Mineralogy of the lunar clinopyroxenes, augite and pigeonite
Apollo 11 lunar rocks and fines, examining clinopyroxenes augite and pigeonite by single crystal X ray diffraction microprobe optical and electron optical techniques
Bence, A. E.↗
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Relative cooling rates of mare basalts at the Apollo 12 and 15 sites as estimated from pyroxene exsolution data
X-ray single-crystal diffraction studies, supplemented by electron microprobe analyses of core pigeonites and rim augites from rocks 12031, 15085, 15475, and 15495, have been used to suggest cooling rates for these and other Apollo 12 and 15 rocks studied by similar methods. The extent of subsolidus phase separation of pyroxenes is used as a measure of the cooling rate. The results were interpreted in terms of model cooling histories of a lava flow whose thickness was estimated from the absolute cooling rates obtained by cooling rate experiments and by temperature-time variation through an extrusive flow computed by employing simplified theory of Jaeger. All available data on the exsolution and cation distributions of pyroxenes from Apollo 12 and 15 samples at present are consistent with the hypothesis that these rocks were derived from the top and interior of lava flows with thicknesses of 4-10 m. A process for exsolution of augite from a host pigeonite on (100) has been related to its low-calcium content.
Takeda, H.↗
Corrosion behavior of surface films on boron-implanted high purity iron and stainless steels
Boron (dose, 2 x 10 to the 17th ions/sq cm) was implanted into high purity iron, AISI 316 austenitic stainless steel, and AISI 440C martensitic stainless steel, at 40 keV. The film structure of implanted samples was examined and characterized by contrast and diffraction analyses utilizing transmission electron microscopy. The effect of B(+) ion implantation on the corrosion behavior was studied using the potentiodynamic polarization technique. Tests were performed in deaerated 1 N H2SO4 and 0.1 M NaCl solutions. Scanning electron microscopy was used to examine the morphology of the corroded surfaces after testing.
Kim, H. J.↗
Crystallization kinetics of BaO-Al2O3-SiO2 glasses
Barium aluminosilicate glasses are being investigated as matrix materials in high-temperature ceramic composites for structural applications. Kinetics of crystallization of two refractory glass compositions in the barium aluminosilicate system were studied by differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). From variable heating rate DTA, the crystallization activation energies for glass compositions (wt percent) 10BaO-38Al2O3-51SiO2-1MoO3 (glass A) and 39BaO-25Al2O3-35SiO2-1MoO3 (glass B) were determined to be 553 and 558 kJ/mol, respectively. On thermal treatment, the crystalline phases in glasses A and B were identified as mullite (3Al2O3-2SiO2) and hexacelsian (BaO-Al2O3-2SiO2), respectively. Hexacelsian is a high-temperature polymorph which is metastable below 1590 C. It undergoes structural transformation into the orthorhombic form at approximately 300 C accompanied by a large volume change which is undesirable for structural applications. A process needs to be developed where stable monoclinic celsian, rather than hexacelsian, precipitates out as the crystal phase in glass B.
Bansal, Narottam P.↗
Crystallization kinetics of BaO-Al2O3-SiO2 glasses
Barium aluminosilicate glasses are being investigated as matrix materials in high-temperature ceramic composites for structural applications. Kinetics of crystallization of two refractory glass compositions in the barium aluminosilicate system were studied by differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). From variable heating rate DTA, the crystallization activation energies for glass compositions (wt percent) 10BaO-38Al2O3-51SiO2-1MoO3 (glass A) and 39BaO-25Al2O3-35SiO2-1MoO3 (glass B) were determined to be 553 and 558 kJ/mol, respectively. On thermal treatment, the crystalline phases in glasses A and B were identified as mullite (3Al2O3-2SiO2) and hexacelsian (BaO-Al2O3-2SiO2), respectively. Hexacelsian is a high-temperature polymorph which is metastable below 1590 C. It undergoes structural transformation into the orthorhombic form at approximately 300 C accompanied by a large volume change which is undesirable for structural applications. A process needs to be developed where stable monoclinic celsian, rather than hexacelsian, precipitates out as the crystal phase in glass B.
Bansal, Narottam P.↗
Growth and characterization of CdTe on GaAs/Si substrates
Epitaxial CdTe has been grown on both (100) GaAs/Si and (111) GaAs/Si substrates. A combination of molecular beam epitaxy and metal organic chemical vapor deposition have been employed to achieve this growth. The GaAs layers are grown in Si substrates by molecular beam epitaxy, followed by the growth of CdTe on GaAs/Si substra by metalorganic chemical vapor deposition. X-ray diffraction, photoluminescence, and scanning electron microscopy have been used to characterize the CdTe films.
Radhakrishnan, G.↗
Surface migration and volume diffusion in the AgGaSe2-Ag2Se system
Surface migration and volume diffusion in the Ag2Se-AgGaSe2 system were investigated using reactive diffusion couples which were analyzed by X-ray diffraction, optical microscopy, and electron probe microanalysis. The surface diffusivities of all mobile species are found to be much larger than volume diffusivities. The results of the study suggest that Se moves together with Ag and Ga to maintain binary (Ag2Se and Ga2Se3) stoichiometry and electroneutrality. The dominance of surface migration kinetics can account for the uniform annihilation of second-phase precipitates during heat treatments.
Kim, N.-H.↗
Thermal spray processing
Thermal spray processing has been used for a number of years to cost-effecticely apply TBC's for a wide range of heat engine applications. In particular, bond coats are applied by plasma spray and HVOF techniques and partially-stabilized zirconia top coats are applied by plasma spray methods. Thermal spray involves melting and rapid transport of the molten particles to the substrate, where high-rate solidification and coating build-up occur. It is the very nature of this melt processing that leads to the unique layered microstructure, as well as the apparent imperfections, so readily identified with thermal spray. Modeling the process, process-induced residual stresses, and thermal conductivity will be discussed in light of a new understanding of porosity and its anisotropy. Microcracking can be understood using new approaches, allowing a fuller view of the processing-performance connection. Detailed electron microscopic, novel neutron diffraction and fracture analysis of the deposits can lead to a better understanding of how overall microstructure can be controlled to influence critical properties of the deposited TBC system.
Herman, H.↗
Quantitative reflectance spectroscopy of buddingtonite from the Cuprite mining district, Nevada
Buddingtonite, an ammonium-bearing feldspar diagnostic of volcanic-hosted alteration, can be identified and, in some cases, quantitatively measured using short-wave infrared (SWIR) reflectance spectroscopy. In this study over 200 samples from Cuprite, Nevada, were evaluated by X ray diffraction, chemical analysis, scanning electron microscopy, and SWIR reflectance spectroscopy with the objective of developing a quantitative remote-sensing technique for rapid determination of the amount of ammonium or buddingtonite present, and its distribution across the site. Based upon the Hapke theory of radiative transfer from particulate surfaces, spectra from quantitative, physical mixtures were compared with computed mixture spectra. We hypothesized that the concentration of ammonium in each sample is related to the size and shape of the ammonium absorption bands and tested this hypothesis for samples of relatively pure buddingtonite. We found that the band depth of the 2.12-micron NH4 feature is linearly related to the NH4 concentration for the Cuprite buddingtonite, and that the relationship is approximately exponential for a larger range of NH4 concentrations. Associated minerals such as smectite and jarosite suppress the depth of the 2.12-micron NH4 absorption band. Quantitative reflectance spectroscopy is possible when the effects of these associated minerals are also considered.
Felzer, Benjamin↗
Volumetric Near-Field Microwave Plasma Generation
A periodic series of microwave-induced plasmoids is generated using the outgoing wave from a microwave horn and the reflected wave from a nearby on-axis concave reflector. The plasmoids are spaced at half-wavelength separations according to a standing-wave pattern. The plasmoids are enhanced by an effective focusing in the near field of the horn (Fresnel region) as a result of a diffractive narrowing. Optical imaging, electron density, and rotational temperature measurements characterize the near field plasma region. Volumetric microwave discharges may have application to combustion ignition in scramjet engines.
Exton, R. J.↗
Oxidation of ZrB2-and HfB2-Based Ultra-High Temperature Ceramics: Effects of Ta Additions
Several compositions of ZrB2- and HfB2-based Ultra-High Temperature Ceramics (UHTC) were oxidized in stagnant air at 1627 C in ten minute cycles for times up to 100 minutes. These compositions include: ZrB2 - 20v% SiC, HfB2 - 20v% SiC, ZrB2 - 20v% SiC - 20v% TaSi2, ZrB2 - 33v% SiC, HfB2 - 20v% SiC - 20v% TaSi2, and ZrB2 - 20v% SiC - 20v% TaC. The weight change due to oxidation was recorded. The ZrB2 - 20v% SiC - 20v% TaSi2 composition was also oxidized in stagnant air at 1927 C and in an arc jet atmosphere. Samples were analyzed after oxidation by x-ray diffraction, field emission scanning electron microscopy, and energy dispersive spectroscopy to determine the reaction products and to observe the microstructure. The ZrB2 - 20v% SiC - 20v% TaSi2 showed the lowest oxidation rate at 1627 C, but performed poorly under the more extreme tests due to liquid phase formation. Effects of Ta-additions on the oxidation of the diboride-based UHTC are discussed.
Opila, Elizabeth↗
Oxidation of High-temperature Alloy Wires in Dry Oxygen and Water Vapor
Small diameter wires (150 to 250 microns) of the high temperature alloys Haynes 188, Haynes 230, Haynes 230, Haynes 214, Kanthal Al and PM2000 were oxidized at 1204 C in dry oxygen or 50% H2O /50% O2 for 70 Hours. The oxidation kinetics were monitored using a thermogravimetric technique. Oxide phase composition and morphology of the oxidized wires were determined by X-ray diffraction,field emission scanning electron microscopy, and energy dispersive spectroscopy. The alumina-forming alloys, Kanthal Al and PM2000, out-performed the chromia-forming alloys under this conditions. PM2000 was recommended as the most promising candidate for advanced hybrid seal applications for space reentry control surface seals or hypersonic propulsion system seals. This study also demonstrated that thermogravimetric analysis of small diameter wires is a powerful technique for the study of oxide volatility, oxide adherence, and breakaway oxidation.
Opila, Elizabeth J.↗
Thermal Infrared Emission Spectroscopy of Synthetic Allophane and its Potential Formation on Mars
Allophane is a poorly-crystalline, hydrous aluminosilicate with variable Si/Al ratios approx.0.5-1 and a metastable precursor of clay minerals. On Earth, it forms rapidly by aqueous alteration of volcanic glass under neutral to slightly acidic conditions [1]. Based on in situ chemical measurements and the identification of alteration phases [2-4], the Martian surface is interpreted to have been chemically weathered on local to regional scales. Chemical models of altered surfaces detected by the Mars Exploration Rover Spirit in Gusev crater suggest the presence of an allophane-like alteration product [3]. Thermal infrared (TIR) spectroscopy and spectral deconvolution models are primary tools for determining the mineralogy of the Martian surface [5]. Spectral models of data from the Thermal Emission Spectrometer (TES) indicate a global compositional dichotomy, where high latitudes tend to be enriched in a high-silica material [6,7], interpreted as high-silica, K-rich volcanic glass [6,8]. However, later interpretations proposed that the high-silica material may be an alteration product (such as amorphous silica, clay minerals, or allophane) and that high latitude surfaces are chemically weathered [9-11]. A TIR spectral library of pure minerals is available for the public [12], but it does not contain allophane spectra. The identification of allophane on the Martian surface would indicate high water activity at the time of its formation and would help constrain the aqueous alteration environment [13,14]. The addition of allophane to the spectral library is necessary to address the global compositional dichotomy. In this study, we characterize a synthetic allophane by IR spectroscopy, X-ray diffraction (XRD), and transmission electron microscopy (TEM) to create an IR emission spectrum of pure allophane for the Mars science community to use in Martian spectral models.
Rampe, E. B.↗
A CAI in the Ivuna CI1 Chondrite
We have recently discovered the first well-preserved calcium aluminum-rich inclusion (CAI) in a CI1 chondrite (Ivuna). Previously, all CI1 chondrites were thought to be devoid of preserved CAI and chondrules due to the near total aqueous alteration to which their parent body (bodies) have been subjected. The CAI is roughly spherical, but with a slight teardrop geometry and a maximum diameter of 170 microns (fig. 1). It lacks any Wark-Lovering Rim. Incipient aqueous alteration, and probably shock, have rendered large portions of the CAI poorly crystalline. It is extremely fine-grained, with only a few grains exceeding 10 microns. We have performed electron microprobe analyses (EPMA), FEG-SEM imaging and element mapping, as well as electron back-scattered diffraction (EBSD) and synchrotron X-ray diffraction (SXRD) in order to determine the fundamental characteristics of this apparently unique object.
Frank, David R.↗
The Shock State of Itokawa Sample
One of the fundamental aspects of any astromaterial is its shock history, since this factor elucidates critical historical events, and also because shock metamorphism can alter primary mineralogical and petrographic features, and reset chronologies [1]. Failure to take shock history into proper account during characterization can result in seriously incorrect conclusions being drawn. Thus the Hayabusa Preliminary Examination Team (HASPET) made shock stage determination of the Itokawa samples a primary goal [2]. However, we faced several difficulties in this particular research. The shock state of ordinary chondrite materials is generally determined by simple optical petrographic observation of standard thin sections. The Itokawa samples available to the analysis team were mounted into plastic blocks, were polished on only one side, and were of non-standard and greatly varying thickness, all of which significantly complicated petrographic analysis but did not prevent it. We made an additional estimation of the sample shock state by a new technique for this analysis - electron back-scattered diffraction (EBSD) in addition to standard petrographic techniques. We are also investigating the crystallinity of Itokawa olivine by Synchrotron X-ray diffraction (SXRD).
Zolensky, Michael↗
Pu'u Poli'ahu, Mauna Kea: A Possible Analog for the Hematite Bearing Layer Located in Gale Crater, Mars.
Hyperspectral data detected by the Compact Reconnaissance Imaging Spectrometer for Mars (CRISM) on board Mars Reconnaissance Orbiter (MRO) indicated the presence of a hematite bearing ridge on Mount Sharp situated in the Gale Crater, Mars. [Fraeman]. The presence of this mineral in high concentrations is indicative of possible aqueous origins. [Fraeman] In 2012, Curiosity Rover landed in Gale Crater on Mars. Curiosity's mission is to determine Mars' habitability and is equipped with an advanced suite of scientific instruments that are capable of conducting analyses on rocks and soil. The hematite bearing ridge on Mount Sharp is thought to be a good candidate of study for Curiosity. To better understand this type of terrain, the study of analog sites similar in geologic setting is of great importance. One site thought to be a comparable analog is a cinder cone called Pu'u Poli'ahu located on the summit of Mauna Kea, Hawaiʻi. Poli'ahu is unique among the tephra cones of Mauna Kea because it is thought to have formed in subaqueous conditions approximately 170,000 to 175,000 years ago. [Porter] Consequently located on the inner flanks of Poli'ahu is a rock outcrop that contains hematite. Samples were collected from the outcrop and characterized using the following instruments: Digital Microscope, Panalytical X‐ray diffraction (XRD), and scanning electron microscope (SEM). The initial preparation of the rocks involved documenting each sample by creating powdered samples, thick sections, and photo documentation.
Adams, M. E.↗
A Combined Study Investigating the Insoluble and Soluble Organic Compounds in Category 3 Carbonaceous Itokawa Particles Recovered by the Hayabusa Mission
At the 3rd International Announcement of Opportunity (AO), we have been approved for five Category 3 carbonaceous Itokawa particles (RA-QD02-0012, RA-QD02-0078, RB-CV-0029, RB-CV-0080 and RB-QD04-0052) recovered by the first Hayabusa mission of JAXA. In this investigation, we aim to provide a comprehensive study to characterize and account for the presence of carbon-bearing phases as suggested by the initial Scanning Electron Microscopy (SEM) analysis carried out by JAXA at the curation facility, and to describe the mineralogical components of the particles. The insoluble organic content of Itokawa particle has been investigated with the use of micro-Raman spectroscopy by Kitajima and co-workers [1]. The Raman spectra of Itokawa particles show broad G- and D-bands typical of low temperature material which offers an interesting contrast to the high metamorphic grade (LL4-6) of the Itokawa parent body. Amino acid analysis has been conducted by Naraoka et al. [2] to study the soluble organic component of Itokawa particles, but since it was a preliminary study and thus did not have the opportunity to target on Category 3 carbonaceous particles, only terrestrial contaminants were identified. The investigation will be carried out in the following order prioritized according to the progressive damage the analytical techniques can induce: (1) micro-Raman spectrometry, (2) two-step laser mass spectrometry (micro-L2MS), (3) ultra-high performance liquid chromatography with fluorescence detection and time-of-flight mass spectrometry (LC-FD/ToF-MS), and optimally if we can recover the particles after wet chemistry analysis, we will mount the samples and perform (4) electron beam microscopy (SEM, electron back-scattered diffraction [EBSD]) and (5) carbon X-ray absorption near edge structure spectroscopy (C-XANES). We will begin the analytical procedures upon receiving the samples in September/October. This work will provide us with an understanding of the variety and origins of the carbon-bearing phases present in primitive solar system bodies from a direct sample-returned mission, which is less likely hampered by risks of terrestrial contamination as compared to meteorite finds and falls.
Chan, Q. H. S.↗
CMAS Interactions with Advanced Environmental Barrier Coatings Deposited via Plasma Spray- Physical Vapor Deposition
Materials for advanced turbine engines are expected to have temperature capabilities in the range of 1370-1500C. At these temperatures the ingestion of sand and dust particulate can result in the formation of corrosive glass deposits referred to as CMAS. The presence of this glass can both thermomechanically and thermochemically significantly degrade protective coatings on metallic and ceramic components. Plasma Spray- Physical Vapor Deposition (PS-PVD) was used to deposit advanced environmental barrier coating (EBC) systems for investigation on their interaction with CMAS compositions. Coatings were exposed to CMAS and furnace tested in air from 1 to 50 hours at temperatures ranging from 1200-1500C. Coating composition and crystal structure were tracked with X-ray diffraction and microstructure with electron microscopy.
Coatings↗