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A wide variety of lunar sample and meteorite studies were performed. Abstracts of the most recent reports are also attached. Experimental techniques employed have included scanning electron microscopy, transmission electron microscopy, Mossbauer spectroscopy, atomic absorption analysis and a variety of simulation studies.
Major accomplishments underlying the basic understanding of cyanobacterial resistance to salt tolerance and osmotic stress were made. The methodology proposed included: the tracing of the pathways of formation of osmoregulatory solutes by traditional methods involving C-14 labelled substrates; gas chromatography; amino acid analysis; X-ray analysis using scanning transmission electron microscopy; and most importantly, C-13 labelled substrates, followed by Nuclear Magnetic Resonance (NMR) spectroscopy. It was found that the cyanobacteria employ a diversity of organic, osmoregulatory solutes. Osmoregulatory solutes were found to serve four functions: adjustment of water activity, noninhibition of enzymes; lowering of K sub m of enzymes to allow functioning at normal levels when the intracellular salt accumulates, and extending the pH optimum of enzymes as intracellular pH rises due to proton-potassium ion pump action during osmoregulation. Differences in osmoregulatory solutes may, but are not always, be attributed to differences in nutritional capabilities. The mechanism of osmoregulation and concomitant salt tolerance in halophilic cyanobacteria was elucidated. The activities of betaine and S-Adenosylhomocysteine hydrolase are discussed.
The effect of anodization in NaOH, H2SO4, and amine salts on the surface chemistry of carbon fibers was examined by X-ray photoelectron spectroscopy (XPS). The surfaces of carbon fibers after anodization in NaOH and H2SO4 were examined by scanning transmission electron microscopy (STEM), angular dependent XPS, UV absorption spectroscopy of the anodization bath, secondary ion mass spectrometry, and polar/dispersive surface energy analysis. Hercules AS-4, Dexter Hysol XAS, and Union Carbide T-300 fibers were examined by STEM, angular dependent XPS, and breaking strength measurement before and after commercial surface treatment. Oxygen and nitrogen were added to the fiber surfaces by anodization in amine salts. Analysis of the plasmon peak in the carbon 1s signal indicated that H2SO4 anodization affected the morphological structure of the carbon fiber surface. The work of adhesion of carbon fibers to thermoplastic resins was calculated using the geometric mean relationship. A correlation was observed between the dispersive component of the work of adhesion and the interfacial adhesion.
A summary of ongoing research on the characterization of a continuous fiber reinforced SiC/Ti-24Al-11Nb (at percent) composite is presented. The powder metallurgy fabrication technique is described as are the nondestructive evaluation results of the as-fabricated composite plates. Tensile properties of the SiC fiber, the matrix material, and the 0-deg SiC/Ti-24Al-11Nb composite (fibers oriented unidirectionally, parallel to the loading axis) from room temperature to 1100 C are presented and discussed with regard to the resultant fractography. The as-fabricated fiber-matrix interface has been examined by scanning transmission electron microscopy and the compounds present in the reaction zone have been identified. Fiber-matrix interaction and stability of the matrix near the fiber is characterized at 815, 985, and 1200 C from 1 to 500 hr. Measurements of the fiber-matrix reaction, the loss of C-rich coating from the surface of the SiC fiber, and the growth of the Beta depleted zone in the matrix adjacent to the fiber are presented. These data and the difference in coefficient of thermal expansion between the fiber and the matrix are discussed in terms of their likely effects on mechanical properties.
This paper discusses the methodologies used for surface property measurement of thin films and coatings, lubricants, and materials in the field of tribology. Surface diagnostic techniques include scanning electron microscopy, transmission electron microscopy, atomic force microscopy, stylus profilometry, x-ray diffraction, electron diffraction, Raman spectroscopy, Rutherford backscattering, elastic recoil spectroscopy, and tribology examination. Each diagnostic technique provides specific measurement results in its own unique way. In due course it should be possible to coordinate the different pieces of information provided by these diagnostic techniques into a coherent self-consistent description of the surface properties. Examples are given on the nature and character of thin diamond films.
Tensile strengths of as-received Hi-Nicalon and Sylramic fibers and those having monazite surface coatings, deposited by atmospheric pressure chemical vapor deposition, were measured at room temperature and the Weibull statistical parameters determined. The average tensile strengths of uncoated Hi-Nicalon and Sylramic fibers were 3.19 +/- 0.73 and 2.78 +/- 0.53 GPa with a Weibull modulus of 5.41 and 5.52, respectively. The monazite-coated Hi-Nicalon and Sylramic fibers showed strength loss of approx. 10 and 15 percent, respectively, compared with the as-received fibers. The elemental compositions of the fibers and the coatings were analyzed using scanning Auger microprobe and energy dispersive X-ray spectroscopy. The LaPO4 coating on Hi-Nicalon fibers was approximately stoichiometric and about 50 nm thick. The coating on the Sylramic fibers extended to a depth of about 100 to 150 nm. The coating may have been stoichiometric LaPO4 in the first 30 to 40 nm of the layer. However, the surface roughness of Sylramic fiber made this profile somewhat difficult to interpret. Microstructural analyses of the fibers and the coatings were done by scanning electron microscopy, transmission electron microscopy, and selected area electron diffraction. Hi-Nicalon fiber consists of fine beta-SiC nanocrystals ranging in size from 1 to 30 mn embedded in an amorphous matrix. Sylramic is a polycrystalline stoichiometric silicon carbide fiber consisting of submicron beta-SiC crystallites ranging from 100 to 300 nm. Small amount of TiB2 nanocrystallites (approx. 50 nm) are also present. The LaPO4 coating on Hi-Nicalon fibers consisted of a chain of peanut shape particles having monazite-(La) structure. The coating on Sylramic fibers consisted of two layers. The inner layer was a chain of peanut shape particles having monazite-(La) structure. The outer layer was comprised of much smaller particles with a microcrystalline structure.
The commercial potential of chemical-vapor-deposited (CVD) diamond films has been established and a number of applications have been identified through university, industry, and government research studies. This paper discusses the methodologies used for property measurement and diagnostic of CVD diamond films and coatings. Measurement and diagnostic techniques studied include scanning electron microscopy, transmission electron microscopy, atomic force microscopy, stylus profilometry, x-ray diffraction, electron diffraction, Raman spectroscopy, Rutherford backscattering, elastic recoil spectroscopy, and friction examination. Each measurement and diagnostic technique provides unique information. A combination of techniques can provide the technical information required to understand the quality and properties of CVD diamond films, which are important to their application in specific component systems and environments. In this study the combination of measurement and diagnostic techniques was successfully applied to correlate deposition parameters and resultant diamond film composition, crystallinity, grain size, surface roughness, and coefficient of friction.
Preferential oriented multiwalled carbon nanotubes were prepared by the injection chemical vapor deposition (CVD) method using either cyclopentadienyliron dicarbonyl dimer or cycloctatetraene iron tricarbonyl as the iron catalyst source. The catalyst precursors were dissolved in toluene as the carrier solvent for the injections. The concentration of the catalyst was found to influence both the growth of the nanotubes as well as the amount of iron in the deposited material. As deposited the multiwalled carbon nanotubes contained as little as 2.8% iron by weight. The material was deposited onto tantalum foil and fused silica substrates. The nanotubes were characterized by scanning electron microscopy, transmission electron microscopy, Raman spectroscopy and thermogravimetric analysis. This synthetic route provides a simple and scalable method to deposit MWNTs with a low defect density, low metal content and preferred orientation.
Brownleeite is a manganese silicide, ideally stoichiometric MnSi, not previously observed in nature until its discovery within an interplanetary dust particle (IDP) that likely originated from a comet [1]. Three discrete brownleeite grains in the IDP L2055 I3 (4 microns in size, hereafter IDP I3) were identified with maximum dimensions of 100, 250 and 600 nm and fully analyzed using scanning-transmission electron microscopy (STEM) [1]. One of the grains (100 nm in size) was poikilitically enclosed by low-Fe, Mn-enriched (LIME) olivine. LIME olivine is epitaxial to the brownleeite with the brownleeite (200) parallel to the olivine c* [1]. LIME olivine is an enigmatic phase first reported from chondritic porous IDPs and some unequilibrated ordinary chondrites [ 2], that is commonly observed in chondritic-porous IDPs. Recently, LIME olivine has been also found in comet Wild-2 (Stardust) samples [3], indicating that LIME olivine is a common mineral component of comets. LIME olivine has been proposed to form as a high temperature condensate in the protosolar nebula [2]. Brownleeite grains also likely formed as high-temperature condensates either in the early Solar System or in the outflow of an evolved star or supernova explosion [1]. The isotopic composition of the brownleeite grains may strongly constrain their ultimate source. To test this hypothesis, we performed isotopic analyses of the brownleeite and the associated LIME olivine, using the NASA/JSC NanoSIMS 50L ion microprobe.
The morphology, mineralogy, chemical composition and optical properties of lunar soils show distinct correlations as a function of grain size and origin [1,2,3]. In the <20 m size fraction, there is an increased correlation between lunar surface properties observed through remote sensing techniques and those attributed to space weathering phenomenae [1,2]. Despite the establishment of recognizable trends in lunar grains <20 in size [1,2,3], the size fraction < 10 m is characterized as a collective population of grains without subdivision. This investigation focuses specifically on grains in the <1 m diameter size fraction for both highland and mare derived soils. The properties of these materials provide the focus for many aspects of lunar research including the nature of space weathering on surface properties, electrostatic grain transport [4,5] and dusty plasmas [5]. In this study, we have used analytical transmission and scanning transmission electron microscopy (S/TEM) to characterize the mineralogy type, microstructure and major element compositions of grains in this important size range in lunar soils.
The Sutter's Mill meteorite is a newly fallen carbonaceous chondrite that was collected and curated quickly after its fall. Preliminary petrographic and isotopic investigations suggest affinities to the CM2 carbonaceous chondrites. The primitive nature of this meteorite and its rapid recovery provide an opportunity to investigate primordial solar system organic matter in a unique new sample. Here we report in-situ analyses of organic nanoglobules in the Sutter's Mill meteorite using UV fluorescence imaging, Fourier-transform infrared spectroscopy (FTIR), scanning transmission electron microscopy (STEM), NanoSIMS, and ultrafast two-step laser mass spectrometry (ultra-L2MS).
The Sutter s Mill meteorite is a newly fallen carbonaceous chondrite that was collected and curated quickly after its fall [1]. Preliminary petrographic and isotopic investigations suggest affinities to the CM2 carbonaceous chondrites. The primitive nature of this meteorite and its rapid recovery provide an opportunity to investigate primordial solar system organic matter in a unique new sample. Organic matter in primitive meteorites and chondritic porous interplanetary dust particles (CP IDPs) is commonly enriched in D/H and N-15/N-14 relative to terrestrial values [2-4]. These anomalies are ascribed to the partial preservation of presolar cold molecular cloud material [2]. Some meteorites and IDPs contain gm-size inclusions with extreme H and N isotopic anomalies [3-5], possibly due to preserved primordial organic grains. The abundance and isotopic composition of C in Sutter's Mill were found to be similar to the Tagish Lake meteorite [6]. In the Tagish Lake meteorite, the principle carriers of large H and N isotopic anomalies are sub-micron hollow organic spherules known as organic nanoglobules [7]. Organic nanoglobules are commonly distributed among primitive meteorites [8, 9] and cometary samples [10]. Here we report in-situ analyses of organic nano-globules in the Sutter's Mill meteorite using UV fluorescence imaging, Fourier-transform infrared spectroscopy (FTIR), scanning transmission electron microscopy (STEM), NanoSIMS, and ultrafast two-step laser mass spectrometry (ultra-L2MS).
Preferential oriented multiwalled carbon nanotubes were prepared by the injection chemical vapor deposition (CVD) method using either cyclopentadienyliron dicarbonyl dimer or cyclooctatetraene iron tricarbonyl as the iron catalyst source. The catalyst precursors were dissolved in toluene as the carrier solvent for the injections. The concentration of the catalyst was found to influence both the growth (i.e., MWNT orientation) of the nanotubes, as well as the amount of iron in the deposited material. As deposited, the multiwalled carbon nanotubes contained as little as 2.8% iron by weight. The material was deposited onto tantalum foil and fused silica substrates. The nanotubes were characterized by scanning electron microscopy, transmission electron microscopy, Raman spectroscopy and thermogravimetric analysis. This synthetic route provides a simple and scalable method to deposit MWNTs with a low defect density, low metal content and a preferred orientation. Subsequently, a small start-up was founded to commercialize the deposition equipment. The contrast between the research and entrepreneurial environments will be discussed.
In this study, local chemical and structural changes along superlattice intrinsic stacking faults combine to represent an atomic-scale phase transformation. In order to elicit stacking fault shear, creep tests of two different single crystal Ni-base superalloys, ME501 and CMSX-4, were performed near 750 degrees Centigrade using stresses of 552 megapascals and 750 megapascals, respectively. Through high resolution Scanning Transmission Electron Microscopy (STEM) and state-of-the-art energy dispersive x-ray spectroscopy, ordered compositional changes were measured along SISFs (Superlattice Intrinsic Stacking Faults) in both alloys. For both instances, the elemental segregation and local crystal structure present along the SISFs are consistent with a nanoscale to D019 (ordering of a hexagonal close-packed crystal) phase transformation. Another notable observation is prominent Cr- and Co-rich Cottrell atmospheres and new evidence of more complex reordering processes responsible for the formation of these faults. These findings are further supported using density functional theory calculations and High Angle Annular Dark Field (HAADF) STEM image simulations.
In this study, two commercially similar polycrystalline Ni-based disk superalloys (LSHR and ME3) were creep tested at 760C and 552MPa to approximately 0.3% plastic strain. LSHR consistently displayed superior creep properties at this stress/temperature regime even though the microstructural characteristics between the two alloys were comparable. High resolution structural and chemical analysis, however, revealed significant differences between the two alloys among active gamma prime shearing modes involving superlattice intrinsic and extrinsic stacking faults. In ME3, Co and Cr segregation and Ni and Al depletion were observed along the intrinsic faults - revealing a gamma prime -to- gamma phase transformation. Conversely in LSHR, an alloy with a higher W content, Co and W segregation was observed along the intrinsic faults. This observation combined with scanning transmission electron microscopy (STEM) simulations confirm a gamma prime-to-D019 phase transformation along the intrinsic faults in LSHR. Using experimental observations and density functional theory calculations, a novel local phase transformation strengthening mechanism is proposed that could be further utilized to improve the high temperature creep capabilities of Ni-base disk alloys.
The high-pressure polymorph of zircon (Zr2SiO4) is reidite, a phase with the scheelite structure that was first discovered to form at ca. 12 GPa in static high-pressure experiments [1]. Reidite was subsequently found to occur in naturally shocked zircons from several terrestrial impact localities [2,3], as well as in shock recovery-reverberation experiments performed above 20 GPa [4]. The nature and distribution of reidite occurrences in terrestrial impact localities has pointed to its potential use as a shock pressure indicator, as well as to the importance of understanding its age-reset effects in zircon geochronology [3]. In this study we have used coordinated SEM/Electron Backscatter Diffraction (EBSD) and Field-Emission Scanning Transmission Electron Microscopy (FE-STEM) to study the micro- and nanostructure of reidite and its shocked zircon host produced at 21.2 GPa under experimental shock recovery/reverberation conditions [5]. Our results document the TEM microstructure of reidite formed at a 21.2 GPa experimental shock pressure that is significantly lower than that observed in previous studies [4]. At these conditions the sample developed a diverse set of microstructures that have not been previously documented on the TEM scale.
The flux of objects impacting the surfaces of solar system airless bodies is dominated by micrometeoroids less than 1 mm diameter whose impact effects play a major role in the space weathering of airless body surfaces. To obtain better understanding of how small scale impact effects vary as a function of impact speed in an important lunar and asteroidal mineral, we produced artificial microcraters in San Carlos olivine using Fe metal dust particles 0.10 to 5 µm in diameter electrostatically accelerated to speeds between 0.35 to 25 km s-1. The crater morphologies, size distrrubiton and microstruc-tures were characterized by field-emission SEM (FE-SEM) and also by FIB cross sectioning of selected craters for field-emission scanning transmission electron microscopy (FE-STEM). These same techniques were also applied to study a natural 20 µm-diameter microcrater in a olivine grain on the surface of lunar rock 12075. Measured microcrater diameters in the experimental sample range between 0.20 to 5 µm with larger craters having more irregular outlines dominated by spallation fractures. FE-SEM and FE-STEM imaging docu-ment the formation of shock melt in the size population of experimental craters below approximately 1 µm in diameter, corresponding to particle impact speeds in the 10-25 km s-1 range. The natural olivine crater exhibits similar shock melt features along the perimeter of its cavity, but the shock melt also contains nanophase Fe metal particles, something not observed in the experimental samples. FE-STEM imaging of the experimental craters reveals complex shock-generated dislocation and nanofracture microstructures in zones extend-ing 1-2 µm into the olivine from the crater cavity. The natural microcrater shows a lower density of shock-generated disloca-tions that extends a factor of 2 deeper into the the olivine than in the experimental samples.
The Moon’s surface is directly exposed to the space environment and subject to alteration by space weathering. One agent of space weathering, the solar wind, enriches the lunar surface with helium. Although we understand how helium is delivered to the Moon, certain aspects of helium concentration processes on the surface remain unknown, such as why impact-generated glass aggregates contain more helium than equally sized soil grains of other types. Here we have analyzed the contents of vesicular iron nanoparticles in lunar impact glasses using aberration-corrected scanning transmission electron microscopy and electron energy loss spectroscopy and show that the nanoparticles contain high concentrations of helium (10-24 atoms/nm3). The widespread occurrence of vesicular iron nanoparticles among lunar samples suggests that they may be an important helium reservoir. These results also suggest that space weathering of iron-rich minerals plays a role in helium sequestration on the Moon and potentially on other airless bodies.