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NASA NTRSDate not supplied

Contamination, Transportation or Transmutation in LENR Material Analyses

LENR experiments using various loading and triggering mechanisms rely on a variety of elemental and isotopic assays to determine LENR effects. These assays include optical microscopy, Scanning Electron Microscopy with Energy Dispersive X-Ray Analysis (SEM/EDX), X-Ray Photoelectron Spectroscopy (XPS) and Transmission Electron Microscopy (TEM). All of these methods observe the surface of a material. By dissolving or vaporizing the sample, Inductively Coupled Plasma Optical Element Spectroscopy (ICP-OES) can determine elemental composition (ppb) or with mass spectroscopy, isotopes (ICP/MS). One can use a focused ion beam (FIB) to cut open a sample and observe the “cut” with either SEM/EDX, or Time-of-Flight Secondary Ion Mass Spectroscopy (TOF-SIMS). High Purity Gamma Ray Spectroscopy (HPGe) and alpha/ beta Liquid Scintillator spectroscopy can be used. We’ve employed these assay methods in our NASA GRC research under both the Advanced Energy Conversion and Lattice Confinement Fusion Projects. However, there are limitations associated with each of these methods ranging from handling contamination, instrumental limitations including sensitivity and field of view, and sample preparation.

Low Energy Nuclear Reactions↗
NASA NTRS2007

Multifunctional, High-Temperature Nanocomposites

In experiments conducted as part of a continuing effort to incorporate multifunctionality into advanced composite materials, blends of multi-walled carbon nanotubes and a resin denoted gPETI-330 h (wherein gPETI h is an abbreviation for gphenylethynyl-terminated imide h) were prepared, characterized, and fabricated into moldings. PETI-330 was selected as the matrix resin in these experiments because of its low melt viscosity (<10 poise at a temperature of 280 C), excellent melt stability (lifetime >2 hours at 280 C), and high temperature performance (>1,000 hours at 288 C). The multi-walled carbon nanotubes (MWCNTs), obtained from the University of Kentucky, were selected because of their electrical and thermal conductivity and their small diameters. The purpose of these experiments was to determine the combination of thermal, electrical, and mechanical properties achievable while still maintaining melt processability. The PETI-330/MWCNT mixtures were prepared at concentrations ranging from 3 to 25 weight-percent of MWCNTs by dry mixing of the constituents in a ball mill using zirconia beads. The resulting powders were characterized for degree of mixing and thermal and rheological properties. The neat resin was found to have melt viscosity between 5 and 10 poise. At 280 C and a fixed strain rate, the viscosity was found to increase with time. At this temperature, the phenylethynyl groups do not readily react and so no significant curing of the resin occurred. For MWCNT-filled samples, melt viscosity was reasonably steady at 280 C and was greater in samples containing greater proportions of MWCNTs. The melt viscosity for 20 weightpercent of MWCNTs was found to be .28,000 poise, which is lower than the initial estimated allowable maximum value of 60,000 poise for injection molding. Hence, MWCNT loadings of as much as 20 percent were deemed to be suitable compositions for scale-up. High-resolution scanning electron microscopy (HRSEM) showed the MWCNTs to be well dispersed in the polymer matrices, while high-resolution transmission electron microscopy shows splits in the walls of the MWCNTs but no catastrophic breakage of tubes. To further assess processing characteristics prior to scale-up, samples containing 10, 15, and 20 weight-percent of MWCNTs were processed through a laboratory melting extruder. HRSEM of the extruded fibers shows significant alignment of MWCNTs in the flow direction (see figure). For the samples containing 20 weight-percent of MWCNTs, difficulties were encountered during feeding, and the temperature of a rotor in the extruder rose to 245 C because of buildup of frictional heat; this indicates that materials of this type having MWCNT concentrations .20 weight- percent may not be melt-processable. On the basis of the results from the foregoing characterizations, samples containing 10, 15, and 20 weight-percent of MWCNTs were scaled up to masses of .300 g and used to make specimens having dimensions of 10.2 by 15.2 by 0.32 cm. These specimens were molded by (1) injecting the mixtures, at temperatures between 260 and 280 C, into a tool made of the low-thermal-expansion alloy InvarR and then (2) curing for 1 hour at 371 C. The tool was designed to impart shear during the injection process in an attempt to achieve some alignment of the MWCNTs in the flow direction.

Connell, John W.↗
NASA NTRS2018

Investigating Variations in Water Abundances in Lunar Felsite Clasts Using Coordinated Field-Emission STEM and NanoSIMS Analyses

As representatives of petrochemically-evolved igneous rocks on the Moon, the granitic felsite clasts in lunar breccias have come under renewed focus as part of new efforts to use feldspars for assessing the inventory of lunar water and other volatiles. Previous petrologic studies of these clasts were tilted towards finding those assemblages and relationships most likely to be direct products of magmatic processes. In support of our on-going NanoSIMS (Nanoscale Secondary Ion Mass Spectrometry) measurements of trace water contents in the feldspars in these clasts, we are using coordinated analytical SEM (Scanning Electron Microscopy), electron probe microanalyzer (EPMA) and analytical field emission scanning transmission electron microscopy (FE-STEM) techniques to re-evaluate the full diversity of processes under which the feldspar-bearing assemblages in these clasts formed. Here we report a comparison of FE-STEM imaging and microanalysis results obtained on focused ion beam (FIB) sections extracted from felsite (alkali feldspar plus SiO2 plus or minus plagioclase) clasts in lunar breccias 15405 and 12013. The feldspars in these clasts have water contents which, although relatively low (7-18 ppm) by terrestrial standards, still show values significantly higher than measurements (approximately 0.5 ppm) of nominally anhydrous NanoSIMS standards.

Christoffersen, Roy↗
NASA NTRS2005

Surface and Internal Structure of Pristine Presolar Silicon Carbide

Silicon carbide is the most well-studied type of presolar grain. Isotope measurements of thousands [1,2] and structural data from over 500 individual grains have been reported [3]. The isotope data indicate that approximately 98% originated in asymptotic giant branch stars and 2% in supernovae. Although tens of different polytypes of SiC are known to form synthetically, only two polytypes have been reported for presolar grains. Daulton et al. [3] found that for SiC grains isolated from Murchison by acid treatments, 79.4% are 3C cubic beta-SiC, 2.7% are 2H hexagonal alpha-SiC, 17.1% are intergrowths of and , and 0.9% are heavily disordered. They report that the occurrence of only the and polytypes is consistent with the observed range of condensation temperatures of circumstellar dust for carbon stars. Further constraint on the formation and subsequent alteration of the grains can be obtained from studies of the surfaces and interior structure of grains in pristine form, i.e., prepared without acid treatments [4,5]. The acid treatments remove surface coatings, produce etch pits around defect sites and could remove some subgrains. Surface oxides have been predicted by theoretical modeling as a survival mechanism for SiC grains exposed to the hot oxidizing solar nebula [6]. Scanning electron microscopy studies of pristine SiC shows some evidence for the existence of oxide and organic coatings [4]. We report herein on transmission electron microscopy studies of the surface and internal structure of two pristine SiC grains, including definitive evidence of an oxide rim on one grain, and the presence of internal TiC and AlN grains.

Stroud, Rhonda, M.↗
NASA NTRS1988

Soil microstructure and electron microscopy

As part of the process of comparing Martian soils with terrestial soils, high resolution electron microscopy and associated techniques should be used to examine the finer soil particles, and various techniques of electron and optical microscopy should be used to examine the undisturbed structure of Martian soils. To examine the structure of fine grained portions of the soil, transmission electron microscopy may be required. A striking feature of many Martian soils is their red color. Although the present-day Martian climate appears to be cold, this color is reminiscent of terrestial tropical red clays. Their chemical contents are broadly similar.

Smart, P.↗
NASA NTRS2003

Morphology of the Vestibular Utricule in Toadfish, Opsanus Tau

The uticle is an otolith organ in the vertebrate inner ear that provides gravitoinertial acceleration information into the vestibular reflex pathways. The aim of the present study was to provide an anatomical description of this structure in the adult oyster toadfish, and establish a morphological basis for interpretation of subsequent functional studies. Light, scanning electron and transmission electron microscopy were applied to visualize the sensory epithelium and its neural innervation. Electrophysiological techniques were used to identify utricular afferents by their response to translation stimuli. Similar to nerve afferents supplying the semicircular canals and lagena, utricular afferents commonly exhibit a short-latency increase of firing rate in response to electrical activation of the central efferent pathway. Afferents were labeled with biocytin either intraaxonally or with extracellular bulk deposits. Light microscope images of serial thick sections were used to make three-dimensional reconstructions of individual labeled afferents to identify the dendritic morphology with respect to epithelial location. Scanning electron microscopy was used to visualize the surface of the otolith mass facing the otolith membrane, and the hair cell polarization patterns of strioler and extrastriolar regions. Transmission electron micrographs of serial thin sections were compiled to create a three-dimensional reconstruction of the labeled afferent over a segment of its dendritic field and to examine the hair cell-afferent synaptic contacts.

Bass, L.↗
NASA NTRS1972

High voltage transmission microscopy of Surveyor 3 camera shrouds

The internal structure of painted and unpainted aluminum alloy sheet samples from the TV camera shrouds were examined by high-voltage transmission electron microscopy. No clear-cut evidence of radiation damage effects was observed. Noticeable differences in microstructures between the upper visor and the sides and bottom of the lower shroud suggest different thermal histories, and the maximum temperatures due to solar heating are estimated to be between 164 and 319 C. Some correlation between microstructures and maximum estimated temperature is noted. It is felt that the apparent temperature rise due to solar heating will not affect the structural integrity of spacecraft components except possibly for very long periods of exposure. However, substantial thermal diffusion could affect interpretation of solar wind rare gas studies.

Fisher, R. M.↗
NASA NTRS1980

Defect structure of web silicon ribbon

The results of a preliminary study of two dendritic web samples are presented. The structure and electrical activity of the defects in the silicon webs were studied. Optical microscopy of chemically etched specimens was used to determine dislocation densities. Samples were mechanically polished, then Secco etched for approximately 5 minutes. High voltage transmission electron microscopy was used to characterize the crystallographic nature of the defects.

Cunningham, B.↗
NASA NTRS2006

Microstructural Study of Micron-Sized Craters Simulating Stardust Impacts in Aluminum 1100 Targets

Various microscopic techniques were used to characterize experimental micro- craters in aluminium foils to prepare for the comprehensive analysis of the cometary and interstellar particle impacts in aluminium foils to be returned by the Stardust mission. First, SEM (Scanning Electron Microscopy) and EDS (Energy Dispersive X-ray Spectroscopy) were used to study the morphology of the impact craters and the bulk composition of the residues left by soda-lime glass impactors. A more detailed structural and compositional study of impactor remnants was then performed using TEM (Transmission Electron Microscopy), EDS, and electron diffraction methods. The TEM samples were prepared by Focused Ion Beam (FIB) methods. This technique proved to be especially valuable in studying impact crater residues and impact crater morphology. Finally, we also showed that InfraRed microscopy (IR) can be a quick and reliable tool for such investigations. The combination of all of these tools enables a complete microscopic characterization of the craters.

Leroux, Hugues↗
NASA NTRS1992

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.↗
NASA NTRS1988

Scanning electron microscopy study of adhesion in sea urchin blastulae

The dissociation supernatant (DS) isolated by disaggregating Strongylocentrotus purpuratus blastulae in calcium- and magnesium-free seawater specifically promotes reaggregation of S. purpuratus blastula cells. The purpose of this study was to use scanning electron microscopy to examine the gross morphology of aggregates formed in the presence of DS to see if it resembles adhesion in partially dissociated blastulae. A new reaggregation procedure developed here, using large volumes of cell suspension and a large diameter of rotation, was utilized to obtain sufficient quantities of aggregates for scanning electron microscopy. The results indicate that aggregates formed in the presence of DS resemble partially dissociated intact embryos in terms of the direct cell-cell adhesion observed. DS did not cause aggregation to form as a result of the entrapment of cells in masses of extracellular material. These studies provide the groundwork for further studies using transmission electron microscopy to more precisely define the adhesive contacts made by cells in the presence of the putative adhesion molecules present in DS.

Crowther, Susan D.↗
NASA NTRS2006

Three-Dimensional Human Bronchial-Tracheal Epithelial Tissue-Like Assemblies (TLAs) as Hosts for Severe Acute Respiratory Syndrome (SARS)-CoV Infection

A three-dimensional (3-D) tissue-like assembly (TLA) of human bronchial-tracheal mesenchymal (HBTC) cells with an overlay of human bronchial epithelial (BEAS-2B) cells was constructed using a NASA Bioreactor to survey the infectivity of SARS-CoV. This TLA was inoculated with a low passage number Urbani strain of SARS-CoV. At selected intervals over a 10-day period, media and cell aliquots of the 3-D TLA were harvested for viral titer assay and for light and electron microscopy examination. All viral titer assays were negative in both BEAS-2B two-dimensional monolayer and TLA. Light microscopy immunohistochemistry demonstrated antigen-antibody reactivity with anti-SARS-CoV polyclonal antibody to spike and nuclear proteins on cell membranes and cytoplasm. Coronavirus Group 2 cross-reactivity was demonstrated by positive reaction to anti-FIPV 1 and anti-FIPV 1 and 2 antibodies. TLA examination by transmission electron microscopy indicated increasing cytoplasmic vacuolation with numerous electron-dense bodies measuring 45 to 270 nm from days 4 through 10. There was no evidence of membrane blebbing, membrane duplication, or fragmentation of organelles in the TLAs. However, progressive disruption of endoplasmic reticulum was observed throughout the cells. Antibody response to SARS-CoV specific spike and nucleocapsid glycoproteins, cross-reactivity with FIPV antibodies, and the cytoplasmic pathology suggests this HBTE TLA model is permissive to SARS-CoV infection.

Suderman, M. T.↗
NASA NTRS1972

An electron microscopy examination of primary recrystallization in TD-nickel.

Primary recrystallization in TD-nickel 1 in. bar has previously been regarded as the process by which the initial fine grain structure is converted to a coarse grain size (increases in grain size by 500 times) under suitable deformation and annealing conditions. This process is dependent on deformation mode. While it occurs readily after rolling transverse to the bar axis and annealing (800 C), it is completely inhibited by longitudinal rolling and swaging deformations, even for very high (1320 C) annealing temperatures. A transmission electron microscopy examination of deformation and annealing substructures indicates that primary recrystallization in TD-nickel 1 in. bar actually occurs on the sub-light optical level, to produce a grain structure similar in size to the initial fine grained state.

Petrovic, J. J.↗
NASA NTRS2005

Focused Ion Beam Microscopy of ALH84001 Carbonate Disks

Our aim is to understand the mechanism(s) of formation of carbonate assemblages in ALH84001. A prerequisite is that a detailed characterization of the chemical and physical properties of the carbonate be established. We present here analyses by transmission electron microscopy (TEM) of carbonate thin sections produced by both focused ion beam (FIB) sectioning and ultramicrotomy. Our results suggest that the formation of ALH84001 carbonate assemblages were produced by considerably more complex process(es) than simple aqueous precipitation followed by partial thermal decomposition as proposed by other investigators [e.g., 1-3].

Thomas-Keprta, Kathie L.↗
NASA NTRS1995

Transmission electron microscope studies of extraterrestrial materials

Transmission Electron Microscopy, X-Ray spectrometry and electron-energy-loss spectroscopy are used to analyse carbon in interplanetary dust particles. Optical micrographs are shown depicting cross sections of the dust particles embedded in sulphur. Selected-area electron diffraction patterns are shown. Transmission Electron Microscope specimens of lunar soil were prepared using two methods: ion-milling and ultramicrotomy. A combination of high resolution TEM imaging and electron diffraction is used to characterize the opaque assemblages. The opaque assemblages analyzed in this study are dominated by ilmenite with lesser rutile and spinel exsolutions, and traces of Fe metal.

Keller, Lindsay P.↗
NASA NTRS1997

Stereological analysis of gravitropism in protonemata of the moss Ceratodon

Apical cells of dark-grown protonemata of the moss Cerotodon purpureus are negatively gravitropic. Previous light microscopy has shown that reorientation to the horizontal induces amyloplast sedimentation and redistribution of microtubules. To determine whether other components become redistributed laterally or axially, the apical 35 micrometers of both vertical and horizontal apical cells were compared stereologically using transmission electron microscopy. Reorientation to the horizontal changed the longitudinal distributions of tubular ER, Golgi stacks, and vesicles but not cisternal ER, mitochondria, and plastids. Only plastids showed a statistically significant lateral redistribution after horizontal placement. Qualitative examination of the sedimentation zone showed plastids sedimented close to peripherally located ER with vacuoles displaced above plastids. These results argue against a model where differential tip growth results from a redistribution of Golgi stacks or exocytic vesicles.

Non-NASA Center↗
NASA NTRS1989

Electron beam analysis of particulate cometary material

Electron microscopy will be useful for characterization of inorganic dust grains in returned comet nucleus samples. The choice of instrument(s) will depend primarily on the nature of the samples, but ultimately a variety of electron-beam methods could be employed. Scanning and analytical (transmission) electron microscopy are the logical choise for morphological, mineralogical, and bulk chemical analyses of dust grains removed from ices. It may also be possible to examine unmelted ice/dust mixtures using an environmental scanning electron microscope equipped with a cryo-transfer unit and a cold stage. Electron microscopic observations of comet nuclei might include: (1) porosities of dust grains; (2) morphologies and microstructures of individual mineral grains; (3) relative abundances of olivine, pyroxene, and glass; and (4) the presence of phases that might have resulted from aqueous alteration (layer silicates, carbonates, sulfates).

Bradley, John↗
NASA NTRS2006

Novel Nanolaminates for Aerospace Applications

Nanolaminate manufacturing (NLM) is a new way of developing materials whose properties can far exceed those of homogeneous materials. Traditional alloys, composites and bulk laminates tend to average the properties of the materials from which they were made. With nanostructured materials, the high density of interfaces between dissimilar materials results in novel material properties. For example, materials made -from alternating nanoscale layers of metals and oxides have exhibited thermal conductivities far below those of the oxides themselves. Also, metallic nanolaminates can have peak strengths 100 times lager than the bulk constituent metals. Recent work at MSFC has focused on the development of nickel/aluminum oxide (Ni/Al2O3)) nanolaminates. Ni/Al2O3 nanolaminates are expected to have better strength, creep and fatigue resistance, oxygen compatibility, and corrosion resistance than the traditional metal-matrix composites of this material, which has been used in a variety of aerospace applications. A chemical vapor deposition (CW) system has been developed and optimized for the deposition of nanolaminates. Nanolaminates with layer thicknesses between 10 and 300 nm have been successfully grown and characterization has included scanning electron microscopy (SEM) and atomic force microscopy (AFM) Nanolaminates have a large variety of potential applications. They can be tailored to have both very small and anisotropic thermal conductivities and are promising as thermal coatings for both rock$ engine components and aerobraking structures. They also have the potential to be used in aerospace applications where strength at high temperatures, corrosion resistance or resistance to hydrogen embrittlement is important. Both CVD and magnetron sputtering facilities are available for the deposition of nanolayered materials. Characterization equipment includes SEM, AFM, X-ray diffraction, transmission electron microscopy, optical profilometry, and mechanical tensile pull testing.

Volz, Martin↗