CO formation and rapid SiC consumption. In this intermediate region, reaction rates appear to be controlled by H2O gas-phase transport to the sample; reacted microstructures exhibit extensive grain-boundary attack in this region. Very low oxygen content is predicted to selectively remove carbon, with free silicon formation.

Jacobson, Nathan S.↗

Integration of Product, Package, Process, and Environment: A Food System Optimization

The food systems slated for future NASA missions must meet crew nutritional needs, be acceptable for consumption, and use resources efficiently. Although the current food system of prepackaged, moderately stabilized food items works well for International Space Station (ISS) missions, many of the current space menu items do not maintain acceptability and/or nutritive value beyond 2 years. Longer space missions require that the food system can sustain the crew for 3 to 5 years without replenishment. The task "Integration of Product, Package, Process, and Environment: A Food System Optimization" has the objective of optimizing food-product shelf life for the space-food system through product recipe adjustments, new packaging and processing technologies, and modified storage conditions. Two emergent food processing technologies were examined to identify a pathway to stable, wet-pack foods without the detrimental color and texture effects. Both microwave-assisted thermal sterilization (MATS) and pressure-assisted thermal stabilization (PATS) were evaluated against traditional retort processing to determine if lower heat inputs during processing would produce a product with higher micronutrient quality and longer shelf life. While MATS products did have brighter color and better texture initially, the advantages were not sustained. The non-metallized packaging film used in the process likely provided inadequate oxygen barrier. No difference in vitamin stability was evident between MATS and retort processed foods. Similarly, fruit products produced using PATS showed improved color and texture through 3 years of storage compared to retort fruit, but the vitamin stability was not improved. The final processing study involved freeze drying. Five processing factors were tested in factorial design to assess potential impact of each to the quality of freeze-dried food, including the integrity of the microstructure. The initial freezing rate and primary freeze drying temperature and pressure were linked to final product quality in freeze-dried corn, indicating processing modifications that could lead to improved product shelf life. Storage temperatures and packaging systems were also assessed for the impact to food quality. Reduced temperature storage had inconclusive impact to the progression of rancidity in butter cookies. Frozen storage was detrimental to fruit and vegetable textural attributes but refrigerated storage helped to sustain color and organoleptic ratings for plant-based foods. With regard to packaging systems, the metallized film overwrap significantly decreased the progression of the rancidity of butter cookies as compared to the highest barrier non-metallized film. The inclusion of oxygen scavengers resulted in noticeable moisture gains in butter cookies over time, independent of packaging film systems. Neither emergent processing technology nor the freeze dry optimization resulted in compelling quality differences from current space food provisions such that a five-year shelf life is likely with these processing changes alone. Using a combination of refrigeration and PATS processing is expected to result in organoleptically-acceptable fruit quality for most fruits through five years. The vitamin degradation will be aided somewhat by the cold temperatures but, given the labile nature of vitamin C, a more stable fortification method, such as encapsulation, should also be investigated to ensure vitamin delivery throughout the product life. Similarly, significant improvement to the packaging film used in the MATS processing, optimization of formulation for dielectric properties, vitamin fortification, and reduced temperature storage should be investigated as a hurdle approach to reach a five year shelf life in wet-pack entrees and soups. Baked goods and other environmentally-sensitive spaceflight foods will require an almost impenetrable barrier to protect the foods from oxygen and moisture ingress but scavengers and reduced storage temperature did not improve baked good shelf life and are not recommended at this time for these foods.

Cooper, Maya R.↗

Laboratory Instruments Available to Support Space Station Researchers at Marshall Space Flight Center

A number of research instruments are available at NASA's Marshall Space Flight Center (MSFC) to support ISS researchers and their investigations. These modern analytical tools yield valuable and sometimes new informative resulting from sample characterization. Instruments include modern scanning electron microscopes equipped with field emission guns providing analytical capabilities that include angstron-level image resolution of dry, wet and biological samples. These microscopes are also equipped with silicon drift X-ray detectors (SDD) for fast yet precise analytical mapping of phases, as well as electron back-scattered diffraction (EBSD) units to map grain orientations in crystalline alloys. Sample chambers admit large samples, provide variable pressures for wet samples, and quantitative analysis software to determine phase relations. Advances in solid-state electronics have also facilitated improvements for surface chemical analysis that are successfully employed to analyze metallic materials and alloys, ceramics, slags, and organic polymers. Another analytical capability at MSFC is a mganetic sector Secondary Ion Mass Spectroscopy (SIMS) that quantitatively determines and maps light elements such as hydrogen, lithium, and boron along with their isotopes, identifies and quantifies very low level impurities even at parts per billion (ppb) levels. Still other methods available at MSFC include X-ray photo-electron spectroscopy (XPS) that can determine oxidation states of elements as well as identify polymers and measure film thicknesses on coated materials, Scanning Auger electron spectroscopy (SAM) which combines surface sensitivity, spatial lateral resolution (approximately 20 nm), and depth profiling capabilities to describe elemental compositions in near surface regions and even the chemical state of analyzed atoms. Conventional Transmission Electron Microscope (TEM) for observing internal microstructures at very high magnifications and the Electron Probe Micro-analyzer (EPMA) for very precise microanalysis are available as needed by the researcher. Space Station researchers are invited to work with MSFC in analyzing their samples using these techniques.

Panda, Binayak↗

Single-Wall Carbon Nanotube Anodes for Lithium Cells

In recent experiments, highly purified batches of single-wall carbon nanotubes (SWCNTs) have shown promise as superior alternatives to the graphitic carbon-black anode materials heretofore used in rechargeable thin-film lithium power cells. The basic idea underlying the experiments is that relative to a given mass of graphitic carbon-black anode material, an equal mass of SWCNTs can be expected to have greater lithium-storage and charge/discharge capacities. The reason for this expectation is that whereas the microstructure and nanostructure of a graphitic carbon black is such as to make most of the interior of the material inaccessible for intercalation of lithium, a batch of SWCNTs can be made to have a much more open microstructure and nanostructure, such that most of the interior of the material is accessible for intercalation of lithium. Moreover, the greater accessibility of SWCNT structures can be expected to translate to greater mobilities for ion-exchange processes and, hence, an ability to sustain greater charge and discharge current densities.

Hepp, Aloysius F.↗

Microstructural investigations of light-emitting porous Si layers

The structural and morphological characteristics of visible-light-emitting porous Si layers produced by anodic and stain etching of single-crystal Si substrates are compared using transmission electron microscopy and atomic force microscopy (AFM). AFM of conventionally anodized, laterally anodized and stain-etched Si layers show that the layers have a fractal-type surface morphology. The anodized layers are rougher than the stain-etched films. At higher magnification 10 nm sized hillocks are visible on the surface. Transmission electron diffraction patterns indicate an amorphous structure with no evidence for the presence of crystalline Si in the near-surface regions of the porous Si layers.

George, T.↗

Micro-Raman Analysis of Irradiated Diamond Films

Owing to its unique and robust physical properties, diamond is a much sought after material for use in advanced technologies such as Microelectromechanical Systems (MEMS). The volume and weight savings promised by MEMS-based devices are of particular interest to spaceflight applications. However, much basic materials science research remains to be completed in this field. Results of micro-Raman analysis of proton (1015 - 1017 H+/cm2 doses) irradiated chemical vapor deposited (CVD) diamond reveals that the microstructure is retained even after high radiation exposure.

Newton, R. L.↗

Onset conditions for gas phase reaction and nucleation in the CVD of transition metal oxides

A combined experimental/theoretical study is presented of the onset conditions for gas phase reaction and particle nucleation in hot substrate/cold gas CVD of transition metal oxides. Homogeneous reaction onset conditions are predicted using a simple high activation energy reacting gas film theory. Experimental tests of the basic theory are underway using an axisymmetric impinging jet CVD reactor. No vapor phase ignition has yet been observed in the TiCl4/O2 system under accessible operating conditions (below substrate temperature Tw = 1700 K). The goal of this research is to provide CVD reactor design and operation guidelines for achieving acceptable deposit microstructures at the maximum deposition rate while simultaneously avoiding homogeneous reaction/nucleation and diffusional limitations.

Collins, J.↗

Environmental fatigue of an Al-Li-Cu alloy. Part 3: Modeling of crack tip hydrogen damage

Environmental fatigue crack propagation rates and microscopic damage modes in Al-Li-Cu alloy 2090 (Parts 1 and 2) are described by a crack tip process zone model based on hydrogen embrittlement. Da/dN sub ENV equates to discontinuous crack advance over a distance, delta a, determined by dislocation transport of dissolved hydrogen at plastic strains above a critical value; and to the number of load cycles, delta N, required to hydrogenate process zone trap sites that fracture according to a local hydrogen concentration-tensile stress criterion. Transgranular (100) cracking occurs for process zones smaller than the subgrain size, and due to lattice decohesion or hydride formation. Intersubgranular cracking dominates when the process zone encompasses one or more subgrains so that dislocation transport provides hydrogen to strong boundary trapping sites. Multi-sloped log da/dN-log delta K behavior is produced by process zone plastic strain-hydrogen-microstructure interactions, and is determined by the DK dependent rates and proportions of each parallel cracking mode. Absolute values of the exponents and the preexponential coefficients are not predictable; however, fractographic measurements theta sub i coupled with fatigue crack propagation data for alloy 2090 established that the process zone model correctly describes fatigue crack propagation kinetics. Crack surface films hinder hydrogen uptake and reduce da/dN and alter the proportions of each fatigue crack propagation mode.

Piascik, Robert S.↗

Design Considerations for Practical Li-S Batteries for Electric Aviation

The development of high-energy, high-safety, and high-power batteries beyond electric automotive standards is critical for future electric aviation applications. Non-volatile solid-state electrolytes (SSE) offer many promising advantages over traditional flammable liquid electrolytes. Solid-state electrolytes may be an enabling technology for certain battery chemistries by preventing detrimental interactions with liquid electrolytes, for example prevention of the dissolution of intermediates in lithium-sulfur common in traditional liquid organic solvents. However, significant manufacturing challenges must be overcome before the adoption of such technology. This research was conducted to identify processing techniques for producing solid-state battery components with practical dimensions and weights for enabling high specific energy cells. Traditional research has identified a range of very high theoretical ionic conductivities but are impractical due to their instability or inability to be manufactured. Electrolytes explored in this study were produced as sulfide-polymer composites with densified thicknesses below 40 micron using a tape-casting technique and thermoplastic elastomer binder. The combination of high chemical compatibility and flexibility produced robust films that had moderate impact on the ionic conductivity but was capable of dramatically reducing the parasitic mass. Despite minimal conductivity losses, films were produced 10-15 times thinner than comparable bulk powder electrolytes thus leading to overall lower film resistance. Conductivity is maintained above 0.2mS/cm for composite electrolytes. Through the analysis of materials based on their physical properties, such as density, practical cells can be designed. Based on this, low density sulfide-solid-state electrolytes are a promising candidate for achieving the energy and safety metrics for electric aviation, however, further optimization of cathode microstructure and composite processing will be required to achieve the high power metrics and will be the focus of further studies. Additionally, fabrication challenges arise when utilizing metallic lithium foil, due to its soft nature, as overflow and mechanical short circuit can occur on assembly which remains a challenge to overcome before metallic lithium anodes can be fully realized.

batteries↗

Organometallic chemical vapor deposition and characterization of ZnGe(1-x)Si(x)P2-Ge alloys on GaP substrates

The epitaxial growth of ZnGe(1-x)Si(x)P2-Ge alloys on GaP substrates by open tube organometallic chemical vapor deposition (OMCVD) is reported. The chemical composition of the alloys characterized by energy dispersive X-ray spectroscopy shows that alloys with x up to 0.13 can be deposited on (001) GaP. Epitaxial growth with mirror smooth surface morphology was achieved for x less than or equal to 0.05. Transmission electron microscopy (TEM) micrographs of these alloys show specular epitaxy and the absence of microstructural defects indicating a defect density of less than 10(exp 7) cm(sup -2). Selected area electron diffraction pattern of the alloy shows that the epitaxial layer crystallizes in the chalcopyrite structure with relatively weak superlattice reflections indicating certain degree of randomness in the cation sublattice. Hall measurements show that the alloys are p-type, like the unalloyed films; the carrier concentration, however, dropped about 10 times from 2 x 10(exp 18) to 2 x 10(exp 17) cm(sup -3). Absorption measurements indicate that the band tailing in the absorption spectra of the alloy was shifted about 0.04 eV towards shorter wavelength as compared to the unalloyed material. Diodes fabricated from the n(+)-GaP/p-ZnSiP2-ZnGeP2-Ge heterostructure at x = 0.05 have a reverse break-down voltage of -10.8 V and a reverse saturation current density of approximately 6 x 10(exp -8) A/sq cm.

Xing, G. C.↗

Fabrication of advanced electrochemical energy materials using sol-gel processing techniques

Advanced materials play an important role in electrochemical energy devices such as batteries, fuel cells, and electrochemical capacitors. They are being used as both electrodes and electrolytes. Sol-gel processing is a versatile solution technique used in fabrication of ceramic materials with tailored stoichiometry, microstructure, and properties. The application of sol-gel processing in the fabrication of advanced electrochemical energy materials will be presented. The potentials of sol-gel derived materials for electrochemical energy applications will be discussed along with some examples of successful applications. Sol-gel derived metal oxide electrode materials such as V2O5 cathodes have been demonstrated in solid-slate thin film batteries; solid electrolytes materials such as beta-alumina for advanced secondary batteries had been prepared by the sol-gel technique long time ago; and high surface area transition metal compounds for capacitive energy storage applications can also be synthesized with this method.

Chu, C. T.↗

A computer simulation of thin film nucleation and growth: The Volmer-Weber case

The computer simulation of thin film nucleation and growth, which was previously performed for the case of single monolayer, was modified to include multilayer growth via the Volmer-Weber mechanism. The simulation results show that: (1) the kinetics of multilayer film growth is nearly identical to that of monolayer growth; (2) when no reevaporation takes place, the cluster density resulting from multilayer growth is higher at high coverage than that resulting from monolayer growth; (3) when reevaporation does take place, the cluster density resulting from multilayer growth is nearly identical to that resulting from monolayer growth. This is not due, however, to similarity in microstructure.

Salik, J.↗

Photochemistry of unsaturated polymers.

The mechanisms of the direct photochemical reactions which occur in unsaturated polymers when irradiated as thin films in vacuo are reviewed. Important reactions in 1,4-polyisoprene and 1,4-polybutadiene are cis-trans isomerization, loss of 1,4-unsaturation, formation of new external double bonds (vinylidene and/or vinyl units) and cyclopropyl formation. In 1,2-polybutadiene and 3,4-polyisoprene, on the other hand, the main reaction is consumption of the external double bonds through cyclization. Recent work on the photoinduced microstructural changes in cis and trans polypentenamers is also discussed.

Golub, M. A.↗

Spatiotemporal chaos near the onset of cellular growth during thin-film solidification of a binary alloy

Thin-film solidification experiments with a succinonitrile-acetone alloy are used to observe the long time-scale dynamics of cellular crystal growth at growth rates only slightly above the critical value VC = Vc(lambda sub c) for the onset of morphological instability. Under these conditions only very small amplitude cells are observed with wavelengths near the value predicted by linear stability theory lambda = lambda sub c. At long times, microstructures with wavelengths significantly finer than lambda suc c form by nucleation at defects across the interface. These interfaces do not have a unique microstructure, but seem to exhibit spatiotemporal chaos on a long time scale caused by the continual birth and death of cells by tip splitting and cell annihilation in grooves.

Lee, J. T. C.↗

The Metastable Persistence of Vapor-Deposited Amorphous Ice at Anomalously High Temperatures

Studies of the gas release, vaporization behavior and infrared (IR) spectral properties of amorphous and crystalline water ice have direct application to cometary and planetary outgassing phenomena and contribute to an understanding of the physical properties of astrophysical ices. Several investigators report anomalous phenomena related to the warming of vapor-deposited astrophysical ice analogs. However gas release, ice volatilization and IR spectral features are secondary or tertiary manifestations of ice structure or morphology. These observations are useful in mimicking the bulk physical and chemical phenomena taking place in cometary and other extraterrestrial ices but do not directly reveal the structural changes which are their root cause. The phenomenological interpretation of spectral and gas release data is probably the cause of somewhat contradictory explanations invoked to account for differences in water ice behavior in similar temperature regimes. It is the microstructure, micromorphology and microchemical heterogeneity of astrophysical ices which must be characterized if the mechanisms underlying the observed phenomena are to be understood. We have been using a modified Transmission Electron Microscope to characterize the structure of vapor-deposited astrophysical ice analogs as a function of their deposition, temperature history and composition. For the present experiments, pure water vapor is deposited at high vacuum onto a 15 K amorphous carbon film inside an Hitachi H-500H TEM. The resulting ice film (approx. 0.05 micrometers thick) is warmed at the rate of 1 K per minute and diffraction patterns are collected at 1 K intervals. These patterns are converted into radial intensity distributions which are calibrated using patterns of crystalline gold deposited on a small part of the carbon substrate. The small intensity contributed by the amorphous substrate is removed by background subtraction. The proportions of amorphous and crystalline material in each pattern are determined by subtracting a percentage of crystalline component relative to amorphous and pure crystalline endmembers. Vapor-deposited water ice undergoes two amorphous to amorphous structural transformations in the temperature range 15-130 K with important astrophysical implications. The onset of cubic crystallization occurs at 142-160 K (at 1K per minute heating rates) during which the 220 and 311 diffraction maxima appear and 0.1 micrometer crystallites can be seen in bright field images. This transition is time dependent.

Blake, David F.↗