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Variable Pressure - Scanning Electron Microscopy (VP-SEM)

Variable Pressure (or Environmental) Scanning Electron Microscopy (VP-SEM) combined with Energy Dispersive X-ray Spectroscopy (EDS) is one of the most powerful methods for characterizing the sub-micron topography and chemical composition of uncoated samples. Terrestrially, VP-SEM is extensively used to non-destructively study geologic and manufactured materials with high spatial resolution (tens of nanometers) and large depth-of-field. An SEM offers a geologist a first survey of microscopic mineral phases via secondary electron imaging (SEI), which provides a topographic look at a sample, as well as backscattered electron (BEI) imaging, which contrasts the phases present based on their geochemistry (atomic number). A VP-SEM utilizes a gas in the sample chamber as a charge dissipation and signal amplification method, allowing analysis of a sample without preparation in the form of a conductive coating. A miniaturized VP-SEM operating in-situ on a lander or rover would be able to use the CO2-rich Martian atmosphere (e.g., Nier et al., 1976; Williams 2016) as an imaging medium for this purpose. Adaptation of a VP-SEM for in-situ Mars surface studies will provide a new imaging capability (via SEI) that is at least an order of magnitude higher resolution than the Mars Hand Lens Imager (MAHLI) on the Mars Science Laboratory (Williams et al., 2015), and equal to or better than the achieved resolution of the Atomic Force Microscope on the Phoenix Mars lander (Pike et al., 2011). In addition, the MVP-SEM is capable of BSI and simultaneous chemical analysis of the imaged region. In this sense, the MVP-SEM can be regarded as an instrument suite that will provide a new set of information not achievable by any other instrument. The Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) was designed, built, and benchtop tested by a team at NASA’s Marshall Space Flight Center and Jet Propulsion Laboratory (JPL), Jacobs Space Exploration Group, Applied Physics Technologies, Inc. (AP-Tech), and Creare LLC, working with a team of technical and science collaborators. Benchtop testing was successful, proving concept feasibility. To date, the MVP-SEM has achieved an imaging resolution of <100 nm in the lab, and with continued optimization, even better performance (~50 nm resolution) is possible. Use in-situ on the lunar or other planetary surfaces would require some redesign to optimize instrument performance, but such an instrument would be equally useful.

Variable Pressure Scanning Electron Microscopy↗

Miniature Variable Pressure - Scanning Electron Microscopy (MVP-SEM)

Variable Pressure (or Environmental) Scanning Electron Microscopy (VP-SEM) combined with Energy Dispersive X-ray Spectroscopy (EDS) is one of the most powerful methods for characterizing the sub-micron topography and chemical composition of uncoated samples. Terrestrially, VP-SEM is extensively used to non-destructively study geologic and manufactured materials with high spatial resolution (tens of nanometers) and large depth-of-field. An SEM offers a geologist a first survey of microscopic mineral phases via secondary electron imaging (SEI), which provides a topographic look at a sample, as well as backscattered electron (BEI) imaging, which contrasts the phases present based on their geochemistry (atomic number). A VP-SEM utilizes a gas in the sample chamber as a charge dissipation and signal amplification method, allowing analysis of a sample without preparation in the form of a conductive coating. A miniaturized VP-SEM operating in-situ on a lander or rover would be able to use the CO2-rich Martian atmosphere (e.g., Nier et al., 1976; Williams 2016) as an imaging medium for this purpose. Adaptation of a VP-SEM for in-situ Mars surface studies will provide a new imaging capability (via SEI) that is at least an order of magnitude higher resolution than the Mars Hand Lens Imager (MAHLI) on the Mars Science Laboratory (Williams et al., 2015), and equal to or better than the achieved resolution of the Atomic Force Microscope on the Phoenix Mars lander (Pike et al., 2011). In addition, the MVP-SEM is capable of BSI and simultaneous chemical analysis of the imaged region. In this sense, the MVP-SEM can be regarded as an instrument suite that will provide a new set of information not achievable by any other instrument. The Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) was designed, built, and benchtop tested by a team at NASA’s Marshall Space Flight Center and Jet Propulsion Laboratory (JPL), Jacobs Space Exploration Group, Applied Physics Technologies, Inc. (AP-Tech), and Creare LLC, working with a team of technical and science collaborators. Benchtop testing was successful, proving concept feasibility. To date, the MVP-SEM has achieved an imaging resolution of <100 nm in the lab, and with continued optimization, even better performance (~50 nm resolution) is possible. Use in-situ on the lunar or other planetary surfaces would require some redesign to optimize instrument performance, but such an instrument would be equally useful.

Variable Pressure Scanning Electron Microscopy↗

In-Situ Alloying of GRCop-42 via Additive Manufacturing: Precipitate Analysis

GRCop-42, a Cu-4at% Cr-2at% Nb alloy, was designed as a high temperature, high strength, high heat flux material for rocket engine combustion chamber liners by NASA Glenn Research Center. In situ alloying of GRCop-42 (ISGRCop-42) using powder bed fusion (PBF) additive manufacturing (AM) takes elemental powders of Cu, Cr, and Nb to be introduced into the PBF environment and develop the GRCop alloy while simultaneously building an AM component. Elemental powders were milled together prior to printing in an effort to facilitate the alloying process. Success of the in situ alloying process may provide lower cost, faster lead times, alloying optimization, and more design freedom in the development of regeneratively-cooled rocket propulsion systems. Evaluation of the ISGRCop-42 was conducted using a phase extraction procedure to isolate the Cr2Nb precipitates from the pure Cu matrix. The isolated precipitates were then examined using x-ray powder diffraction (XRD), scanning electron microscopy (SEM), and energy dispersion spectroscopy (EDS). It was found that ISGRCop-42 successfully and repeatedly formed Cr2Nb at a yield as high as 89% of potential Cr2Nb. Further, it was identified that the preparation of the powder was the most influential factor in alloying success, and the second most influential factor was the laser power.

In Situ alloying↗

Coordinated Analysis of Organic Matter in Primitive Meteorites

Carbonaceous chondrites (CC) preserve a diverse range of organic matter formed within cold interstellar environments, the solar nebula, and during subsequent parent body asteroidal processing. This organic matter maintains a unique geochemical and istopic record of organic evolution [1-4]. Bulk studies of organics within CC have revealed a complex array of organic species. However, bulk studies invariably involve solvent extraction, resulting in a loss of spatial context of the host mineral matrix [3, 5]. Correlated in situ chemical and isotopic studies suggest preservation of interstellar organics in the form of spherical, often hollow, micrometer sized organic nano-globules. Nanoglobules often exhibit significant delta 15N and delta D enrichments that imply formation through fractionation of ion-molecule reactions within cold molecular clouds and/or the outer protoplanetary disk [5]. In situ studies such as 6-8 are necessary to understand the organic evolutionary stages of nanoglobules and other components in the nebula and parent body [7]. We carried out coordinated in situ micrometer-scale chemical, mineralogical and isotopic studies of the Murchison (CM2), QUE 99177 (CR3), and Tagish Lake (C2 Ung) CC. These studies were performed using fluorescent microscopy, two-step laser mass spectrometry (microL2MS), NanoSIMS, and Scanning Electron Microscopy (SEM) with Energy Dispersive X-Ray Spectroscopy (EDX). Comparative analysis of three different meteorites will help reveal the effects of parent body processes on the chemistry and isotopic composition of organic matter.

meteorites↗

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↗

Production of otoconia in the endolymphatic sac in the Japanese red-bellied newt, Cynops pyrrhogaster: light and transmission electron microscopic study

The formation of otoconia in the endolymphatic sac (ES) of the larval newt, Cynops pyrrhogaster, has been studied by light and transmission electron microscopy. Some of the epithelial cells of the ES contain an abundance of swollen vesicles, Golgi complexes, rough endoplasmic reticula and ribosomes at the late larval stages 50 and 51, approximately 26-30 days after eggs are laid. Five days later, at stage 52, crystals are present in the vacuoles between the epithelial cells. Serial sections indicate that these vacuoles actually form small canals which lie in the wall and join the lumen of the ES. Reconstruction of the ES shows that several canals are contained in the ES wall. At stage 56, about 72 days after eggs are laid, a large number of otoconia are present in the ES lumen, while the otoconia disappear from the canals. It appears that the otoconia are first produced in the canals and then released to the lumen. Some epithelial cells of the ES are thought to expel the organic and inorganic material to the canals to form the otoconia in situ. The process of formation of the otoconia in the ES is discussed.

Non-NASA Center↗

Lunar and Planetary Science XXXV: Interplanetary Dust and Aerogel

Contents include the following: Isotopically Primitive Interplanetary Dust Particles of Cometary Origin: Evidence from Nitrogen Isotopic Compositions. The Solar Nebula s First Accretionary Particles (FAPs) Are They Preserved in Collected Interplanetary Dust Samples? On the Origin of GEMS. An Analytical SuperSTEM for Extraterrestrial Materials Research. Sub-Micrometer Scale Minor Element Mapping in Interplanetary Dust Particles: A Test for Stratospheric Contamination. First Report of Taenite in an Asteroidal Interplanetary Dust Particle: Flash-heating Simulates Nebular Dust Evolution. FTIR Analyses of IDPs: Comparison with the InfraRed Spectra of the Interstellar Medium. Mineralogical Study of Hydrated IDPs: X-Ray Diffraction and Transmission Electron Microscopy. Focused Ion Beam Recovery and Analysis of Interplanetary Dust Particles (IDPs) and Stardust Analogues. Technique for Concentration of Carbonaceous Material from Aerogel Collectors Using HF-Vapor Etching. Synchrotron X-Ray Analysis of Captured Particle Residue in Aerogel. In-Situ Analyses of Earth Orbital Grains Trapped in Aerogel, Using Synchrotron X-Ray Microfluorescence Techniques. Igneous Rims on Micrometeorites and the Sizes of Chondrules in Main Belt Asteroids.

Source record↗

Investigating the Role of Incident Ion Flux in Solar Wind Space Weathering of Carbon-Rich Asteroidal Regolith Via H+ and He+ Irradiation of the Murchison Meteorite

We present results from a set of low and high flux 1 keV/amu H + and He + irradiation experiments performed on slabs of the Murchison CM2 carbonaceous chondrite. The low flux conditions for H + and He + irradiation were ~1-1.5 orders of magnitude lower than the high flux conditions, and each experiment was irradiated to a total fluence between ~3 × 10 16 to ~6 × 10 16 ions/cm 2 . Irradiation-induced changes in the surface chemistry and optical properties of the Murchison samples were evaluated using in situ X-ray photoelectron spectroscopy (XPS) and visible and near-infrared spectroscopy (VNIR). We characterized the microstructure and composition of ion damaged rims in focused ion beam (FIB) cross-sections extracted from olivine and matrix material in each irradiated Murchison slab using transmission electron microscopy (TEM). XPS results suggest that both low flux and high flux H + and He + irradiation cause minor sputtering of surface carbon as well as a reduction in the valence state of iron, from Fe 3+ to Fe 2+ . Slope bluing is observed in VNIR spectra of the irradiated samples which may reflect carbonization and dehydrogenation of organic species and contrasts with reddening trends associated with npFe 0 formation. Although we do not observe a strong flux-dependence on the crystallinity of ion-damaged olivine, TEM analyses reveal a variety of microstructures in all olivine FIB-sections, suggesting that crystallographic orientation affects amorphization efficiency. Analyses of matrix FIB-sections indicate that phyllosilicate alteration is mainly driven by He+ irradiation, where the higher incident flux leads to greater amorphization and the formation of more distinct ion-damaged layers, similar to smooth layers in returned Ryugu particles. TEM results also provide some evidence that higher ion flux leads to greater vesiculation, with He + irradiation being more efficient at vesiculation than H + irradiation, and that higher ion flux may promote the segregation of Mg and Si into laterally extensive lenses and layers in olivine samples. We discuss the implications of these findings for constraining the role that ion flux plays in the development of space weathering characteristics in silicate phases present in carbonaceous asteroidal regoliths. These results will be important for understanding the complexity of this process and how it operates on carbon-rich airless bodies like asteroids Bennu and Ryugu.

meteorites↗

GLUT-3 expression in human skeletal muscle

Muscle biopsy homogenates contain GLUT-3 mRNA and protein. Before these studies, it was unclear where GLUT-3 was located in muscle tissue. In situ hybridization using a midmolecule probe demonstrated GLUT-3 within all muscle fibers. Fluorescent-tagged antibody reacting with affinity-purified antibody directed at the carboxy-terminus demonstrated GLUT-3 protein in all fibers. Slow-twitch muscle fibers, identified by NADH-tetrazolium reductase staining, possessed more GLUT-3 protein than fast-twitch fibers. Electron microscopy using affinity-purified primary antibody and gold particle-tagged second antibody showed that the majority of GLUT-3 was in association with triads and transverse tubules inside the fiber. Strong GLUT-3 signals were seen in association with the few nerves that traversed muscle sections. Electron microscopic evaluation of human peripheral nerve demonstrated GLUT-3 within the axon, with many of the particles related to mitochondria. GLUT-3 protein was found in myelin but not in Schwann cells. GLUT-1 protein was not present in nerve cells, axons, myelin, or Schwann cells but was seen at the surface of the peripheral nerve in the perineurium. These studies demonstrated that GLUT-3 mRNA and protein are expressed throughout normal human skeletal muscle, but the protein is predominantly found in the triads of slow-twitch muscle fibers.

NASA Discipline Regulatory Physiology↗

Microstructural Characterization of Felsite Fragments From the Apollo Next Generation Sample Analysis (ANGSA) Double Drive Tube 73001/73002

While the Moon’s surface is dominated by mafic igneous products formed through the crystallization of the lunar magma ocean, and the subsequent eruption of mare basalts – felsic magmatic fragments (variably referred to as felsites, granites, rhyolites or granophyres) have been identified from a number of Apollo samples (e.g. 12013[1], 14321[2], 15405[3] and 73215[4]). Magmatic edifices like the Gruithuisen Domes – silicic constructs sometimes found proximal to the basaltic mare provinces filling nearside basins, may represent a petrogenetic origin. However, this is, is complicated by the fact that they apparently predate mare volcanism (e.g. [5]). Additionally, crater-counting indicates that these silicic surface features also postdate radiogenic ages of Apollo felsites [6]. Various modes of felsic magmatism have been invoked to explain the presence of felsic lithologies on the Moon, including: 1) fractional crystallization and silicate liquid immiscibility; 2) partial melting of lunar crust through basaltic underplating; and 3) fractional crystallization of the mare parent magmas. Although these models are plausible, based on known Apollo samples and lunar meteorites, they are complicated by the lack of sample lithologies with intermediate composition between basaltic magmas and the felsic components, and the fact that partial melting of many crustal rock types on the Moon (e.g., anorthosite, troctolites) are unlikely to form granites. Along with other unique magmatic lithologies, new felsites have been identified within the < 1 mm size fractions of the ANGSA double drive core tube (73001/73002) from Apollo 17 station 3, sampling the light mantle landslide deposit from the South Massif [7]. These additional examples of lunar felsite will help us to better constrain the processes that lead to the formation of these evolved lithologies. To do this, we have employed a gambit of high-resolution scanning electron microscopy (SEM) and scanning transmission electron microscopy (TEM) analytical techniques, including electron backscatter diffraction (EBSD), cathodoluminescence and high-angle annular dark field (HAADF) imaging. These data provide unique insights into the felsite mineralogy and microstructures including the coexistence of quartz and tridymite in many of the fragments. In addition, these analyses provide petrological context and assist targeted in situ secondary ion mass spectrometry (SIMS) measurements of the U-Pb systematics of accessory minerals, and the volatile abundances and D/H ratios of apatite grains identified within the clasts.

lunar↗

A technique for measuring in situ size distribution of aerosols

A multistage cascade impactor instrument employing piezoelectric crystals for real-time aerosol size distribution measurements is described in this paper. The instrument measures the aerosol mass concentration as a function of particle size in 10 size intervals ranging from 0.05 micrometers to 25 micrometers in diameter. The particles are then analyzed for elemental composition and morphology by means of scanning electron microscopy (SEM). Examples of particle size distributions in rocket motor exhaust plumes measured with the instrument are presented together with the elemental composition and morphology obtained by SEM.

Woods, D. C.↗

The Combined Detection of Morphological and Molecular Biomarkers: Implications for Astrobiology

Experience gathered by previous researchers during their hunt for evidence of early Earth life has shown the complexity in interpreting observations of possible microfossils and to establish the evidence to be positive. Similarly, the stillsimmering controversy on the nature of the nano-structures in Martian meteorite ALH84001 described by McKay et al. (1996) emphasizes the difficulties of conclusively identifying those structures as (a) fossilized bacterial cells and (b) establish their indigeneity. A better understanding of biological signatures in rocks is needed in order to identify traces of microbial life, which include morphological, mineralogical and chemical traces. It is thus considered crucial to tackle the problems emerging in the search for evidence of early life on Earth and in exopaleontological research with a multidisciplinary approach. With this is mind we applied surface sensitive Time of Flight-Secondary Ion Mass Spectroscopy (ToF-SIMS) to a previously described 25 m.y. old fossil bacterial biofilm. This technique allows in situ analysis with high mass resolution as well as molecular imaging of micron sized structures. As no extraction or derivatisation of the sample is required for ToF-SIMS analysis, electron microscopical investigation of the same samples subsequent to analysis is possible, thus allowing the combination of molecular and morphological biomarkers. The analysed fossil bacterial biofilms were associated with macrofossils from volcanoclastic lacustrine sediments from the Upper Oligocene Enspel formation (Germany). Preliminary scanning electron microscopy (SEM) studies have shown that a fossil structure interpreted as a coprolite purely consisted of fossilized bacterial biofilm. For ToF-SIMS investigation small particles were taken from the fossil biofilm and mounted onto Au-coated In-foil and analysed in a Phi Evans T-2000 TRIFT system. The ToF-SIMS analysed samples were Au/Pd-sputter coated and imaged using a Philips XL40 Field Emission Gun SEM (FEG-SEM). ToF-SIMS analysis of the organic rich fossil biofilm (TOC 29%) in the 0-100 Dalton (Da) range showed significant amounts of inorganic species, confirming the results obtained previously by EDX analysis, clearly showing the bacterial fossils to be mineralised. ToF-SIMS furthermore revealed the presence of a variety of low- and high-mass organic molecules and fragments thereof. These include peaks indicative of alkenes and alkanes, aromatic organic species and the polycyclic aromatic hydrocarbon naphthalene. More tentatively, peaks indicative of alkyl pyrroles and pyridyl-CH2 were identified. Other peaks of interest include peaks indicative of C(n)H(2n)O2 and C(n)H(2n-2)O2, which according to their general formula would suggest the presence of both saturated and unsaturated fatty acids although further in situ derivatisation experiments and GC-MS (Gas Chromatography MS) need to be applied to verify this beyond doubt. Furthermore, peaks at m/z 370, 384, 398, 412, 426, 440, 454 and 468 were identified, which indicate the potential presence of bacterial hopanes, a class of biomarkers indicative of bacteria. The main diagnostic peak for this group of chemicals is the fragment at m/z 191.18. Our studies conducted on purified hopane standards have shown that in the high-mass resolution mode differentiation of this diagnostic hopane peak and polyethylene at m/z 191.05 is possible. However, the spectra discussed here were collected in the lower resolution mapping mode, therefore this differentiation was not possible. The centroids of the possible hopane peaks obtained on the fossil biofilms are well within the range associated with bacterial hopanes. There is a strong possibility therefore that hopanoids may be associated with the fossil bacterial cells. Due to the non-destructive nature of ToF-SIMS, analysed samples can be studied using SEM, thus allowing the combination of morphological and molecular biomarkers. Subsequent SEM analysis of the ToF-SIMS analysed samples confirmed that the analysed material purely consists of fossil bacterial cells. This is thus the first successful effort to demonstrate the combination of spectral and morphological biomarkers. The advantages of highly sensitive non-destructive in situ analysis techniques for biomarker detection are invaluable, particularly with respect to envisaged Mars sample return missions, as it may allow us to identify remains and traces of former microbial life in both ancient terrestrial and extraterrestrial materials. This technique may prove particularly useful in the quest for extraterrestrial life with respect to precious extraterrestrial materials, as minute quantities are sufficient to conduct analysis.

Toporski, J.↗

Assessing Degradation of Advanced Coatings for Carbon/Carbon Composites

Carbon/carbon (C/C) composites are a well-utilized material system for hot structures to enable hypersonic flight. However, C/C materials are susceptible to attack by environmental degradation mechanisms, notably oxidation, which can limit the durability of components resulting in premature failure. Environmental barrier coatings (EBCs) have been developed to mitigate deleterious oxidation. Coating compositions based on silicon carbide (SiC) offer promise as a protective coating material for C/C composites. Under particular hypersonic flight conditions, a passivating silica scale can form at the surface of the EBC, acting as a barrier that can protect the underlying coating and substrate. However, the transition from passive to active oxidation, which varies with temperature and pressure, causes the formation of gaseous SiO that volatilizes leading to detrimental consumption of the SiC coating. In this work, arc-jet testing of SiC-based coatings developed to protect Advanced C/C-6 (ACC-6) was performed under a range of conditions to replicate varying oxidation conditions. In-situ optical emission spectroscopic measurements of the gas-surface interactions were collected and evaluated to render compositional degradation of the coating and underlying composite during arc-jet testing. Specimens were evaluated before, during and after arc-jet testing using destructive and non-destructive materials characterization methods, including optical and scanning electron microscopy and energy dispersive spectroscopy.

Coatings, Hypersonics, Composites↗

Predatory prokaryotes: predation and primary consumption evolved in bacteria

Two kinds of predatory bacteria have been observed and characterized by light and electron microscopy in samples from freshwater sulfurous lakes in northeastern Spain. The first bacterium, named Vampirococcus, is Gram-negative and ovoidal (0.6 micrometer wide). An anaerobic epibiont, it adheres to the surface of phototrophic bacteria (Chromatium spp.) by specific attachment structures and, as it grows and divides by fission, destroys its prey. An important in situ predatory role can be inferred for Vampirococcus from direct counts in natural samples. The second bacterium, named Daptobacter, is a Gram-negative, facultatively anaerobic straight rod (0.5 x 1.5 micrometers) with a single polar flagellum, which collides, penetrates, and grows inside the cytoplasm of its prey (several genera of Chromatiaceae). Considering also the well-known case of Bdellovibrio, a Gram-negative, aerobic curved rod that penetrates and divides in the periplasmic space of many chemotrophic Gram-negative bacteria, there are three types of predatory prokaryotes presently known (epibiotic, cytoplasmic, and periplasmic). Thus, we conclude that antagonistic relationships such as primary consumption, predation, and scavenging had already evolved in microbial ecosystems prior to the appearance of eukaryotes. Furthermore, because they represent methods by which prokaryotes can penetrate other prokaryotes in the absence of phagocytosis, these associations can be considered preadaptation for the origin of intracellular organelles.

Non-NASA Center↗

Bosch Carbon Catalyst Regeneration in Water II: Analysis of Bosch Catalyst Beads Throughout the Initial Regeneration Process

Catalyst integrity is an important factor in reactor longevity since it changes the effectiveness of a reaction. A Carbon Formation Reactor (CFR), used within Series Bosch (S-Bosch), utilizes an iron alloy catalyst to convert carbon monoxide and hydrogen into water and solid carbon. The catalyst promotes the formation of carbon to such an extent that pressure-causing clogs form within the reactor and reaction sites on the catalyst become limited. To remove carbon from both the reactor and the surface of the iron alloy catalyst, a technique was developed that utilizes water, an In-Situ Resource Utilization (ISRU) Resource, and agitation to regenerate the reactor. To ascertain catalyst integrity throughout this regenerative process, sample catalyst beads were taken before and after the carbon formation reaction, and then after the regeneration process. Additionally, wastewater from the regeneration process was sampled. The sampled beads and wastewater were observed under a Scanning Electron Microscopy (SEM) microscope and the beads were chemically etched to determine if the catalyst had degraded at any point during this process, and if catalyst was lost. Minimal catalyst degradation was observed after carbon formation in the CFR.

regeneration↗

Bosch Carbon Catalyst Regeneration in Water II: Analysis of Bosch Catalyst Beads Throughout the Initial Regeneration Process

Catalyst integrity is an important factor in reactor longevity since it changes the effectiveness of a reaction. A Carbon Formation Reactor (CFR), used within Series Bosch (S-Bosch), utilizes an iron alloy catalyst to convert carbon monoxide and hydrogen into water and solid carbon. The catalyst promotes the formation of carbon to such an extent that pressure-causing clogs form within the reactor and reaction sites on the catalyst become limited. To remove carbon from both the reactor and the surface of the iron alloy catalyst, a technique was developed that utilizes water, an In-Situ Resource Utilization (ISRU) Resource, and agitation to regenerate the reactor. To ascertain catalyst integrity throughout this regenerative process, sample catalyst beads were taken before and after the carbon formation reaction, and then after the regeneration process. Additionally, wastewater from the regeneration process was sampled. The sampled beads and wastewater were observed under a Scanning Electron Microscopy (SEM) microscope and the beads were chemically etched to determine if the catalyst had degraded at any point during this process, and if catalyst was lost. Minimal catalyst degradation was observed after carbon formation in the CFR.

Series Bosch↗

Low-Temperature Production of Cosmic Grains Analogs From Gas-Phase Molecular Precursors with the NASA Ames' COSmIC Facility

Complex carbon molecules and ions are ubiquitous in space and form the building blocks of carbonaceous cosmic dust grains, ultimately contributing to the formation of planets. Here, we report the first experimental investigations of the low temperature chemical pathways leading to the production of cosmic grain analogs from gas phase molecular precursors in order to better understand the evolution of cosmic carbon. The experiments were performed using the COsmic SImulation Chamber (COSmIC) to generate and characterize grains formed from gas phase precursors under controlled conditions representative of astrophysical environments [1]. Using COSmIC, it is possible to investigate the evolution of cosmic carbon from the formation of neutral and ionized gas phase hydrocarbons and PAHs [2], to carbon grains [3, 4]. This is achieved by using a discharge nozzle to (1) produce an adiabatic jet expansion and cool down Ar-hydrocarbon/PAH gas mixtures to astrophysically relevant temperature (150 K) before inducing chemistry by generating a plasma discharge in the stream of the expansion. This plasma-induced chemistry results in the formation of complex molecules and solid particles, analogs of cosmic grains. Solid grains are produced in-situ in the plasma expansion, carried by the accelerated gas in the expansion, and collected on substrates placed a few centimeters downstream of the electrodes. The results of a preliminary solid phase ex-situ analysis of cosmic grain analogs produced at low temperature in COSmIC from gas mixtures including molecular precursors of cosmic carbon grains, i.e., such as CH4 and C2H2 found in circumstellar ejecta of late C stars [3] as well as PAHs ubiquitously detected in IR emission bands seen in galactic and extragalactic environments [4] will be discussed. Scanning Electron Microscopy imaging was used to provide insight on the morphology and growth structure of the grains produced in COSmIC, and to investigate how the precursors used to produce the grains affect these parameters [3]. Laser desorption mass spectrometry was used to identify the molecules making up the main structures within the condensed grains [4]. NIR to FIR optical properties are characterized to provide critical information (functional groups, optical constants) to the scientific community, for use in radiative transfer models in particular, and to help decipher and enhance the return data from space observations.

F. Salama↗

Building and Breaking Carbon Composites with REACTER

Carbon composites have become indispensable for aerospace and other high-performance applications, and a detailed picture of their morphology and failure mechanisms remains difficult to obtain through experiment. REACTER is a versatile computational modeling tool for atomistic molecular dynamics designed to model chemical reactions at the speed and length scales of classical force fields.1 In this work, several recent features of REACTER were applied to the creation and subsequent mechanical testing of two classes of carbon composites, carbon-fiber reinforced polymers (CFRP) and carbon nanotube (CNT) composites. Carbon fiber core morphologies were created by the method of Desai et al.,2 but using the advanced reaction constraints framework of REACTER, their proposed multistep procedure was reduced to a single uninterrupted molecular dynamics simulation. The carbon fiber filler was embedded into a polymer matrix by simulated in situ polymerization of several thermosetting resins, including bismaleimide and polyarylacetylene, to obtain the final CFRP model. To generate the second class of carbon composite, CNT networks were grown dynamically using the new ‘create atoms’ feature of REACTER, and similarly infiltrated with resin to obtain CNT composites. The resulting models were compared directly to experiment using simulated high resolution transmission electron microscopy and x-ray diffraction. Failure mechanisms were elucidated by simulating mechanically induced bond breaking, as characterized by third-order DFT-based tight-binding (DFTB3) simulations, via a reaction constraint on the total potential energy of the involved atoms.

Molecular Dynamics↗