Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “electron probe microanalysis”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 109 records · Page 6

Calculated X-ray Intensities Using Monte Carlo Algorithms: A Comparison to Experimental EPMA Data

Monte Carlo (MC) modeling has been used extensively to simulate electron scattering and x-ray emission from complex geometries. Here are presented comparisons between MC results and experimental electron-probe microanalysis (EPMA) measurements as well as phi(rhoz) correction algorithms. Experimental EPMA measurements made on NIST SRM 481 (AgAu) and 482 (CuAu) alloys, at a range of accelerating potential and instrument take-off angles, represent a formal microanalysis data set that has been widely used to develop phi(rhoz) correction algorithms. X-ray intensity data produced by MC simulations represents an independent test of both experimental and phi(rhoz) correction algorithms. The alpha-factor method has previously been used to evaluate systematic errors in the analysis of semiconductor and silicate minerals, and is used here to compare the accuracy of experimental and MC-calculated x-ray data. X-ray intensities calculated by MC are used to generate a-factors using the certificated compositions in the CuAu binary relative to pure Cu and Au standards. MC simulations are obtained using the NIST, WinCasino, and WinXray algorithms; derived x-ray intensities have a built-in atomic number correction, and are further corrected for absorption and characteristic fluorescence using the PAP phi(rhoz) correction algorithm. The Penelope code additionally simulates both characteristic and continuum x-ray fluorescence and thus requires no further correction for use in calculating alpha-factors.

Carpenter, P. K.↗

Preparation and Characterization of the Skutterudite-Related Phase Ru0.5Pd0.5 Sb3

A new skutterudite phase Ru0.5Pd0.5 Sb3 was prepared. It adds to the many materials with the skutterudite structure that have shown a good potential for thermoelectric applications. Single- phase polycrystalline samples were prepared and characterized by x-ray analysis, electron probe microanalysis, density, sound velocity, thermal expansion coefficient, and differential thermal analysis measurements.

ternary↗

Al, Ti, and Cr: Complex Zoning in Synthetic and Natural Nakhlite Pyroxenes

Nakhlites are olivine-bearing clinopyroxene cumulates. The cumulus pyroxenes have cores that are relatively homogeneous in Fe, Mg, and Ca, but show complex zoning of minor elements, especially Al, Ti, and Cr. Zoning patterns contain information about crystallization history parent magma compositions. But it has proven difficult to decipher this information and translate the zoning patterns into petrogenetic processes. This abstract reports results of high-precision Electron Probe MicroAnalysis (EPMA) analysis of synthetic nakhlite pyroxenes run at fO2 from IW to QFM. It compares these with concurrent analyses of natural nakhlite MIL03346 (MIL), and with standardprecision analyses of Y000593 (Y593) collected earlier. Results suggest that (1) different processes are responsible for the zoning of MIL and other more slowly-cooled nakhlites such as Y593, and (2) changes in oxidation conditions during MIL crystallization are not responsible for the unusual Cr zoning pattern

McKay, G.↗

Quantitative EPMA Compositional Mapping of NWA 2995: Characterization, and Petrologic Interpretation of Mafic Clasts

We present the first fully quantitative compositional maps of lunar meteorite NWA 2995 using electron microprobe stage mapping, and compare selected clast mineralogy and chemistry. NWA 2995 is a feldspathic fragmental breccia containing numerous highland fine grained lithologies, including anorthosite, norite, olivine basalt, subophitic basalt, gabbro, KREEP-like basalt, granulitic and glassy impact melts, coarse-grained mineral fragments, Fe-Ni metal, and glassy matrix [1]. Chips of NWA 2995, representing these diverse materials, were analyzed by INAA and fused-bead electron-probe microanalysis (EPMA); comparison of analytical data suggests grouping of lunar meteorites NWA 2995, 2996, 3190, 4503, 5151, and 5152. The mean composition of NWA 2995 corresponds to a 2:1 mixture of feldspathic and mare material, with approximately 5% KREEP component [2]. Clast mineral chemistry and petrologic interpretation of paired stone NWA 2996 has been reported by Mercer et al. [3], and Gross et al. [4]. This study combines advances in quantitative EPMA compositional mapping and data analysis, as applied to selected mafic clasts in a polished section of NWA 2995, to investigate the origin of mafic lithic components and to demonstrate a procedural framework for petrologic analysis.

Carpenter, P. K.↗

Examining the Possibility of Carbon as a Light Element in the Core of Mercury

Results from the MErcury Surface, Space ENvironment, GEochemistry and Ranging (MESSENGER) spacecraft have shown elevated abundances of C on the surface of Mercury. Peplowski et al. used GRS data from MESSENGER to show an average northern hemisphere abundance of C on the planet of 0 to 4.1 wt% C at the three-sigma detection limit. Confirmation of C on the planet prompts many questions regarding the role of C during the differentiation and evolution of Mercury. The elevated abundances of both S and C on Mercury's surface, coupled with the low abundances of iron, suggest that the oxygen fugacity of the planet is several log10 units below the Iron-Wustite buffer. These observations spark questions about the bulk composition of Mercury's core. This experimental study seeks to understand the impact of C as a light element on potential mercurian core compositions. In order to address this question, experiments were conducted at 1 GPa and a variety of temperatures (700 - 1500 C) on metal compositions ranging from Si5Fe95 to Si22Fe78, possibly representative of the mercurian core. All starting metals were completely enclosed in a graphite capsule to ensure C saturation at a given set of run conditions. All elements, including C, were analyzed using electron probe microanalysis. Precautions were taken to ensure accurate measurements of C with this technique including using the LDE2 crystal, the cold finger on the microprobe to minimize contamination and increase the vacuum, and an instrument with no oil based pumps. Based on the superliquidus experimental results in the present study, as Fe-rich cores become more Si-rich, the C content of that core composition will decrease. Furthermore, although C concentration at graphite saturation (CCGS) varies from a liquid to a solid, temperature does not seem to play a substantial role in CCGS, at least at 1 GPa.

Vander Kaaden, Kathleen↗

Experimental Constraints on the Partitioning Behavior of F, Cl, and OH Between Apatite and Basaltic Melt

The mineral apatite is present in a wide range of planetary materials. The presence of volatiles (F, Cl, and OH) within its crystal structure (X-site) have motivated numerous studies to investigate the partitioning behavior of F, Cl, and OH between apatite and silicate melt with the end goal of using apatite to constrain the volatile contents of planetary magmas and mantle sources. A number of recent experimental studies have investigated the apatite-melt partitioning behavior of F, Cl, and OH in magmatic systems. Apatite-melt partitioning of volatiles are best described as exchange equilibria similar to Fe-Mg partitioning between olivine and silicate melt. However, the partitioning behavior is likely to change as a function of temperature, pressure, oxygen fugacity, apatite composition, and melt composition. In the present study, we have conducted experiments to assess the partitioning behavior of F, Cl, and OH between apatite and silicate melt over a pressure range of 0-6 gigapascals, a temperature range of 950-1500 degrees Centigrade, and a wide range of apatite ternary compositions. All of the experiments were conducted between iron-wustite oxidation potentials IW minus 1 and IW plus 2 in a basaltic melt composition. The experimental run products were analyzed by a combination of electron probe microanalysis and secondary ion mass spectrometry (NanoSIMS). Temperature, apatite crystal chemistry, and pressure all play important roles in the partitioning behavior of F, Cl, and OH between apatite and silicate melt. In portions of apatite ternary space that undergo ideal mixing of F, Cl, and OH, exchange coefficients remain constant at constant temperature and pressure. However, exchange coefficients vary at constant temperature (T) and pressure (P) in portions of apatite compositional space where F, Cl, and OH do not mix ideally in apatite. The variation in exchange coefficients exhibited by apatite that does not undergo ideal mixing far exceeds the variations induced by changes in temperature (T) or pressure (P) . In regions where apatite undergoes ideal mixing of F, Cl, and OH, temperature has a stronger effect than pressure on the partitioning behavior, but both are important. Furthermore, fluorine becomes less compatible in apatite with increasing pressure and temperature. We are still in the process of analyzing our experimental run products, but we plan to quantify the effects of P and T on apatite-melt partitioning of F, Cl, and OH.

McCubbin, Francis M.↗

Discreditation of Bobdownsite and the Establishment of Criteria for the Identification of Minerals with Essential Monofluorophosphate (PO3F2-)

Bobdownsite, IMA number 2008-037, was approved as a new mineral by the Commission on New Minerals, Nomenclature and Classification (CNMNC) as the fluorine endmember of the mineral whitlockite. The type locality of bobdownsite is in Big Fish River, Yukon Canada, and bobdownsite was reported to be the first naturally occurring mineral with essential monofluorophosphate (PO3F2-). The type specimen of bobdownsite has been reinvestigated by electron probe microanalysis (EPMA), and our data indicate that fluorine abundances are below detection in the mineral. In addition, we conducted detailed analysis of bobdownsite from the type locality by gas chromatography isotope ratio mass spectrometry, Raman spectroscopy, EPMA, and NMR spectroscopy. These data were compared with previously published data on synthetic monofluorophosphate salts. Collectively, these data indicate that bobdownsite is indistinguishable from whitlockite with a composition along the whitlockite-merrillite solid solution. Bobdownsite is therefore discredited as a valid mineral species. An additional mineral, krásnoite, has been purported to have monofluorophosphate components in its structure, but reexamination of those data indicate that F- in krásnoite forms bonds with Al, similar to OH- bonded to Al in perhamite. Consequently, krásnoite also lacks monofluorophosphate groups, and there are currently no valid mineral species with monofluorophosphate in their structure. We recommend that any future reports of new minerals that contain essential monofluorophosphate anions be vetted by abundance measurements of fluorine, vibrational spectroscopy (both Raman and FTIR), and where paramagnetic components are permissibly low, NMR spectroscopy. Furthermore, we emphasize the importance of using synthetic compounds containing monofluorophosphate anions as a point of comparison in the identification of minerals with essential monofluorophosphate. Structural data that yield satisfactory P-F bond lengths determined by X-ray crystallography, coupled with direct chemical analyses of fluorine in a material do not constitute sufficient evidence alone to identify a new mineral with essential monofluorophosphate anions.

McCubbin, Francis M.↗

Future Planetary Instrument Capabilities Made Possible by Micro- and Nanotechnology

A number of new instrument capabilities are currently in maturation for future in situ use on planetary science missions. Moving beyond the impressive in situ instrumentation already operating in planetary environments beyond Earth will enable the next step in scientific discovery. The approach for developing beyond current instrumentation requires a careful assessment of science-driven capability advancement. To this end, two examples of instrument technology development efforts that are leading to new and important analytical capabilities for in situ planetary science will be discussed: (1) an instrument prototype enabling the interface between liquid separation techniques and laser desorption/ionization mass spectrometry and (2) an addressable excitation source enabling miniaturized electron probe microanalysis for elemental mapping of light and heavy elements.

Getty, Stephanie A.↗

Petrology, Geochemistry, and Pairing of Lunar Meteorites from the Dominion Range

Introduction: During the 2018-2019 Antarctic Search for Meteorites (ANSMET) field season in the Dominion Range (DOM), 7 lunar meteorite stones were collected: DOM 18242 (15.1 g), DOM 18244 (25.1 g), DOM 18262 (6.8 g), DOM 18509 (16.5 g), DOM 18543 (13.6 g), DOM 18666 (45.9 g), and DOM 18678 (11.6 g). Here we present the initial results of electron microprobe and X-ray computed tomography (XCT) studies of these stones and look at the details of their petrography and mineral chemistry, as well as investigate possible pairing relationships, both with each other and with previously described lunar meteorites. Most of the work presented here is on the DOM 18509, 18543, and 18678 stones; subsamples of the other stones are in hand and similar measurements will be made on them by the time of the meeting. Methods: Textures in DOM 18509, DOM 18543, and DOM 18678 were characterized in 2D by optical microscopy, backscattered electron (BSE) imaging and elemental X-ray images on thin sections, as well as in 3D by X-ray computed tomography (XCT) on sample chips. Mineral compositions were assessed through a combination of wavelength dispersive spectroscopy EPMA (electron probe microanalysis) and x-ray mapping on the JEOL 8530 at NASA JSC. The bulk composition of all three meteorites was determined based on analyses of the fusion crust glass. XCT analyses were done on the Nikon XTH 320 at NASA JSC. ICP-MS data on bulk rock subsamples for each meteorite will be carried out in the near future. Results: The stones are all similar in macroscopic appearance with a dark aphanitic matrix hosting a variety of small- to medium-sized angular mineral and lithic fragments (often light colored in nature) [1,2]. Based on EPMA and XCT results, the three meteorites are polymict regolith breccias comprised of mineral, glass, and lithic clasts ranging up to several mm in length. Melt veins run through all three meteorite samples. Mineral clasts in all 3 stones are dominated by pyroxene and plagioclase (An82-96), with minor amounts of SiO2, olivine (Fo1-52), and FeTi-oxides. Pyroxene grains are mostly Fe-rich pigeonite and augite, and larger clasts are normally zoned and have fine exsolution lamellae. The lithic clasts in all stones consists of: (1) basalt clasts that contain zoned pyroxene, plagioclase laths, and ilmenite, with minor silica and Fe-rich olivine; (2) granulitic clasts; (3) anorthosite clasts; (4) Si-rich clasts that also contain ilmenite, troilite, high-Ca pyroxene, fayalite, and K-feldspar likely mesostasis from late stage basalts). All three meteorites contain glassy fusion crust that is highly vesicular, high in FeO and Al2O3 (15-17 wt% each), ferroan (Mg# of 23-24), and moderately rich in TiO2 (1.4-1.8 wt%). The composition of the fusion crust can serve as a proxy for the bulk meteorite composition and is identical within error for all three meteorites. Implications: The lithic and mineral clasts in all three stones are similar in clast population and assemblages as well as mineral chemistry. In addition, the fusion crust composition, a proxy for bulk composition, is within error of each other for all three stones. Thus DOM 18509, DOM 18543, and DOM 18678 are almost certainly paired. Based on similarities in macroscopic description as well as preliminary classification data [1,2], all 7 lunar stones from DOM are likely paired, though additional quantitative analyses are needed to confirm this. The presence of spherules and vesicular fusion crusts indicates that the DOM pairing group is a regolith breccia. The presence of basaltic and gabbroic clasts as well as more feldspathic materials, suggest that the regolith from which these meteorites formed contained a mixture of feldspathic highland material and mare material, suggesting a possible provenance near a marehighlands boundary. No evidence of KREEPy lithologies have been observed so far in these meteorites, however, future ICP-MS data on bulk rock chips for the stones will reveal any KREEP component if present. The DOM pairing group has many similarities to previously described lunar breccia meteorite MET 01210, however more detailed compositional data will be needed to make a definitive comparison.

R.A. Zeigler↗

Petrography and Mineralogy of Basalt Fragments in Apollo 17 Double Drive Tube 73002 and 73001

The ANGSA program was formed, in part, to examine previously unstudied Apollo 17 double drive tube samples. As a part of this project, the Moon United team received eight basalt fragments from 73001 and 73002. Here we present the petrography and mineralogy of these basalt fragments. Methods: We analyzed the petrography and mineralogy of the 73001/73002 particles using Electron Probe Microanalysis (EMPA) at both Carnegie Institution for Science and the Smithsonian Institution. We made quantitative compositional maps for each sample following the methods of [1,2].

S. N. Valencia↗

Mineralogical and chemical characterization of iron-, manganese-, and copper-containing synthetic hydroxyapatites

The National Aeronautics and Space Administration's (NASA) Advanced Life Support (ALS) Program is evaluating the use of Fe-, Mn-, and Cu-containing synthetic hydroxyapatite (SHA) as a slow release fertilizer for crops that might be grown on the International Space Station or at Lunar and Martian outposts. Separate Fe-, Mn-, and Cu-containing SHA materials along with a transition-metal free SHA (pure-SHA) were synthesized using a precipitation method. Chemical and mineralogical analyses determined if and how Fe, Mn, and Cu were incorporated into the SHA structure. X-ray diffraction (XRD), Rietveld refinement, and transmission electron microscopy (TEM) confirmed that SHA materials with the apatite structure were produced. Chemical analyses indicated that the metal containing SHA materials were deficient in Ca relative to pure-SHA. The shift in the infrared PO4-mu 3 vibrations, smaller unit cell parameters, smaller particle size, and greater structural strain for Fe-, Mn-, and Cu-containing SHA compared with pure-SHA suggested that Fe, Mn, and Cu were incorporated into SHA structure. Rietveld analyses revealed that Fe, Mn, and Cu substituted into the Ca2 site of SHA. An Fe-rich phase was detected by TEM analyses and backscattered electron microscopy in the Fe-containing SHA material with the greatest Fe content. The substitution of metals into SHA suggests that metal-SHA materials are potential slow-release sources of micronutrients for plant uptake in addition to Ca and P.

NASA Center JSC↗

Invited Review Paper in Commemoration of Over 50 Years of Oxidation of Metals: Addressing the Role of Water Vapor on Long-Term Stainless Steel Oxidation Behavior

In the past 20 years, it has become clear that the long-term exposure of chromia-forming austenitic stainless steels to air containing ~ 10 vol% water vapor at 650–800 °C significantly increases the Cr consumption rate compared to laboratory air. However, a similar acceleration does not occur in 100% steam because O 2 is not available to form volatile CrO 2 (OH) 2 . As the research has shown, this accelerated Cr loss is particularly important for thin-walled components like gas turbine recuperators. Typically, conventional austenitic stainless steels exhibit accelerated attack (i.e., rapid formation of Fe-rich oxide nodules), while higher alloyed steels resist this type of degradation until the alloy surface becomes Cr depleted. The development of strategies and solutions for this issue are reviewed. Model Fe–Cr–Ni alloys have been used to study composition effects on this behavior. For example, increasing the Mn content up to ~ 4 wt% was not beneficial, but increasing the Ni content improved oxidation resistance in this environment. However, at 650–700 °C even highly alloyed steels showed surface Cr depletion at alloy grain boundaries resulting in Fe-rich oxide nodule formation. The path forward for this issue will require more refined mechanistic understanding and increased used of modeling to develop better application-specific lifetime models to identify the most cost-effective alloy solutions.

36 MATERIALS SCIENCE↗

Single-component-at-a-time variation study for glass-ceramic waste forms

Here, a 51-sample composition variation study was performed on glass-ceramic waste forms for a raffinate waste stream from aqueous reprocessing of used nuclear fuel containing high fractions of Mo, alkalis, alkaline earths (AEs), and rare earths (REs). The study was designed with a single-component-at-a-time variation approach off a centroid composition. The components that were varied included Al, B, Ca, Li, Mo, Na, REs, Si, Zr, and Others (containing minor components). Data analysis included crystallization curves, microstructure, and phase compositions. A number of components (i.e., Li 2 O, B 2 O 3 , REO x , MoO 3 , Na 2 O, and ZrO 2 ) significantly impacted the concentration and chemistry of phases, especially the primary phases of oxyapatite [i.e., Ca 2 RE 8 (SiO 4 ) 6 O 2 ] and powellite (i.e., AEMoO 4 ), precipitated in the slow-cool heat-treated waste forms; minor phases included cerianite [i.e., Ce x Zr (1-x) O 2 ], Ba-molybdate [i.e., Ba(Gd 0.67 Mo 0.33 O 3 ], noble metals, pollucite (i.e., CsAlSiO 4 ), and RE-borosilicate (i.e., RE 3 BSi 2 O 10 ).

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

EPMA-Based Mass Balance Method for Quantitative Fission Product Distribution Comparison between TRISO Particles

Two irradiated AGR-2 TRISO particles were chosen to demonstrate a recently developed mass balance technique in which EPMA-generated concentration data was used to determine fission product mass on a layer-by-layer basis in TRISO particles. EPMA-calculated fission product masses for most fission products in the two particles were within +/- 20% of their ORIGEN-modelled masses. Results show that Sr, Ba, and Eu accumulate preferentially in the carbon-rich kernel periphery on the particles’ side that lacks a gap between the buffer and IPyC. In addition, the more mobile elements--Cs, Sr, and Pd, accumulate in greater quantity in the outer layers of particle AGR2-223-RS34 compared to particle AGR2-223-RS06, which has relatively more of those elements’ mass located in the kernel and kernel periphery, suggesting enhanced fission product transport in particle AGR2-223-RS34. This model can be used better understand and test fission product transport in TRISO particles.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Calcium localization and tipburn development in lettuce leaves during early enlargement

Tissue concentrations of Ca, Mg, and K were determined across immature leaves of lettuce (Lactuca sativa L. 'Buttercrunch') at different stages of enlargement using electron microprobe x-ray analysis. The analysis was with a wavelength dispersive spectrometer to permit detection of low concentrations of Ca. Patterns of mineral accumulation in immature leaves that were exposed were compared to patterns of accumulation in leaves that were enclosed within a developing head. The leaves developing without enclosure were free to transpire and developed normally whereas leaves developing with enclosure were restricted in transpiration and developed an injury that was characteristic of Ca deficiency. In the exposed leaves, Ca concentrations increased from an average of 1.0 to 2.1 mg g-1 dry weight (DW) as the leaves enlarged from 5 to 30 mm in length. In the enclosed leaves, Ca concentrations decreased from 1.0 to 0.7 mg g-1 DW as the leaves enlarged from 5 to 30 mm in length. At the tips of these enclosed leaves a larger decrease was found, from 0.9 to 0.3 mg g-1 DW during enlargement. Necrotic injury first became apparent in this tip area when the concentration was approximate to 0.4 mg g-1 DW. Magnesium concentrations across the exposed leaves were similar to concentrations across the enclosed leaves, and did not change with enlargement. Magnesium concentrations averaged 3.5. mg g-1 DW in both enclosed and exposed leaves during enlargement from 5 to 30 mm. In both exposed and enclosed leaves, K concentrations increased during enlargement from 40 to approximate to 60 mg g-1 DW. Potassium concentrations were highest toward the leaf apex and upper margin where injury symptoms occurred, and this may have enhanced injury development. This research documents the critical low levels of Ca (0.2 to 0.4 mg g-1 DW) that can occur in enclosed leaves of plants and which apparently leads to the marginal apex necrosis of developing leaves seen frequently on lettuce and other crops.

NASA Discipline Life Support Systems↗

Martian soil component in impact glasses in a Martian meteorite

Chemical compositions of impact melt glass veins, called Lithology C (Lith C) in Martian meteorite EET79001 were determined by electron microprobe analysis. A large enrichment of S, and significant enrichments of Al, Ca, and Na were observed in Lith C glass compared to Lithology A (Lith A). The S enrichment is due to mixing of plagioclase- enriched Lith A material with Martian soil, either prior to or during impact on Mars. A mixture of 87% Lith A, 7% plagioclase, and 6% Martian soil reproduces the average elemental abundances observed in Lith C. Shock melting of such a mixture of plagioclase-enriched, fine-grained Lith A host rock and Martian soil could yield large excesses of S (observed in this study) and Martian atmospheric noble gases (found by Bogard et al., 1983) in Lith C. These mixing proportions can be used to constrain the elemental abundance of phosphorus in Martian soil.

NASA Center JSC↗