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All sourcesNASA NTRSDOE OSTI
NASA NTRS2013

Packaging Technologies for High Temperature Electronics and Sensors

This paper reviews ceramic substrates and thick-film metallization based packaging technologies in development for 500degC silicon carbide (SiC) electronics and sensors. Prototype high temperature ceramic chip-level packages and printed circuit boards (PCBs) based on ceramic substrates of aluminum oxide (Al2O3) and aluminum nitride (AlN) have been designed and fabricated. These ceramic substrate-based chiplevel packages with gold (Au) thick-film metallization have been electrically characterized at temperatures up to 550degC. A 96% alumina based edge connector for a PCB level subsystem interconnection has also been demonstrated recently. The 96% alumina packaging system composed of chip-level packages and PCBs has been tested with high temperature SiC devices at 500degC for over 10,000 hours. In addition to tests in a laboratory environment, a SiC JFET with a packaging system composed of a 96% alumina chip-level package and an alumina printed circuit board mounted on a data acquisition circuit board was launched as a part of the MISSE-7 suite to the International Space Station via a Shuttle mission. This packaged SiC transistor was successfully tested in orbit for eighteen months. A spark-plug type sensor package designed for high temperature SiC capacitive pressure sensors was developed. This sensor package combines the high temperature interconnection system with a commercial high temperature high pressure stainless steel seal gland (electrical feed-through). Test results of a packaged high temperature capacitive pressure sensor at 500degC are also discussed. In addition to the pressure sensor package, efforts for packaging high temperature SiC diode-based gas chemical sensors are in process.

Electronic packaging↗
NASA NTRS2012

Overheating Anomalies during Flight Test Due to the Base Bleeding

In this paper we present the results of the analytical and numerical studies of the plume interaction with the base flow in the presence of base out-gassing. The physics-based analysis and CFD modeling of the base heating for single solid rocket motor performed in this research addressed the following questions: what are the key factors making base flow so different from that in the Shuttle [1]; why CFD analysis of this problem reveals small plume recirculation; what major factors influence base temperature; and why overheating was initiated at a given time in the flight. To answer these questions topological analysis of the base flow was performed and Korst theory was used to estimate relative contributions of radiation, plume recirculation, and chemically reactive out-gassing to the base heating. It was shown that base bleeding and small base volume are the key factors contributing to the overheating, while plume recirculation is effectively suppressed by asymmetric configuration of the flow formed earlier in the flight. These findings are further verified using CFD simulations that include multi-species gas environment both in the plume and in the base. Solid particles in the exhaust plume (Al2O3) and char particles in the base bleeding were also included into the simulations and their relative contributions into the base temperature rise were estimated. The results of simulations are in good agreement with the temperature and pressure in the base measured during the test.

base bleeding↗
NASA NTRS2014

Connecting Lunar Meteorites to Source Terrains on the Moon

The number of named stones found on Earth that have proven to be meteorites from the Moon is approx. 180 so far. Since the Moon has been mapped globally in composition and mineralogy from orbit, it has become possible to speculate broadly on the region of origin on the basis of distinctive compositional characteristics of some of the lunar meteorites. In particular, Lunar Prospector in 1998 [1,2] mapped Fe and Th at 0.5 degree/pixel and major elements at 5 degree/pixel using gamma ray spectroscopy. Also, various multispectral datasets have been used to derive FeO and TiO2 concentrations at 100 m/pixel spatial resolution or better using UV-VIS spectral features [e.g., 3]. Using these data, several lunar meteorite bulk compositions can be related to regions of the Moon that share their distinctive compositional characteristics. We then use EPMA to characterize the petrographic characteristics, including lithic clast components of the meteorites, which typically are breccias. In this way, we can extend knowledge of the Moon's crust to regions beyond the Apollo and Luna sample-return sites, including sites on the lunar farside. Feldspathic Regolith Breccias. One of the most distinctive general characteristics of many lunar meteorites is that they have highly feldspathic compositions (Al2O3 approx. 28% wt.%, FeO <5 wt.%, Th <1 ppm). These compositions are significant because they are similar to a vast region of the Moon's farside highlands, the Feldspathic Highlands Terrane, which are characterized by low Fe and Th in remotely sensed data [4]. The meteorites provide a perspective on the lithologic makeup of this part of the Moon, specifically, how anorthositic is the surface and what, if any, are the mafic lithic components? These meteorites are mostly regolith breccias dominated by anorthositic lithic clasts and feldspathic glasses, but they do also contain a variety of more mafic clasts. On the basis of textures, we infer these clasts to have formed by large impacts that excavated and mixed rocks from depth within the lunar crust and possibly the upper mantle. One of the key questions is whether the mafic materials are ferroan or magnesian, which remote sensing does not clearly distinguish, and if mafic, whether they might contain mantlederived components such as olivine (dunite). Many but not all have mainly ferroan mafic components, consistent with a ferroan crustal source that is complementary to the ferroan anorthositic suite and that represents primary magma-ocean-derived feldspathic crust. Meteorites such as ALH 81005 [5] and Shişr 161 [6], however, contain coarse-grained magnesian mafic clasts (Fig. 1a) derived from deeply seated and melted material associated with impact basins. Comparison to LP gamma-ray data [2] supports an origin for magnesian feldspathic meteorites such as these (e.g., Shişr 161) as shown in Fig. 1b. Sayh al Uhaymir (SaU) 169. Another distinctive but much less common composition is represented by relatively mafic impact-melt breccia that is rich in incompatible elements known as KREEP. These meteorites can be related to the western nearside Procellarum KREEP Terrane, especially through a combination of Fe and Th contents. Among the most enriched is SaU 169, which has been related to high- Th impact-melt breccia found at the Apollo 12 site [7]. Through detailed EPMA and ion microprobe analysis we have shown that these two rock types are related in age and origin.

Jolliff, B. L.↗
NASA NTRS2012

Addressing Machining Issues for the Intermetallic Compound 60-NITINOL

60-NITINOL (60 wt.% Ni - 40 wt.% Ti) is being studied as a material for advanced aerospace components. Frequent wire breakage during electrical-discharge machining of this material was investigated. The studied material was fabricated from hot isostatically pressed 60-NITINOL powder obtained through a commercial source. Bulk chemical analysis of the material showed that the composition was nominal but had relatively high levels of certain impurities, including Al and O. It was later determined that Al2O3 particles had contaminated the material during the hot isostatic pressing procedure and that these particles were the most likely cause of the wire breakage. The results of this investigation highlight the importance of material cleanliness to its further implementation.

Stanford, Malcolm K.↗
NASA NTRS2014

Dielectric Performance of a High Purity HTCC Alumina at High Temperatures - a Comparison Study with Other Polycrystalline Alumina

A very high purity (99.99+%) high temperature co-fired ceramic (HTCC) alumina has recently become commercially available. The raw material of this HTCC alumina is very different from conventional HTCC alumina, and more importantly there is no glass additive in this alumina material for co-firing processing. Previously, selected HTCC and LTCC (low temperature co-fired ceramic) alumina materials were evaluated at high temperatures as dielectric and compared to a regularly sintered 96% polycrystalline alumina (96% Al2O3), where 96% alumina was used as the benchmark. A prototype packaging system based on regular 96% alumina with Au thickfilm metallization successfully facilitated long term testing of high temperature silicon carbide (SiC) electronic devices for over 10,000 hours at 500 C. In order to evaluate this new high purity HTCC alumina for possible high temperature packaging applications, the dielectric properties of this HTCC alumina substrate were measured and compared with those of 96% alumina and a previously tested LTCC alumina from room temperature to 550 C at frequencies of 120 Hz, 1 KHz, 10 KHz, 100 KHz, and 1 MHz. A parallel-plate capacitive device with dielectric of the HTCC alumina and precious metal electrodes were used for measurements of the dielectric constant and dielectric loss of the co-fired alumina material in the temperature and frequency ranges. The capacitance and AC parallel conductance of the capacitive device were directly measured by an AC impedance meter, and the dielectric constant and parallel AC conductivity of the dielectric were calculated from the capacitance and conductance measurement results. The temperature and frequency dependent dielectric constant, AC conductivity, and dissipation factor of the HTCC alumina substrate are presented and compared to those of 96% alumina and a selected LTCC alumina. Other technical advantages of this new co-fired material for possible high packaging applications are also discussed.

Electronic packaging↗
NASA NTRS2013

Interstellar and Ejecta Dust in the Cas A Supernova Remnant

The ejecta of the Cas A supernova remnant has a complex morphology, consisting of dense fast-moving line emitting knots and diffuse X-ray emitting regions that have encountered the reverse shock, as well as more slowly expanding, unshocked regions of the ejecta. Using the Spitzer 5-35 micron IRS data cube, and Herschel 70, 100, and 160 micron PACS data, we decompose the infrared emission from the remnant into distinct spectral components associated with the different regions of the ejecta. Such decomposition allows the association of different dust species with ejecta layers that underwent distinct nuclear burning histories, and determination of the dust heating mechanisms. Our decomposition identified three characteristic dust spectra. The first, most luminous one, exhibits strong emission features at approx. 9 and 21 micron, and a weaker 12 micron feature, and is closely associated with the ejecta knots that have strong [Ar II] 6.99 micron and [Ar III] 8.99 micron emission lines. The dust features can be reproduced by magnesium silicate grains with relatively low MgO-to-SiO2 ratios. A second, very different dust spectrum that has no indication of any silicate features, is best fit by Al2O3 dust and is found in association with ejecta having strong [Ne II] 12.8 micron and [Ne III] 15.6 micron emission lines. A third characteristic dust spectrum shows features that best matched by magnesium silicates with relatively high MgO-to-SiO2 ratio. This dust is primarily associated with the X-ray emitting shocked ejecta and the shocked interstellar/circumstellar material. All three spectral components include an additional featureless cold dust component of unknown composition. Colder dust of indeterminate composition is associated with [Si II] 34.8 micron emission from the interior of the SNR, where the reverse shock has not yet swept up and heated the ejecta. The dust mass giving rise to the warm dust component is about approx. 0.1solar M. However, most of the dust mass is associated with the unidentified cold dust component. Its mass could be anywhere between 0.1 and 1 solar M, and is primarily limited by the mass of refractory elements in the ejecta. Given the large uncertainty in the dust mass, the question of whether supernovae can produce enough dust to account for ISM dust masses in the local and high-z universe remains largely unresolved.

Interstellar↗
NASA NTRS2014

Diffusivity in Alumina Scales Grown on Al-MAX Phases

Ti3AlC2, Ti2AlC, and Cr2AlC are oxidation resistant MAX phase compounds distinguished by the formation of protective Al2O3 scales with well controlled kinetics. A modified Wagner treatment was used to obtain interfacial grain boundary diffusivity, deltaD(sub gb,O,int.), from scale growth rates and corresponding grain size. It is based on the p(O2)(exp -1/6) dependency of the double charged oxygen vacancy and oxygen diffusivity, coupled with the effective diffusion constant for short circuit grain boundary paths. Data from the literature for MAX phases was analyzed accordingly, and deltaD(sub gb,O,int.) was found to nearly coincide with the Arrhenius line developed for Zr-doped FeCrAl, where: deltaD(sub gb,O,int.) = 1.8x10(exp -10) exp(-375 kJ/RT) cubic meters/s. Furthermore, this oxidation relation suggests the more general format applicable to bulk samples under ambient conditions: deltaD(sub gb,O) = 7.567x10(exp -8) exp(-544 kJ/RT) p(O2)(exp -1/6) cubic meters/[s x Pa(exp -1/6)]. Data from many other FeCrAl(X) studies were similarly assessed to show general agreement with the relation for deltaD(sub gb,O,int.). This analysis reinforces the view that protective alumina scales grow by similar mechanisms for these Al-MAX phases and oxidation resistant FeCrAl alloys.

aluminum oxide↗
NASA NTRS2012

Dielectric Performance of High Purity HTCC Alumina at High Temperatures - A Comparison Study with Other Polycrystalline Alumina

A very high purity (99.99+) high temperature co-fired ceramic (HTCC) alumina has recently become commercially available. The raw material of this HTCC alumina is very different from conventional HTCC alumina, and more importantly there is no glass additive in this co-fired material. Previously, selected HTCC and LTCC (low temperature co-fired ceramic) alumina materials were evaluated at high temperatures as dielectric and compared to a regularly sintered 96 polycrystalline alumina (96 Al2O3), where 96 alumina was used as the benchmark. A prototype packaging system based on regular 96 alumina with Au thick-film metallization successfully facilitated long term testing of high temperature silicon carbide (SiC) electronic devices for over 10,000 hours at 500C. In order to evaluate this new HTCC alumina for possible high temperature packaging applications, the dielectric properties of this HTCC alumina substrate were measured and compared with those of 96 alumina and a LTCC alumina from room temperature to 550C at frequencies of 120 Hz, 1 KHz, 10 KHz, 100 KHz, and 1 MHz. A parallel-plate capacitive device with dielectric of the HTCC alumina and precious metal electrodes were used for measurements of the dielectric constant and dielectric loss of the co-fired alumina material in the temperature and frequency ranges. The capacitance and AC parallel conductance of the capacitive device were directly measured by an AC impedance meter, and the dielectric constant and parallel AC conductivity of the dielectric were calculated from the capacitance and conductance measurement results. The temperature and frequency dependent dielectric constant, AC conductivity, and dissipation factor of the HTCC alumina substrate are presented and compared to those of 96 alumina. Other technical advantages of this new co-fired material for possible high packaging applications are also discussed.

High temperature↗
NASA NTRS2015

Gusev-Meridiani-Type Soil Component Dissolved in Some Shock Glasses in Shergottites

Modal analysis, based on APXS, MiniTES and Mossbauer results obtained at Gusev and Meridiani sites on Mars, indicates that Martian soils consist predominantly of igneous minerals such as olivine, pyroxene and feldspar (approximately70 - 80%), with the balance consisting of alteration minerals such as sulfates, silica and chlorides]. These studies also showed that soil alteration did not occur in-situ and igneous and alteration components are derived from different sources. Below, we analyse the chemical abundance data obtained from shock glasses in shergottites using mass balance mixing models. In these models, the two main end members used are (a) host rock chemical composition and (b) the GM soils average composition as the second component. Here, we consider the S-bearing phases as indicators of added alteration phases in the shock glasses and GM soils. Although the S-bearing phase in shock glasses occurs as micron sized sulfide blebs, we showed in earlier abstracts that sulfur was originally present as sulfate in impact glass-precursor materials and was subsequently reduced to sulfide during shock melting. This conclusion is based on results obtained from S-K XANES studies, Fe/S atomic ratios in sulfide blebs and 34S/32S isotopic measurements in these sulfide blebs. Additionally, sulfur in several EET79001 Lith. A glasses is found to correlate positively with Al2O3 and CaO (and negatively with FeO and MgO), suggesting the presence of Al- and Ca- sul-fate-bearing phases. The distribution of the 87Sr/86Sr iso-topic ratios determined in Lith. A glasses (,27 &,188 and,54) indicate that Martian soil gypsum and host rock material were mixed with each other in the glass precursors. In some vugs in Lith A glass,27 detected gypsum laths. Furthermore, the Martian regolith-de-rived component (where sulfur typically occurs as sul-fate) is identified in these glasses by determining neutron produced isotopic excesses/deficits in 80Kr and 149Sm isotopes. Moreover, the suggestion that the large amount of sulfur found in,507 was sourced from pyrrhotite in the host rock, would require that excessive quantities of host rock would need to be stripped of sulfur to make this sulfide-rich glass. These results provide ample evidence that S occurred as sulfate and was added to glass precursor materials prior to impact shock.

Ross, D. K.↗
NASA NTRS2013

The DUV Stability of Superlattice-Doped CMOS Detector Arrays

JPL and Alacron have recently developed a high performance, DUV camera with a superlattice doped CMOS imaging detector. Supperlattice doped detectors achieve nearly 100% internal quantum efficiency in the deep and far ultraviolet, and a single layer, Al2O3 antireflection coating enables 64% external quantum efficiency at 263nm. In lifetime tests performed at Applied Materials using 263 nm pulsed, solid state and 193 nm pulsed excimer laser, the quantum efficiency and dark current of the JPL/Alacron camera remained stable to better than 1% precision during long-term exposure to several billion laser pulses, with no measurable degradation, no blooming and no image memory at 1000 fps.

silicon detectors↗
NASA NTRS2015

SRAG Measurements Performed During the Orion EFT-1 Mission

The Exploration Flight Test 1 (EFT-1) was the first flight of the Orion Multi-Purpose Crew Vehicle (MPCV). The flight was launched on December 5, 2014, by a Delta IV Heavy rocket and lasted 4.5 hours. The EFT-1 trajectory involved one low altitude orbit and one high altitude orbit with an apogee of almost 6000 km. As a result of this particular flight profile, the Orion MPCV passed through intense regions of trapped protons and electron belts. In support of the radiation measurements aboard the EFT-1, the Space Radiation Analysis Group (SRAG) provided a Battery-operated Independent Radiation Detector (BIRD) based on Timepix radiation monitoring technology similar to that employed by the ISS Radiation Environmental Monitors (REM). In addition, SRAG provided a suite of optically and thermally stimulated luminescence detectors, with 2 Radiation Area Monitor (RAM) units collocated with the BIRD instrument for comparison purposes, and 6 RAM units distributed at different shielding configurations within the Orion MPCV. A summary of the EFT-1 Radiation Area Monitors (RAM) mission dose results obtained from measurements performed in the Space Radiation Dosimetry Laboratory at the NASA Johnson Space Center will be presented. Each RAM included LiF:Mg,Ti (TLD-100), (6)LiF:Mg,Ti (TLD-600), (7)LiF:Mg,Ti (TLD-700), Al2O3:C (Luxel trademark), and CaF2:Tm (TLD-300). The RAM mission dose values will be compared with the BIRD instrument total mission dose. In addition, a similar comparison will be shown for the ISS environment by comparing the ISS RAM data with data from the six Timepix-based REM units deployed on ISS as part of the NASA REM Technology Demonstration.

Gaza, Ramona↗
NASA NTRS2015

Investigating the Effects of Temperature on the Signatures of Shocks Propagated Through Impacts into Minerals Found in Comets and Asteroids

Comets and asteroids are subjected to extremely cold conditions throughout their lifetimes. During their sojourns in the solar system, they are subjected to collisions at speeds that are easily capable of generating shock waves in their constituent materials. In addition to ices, more common silicate minerals such as olivines and pyroxenes are important components of these objects. The collision-induced shocks could affect the spectral signatures of those mineral components, which could in turn be detected telescopically. We have embarked on a project to determine how impact-generated shock might affect the reflectance spectra and structures of select silicates as both impact speed and target temperature are varied systematically. While the effects of impact speed (in the form of shock stress) on numerous materials have been and continue to be studied, the role of target temperature has received comparatively little attention, presumably because of the operational difficulties it can introduce to experimentation. Our experiments were performed with the vertical gun in the Experimental Impact Laboratory of the Johnson Space Center. A liquid-nitrogen system was plumbed to permit cooling of the target container and its contents under vacuum to temperatures as low as -100 C (173 K). Temperatures were monitored by thermocouples mounted on the outside of the target container. Because those sensors were not in contact with the target material at impact, the measured temperatures are treated as lower limits for the actual values. Peridot (Mg-rich olivine) and enstatite (Mg-rich orthopyroxene) were used as targets, which involved the impact of alumina (Al2O3) spheres at speeds of 2.0 - 2.7 km s(exp -1) and temperatures covering 25 C to -100 C (298 K to 173 K). We have begun collecting and analyzing data in the near to mid-IR with a Fourier-transform infrared spectrometer, and preliminary analyses show that notable differences in absorption-band strength and position occur as functions of both impact speed (peak shock stress) and initial temperature.

Lederer, Susan M.↗
NASA NTRS2015

Packaging Technologies for 500 C SiC Electronics and Sensors: Challenges in Material Science and Technology

This paper presents ceramic substrates and thick-film metallization based packaging technologies in development for 500C silicon carbide (SiC) electronics and sensors. Prototype high temperature ceramic chip-level packages and printed circuit boards (PCBs) based on ceramic substrates of aluminum oxide (Al2O3) and aluminum nitride (AlN) have been designed and fabricated. These ceramic substrate-based chip-level packages with gold (Au) thick-film metallization have been electrically characterized at temperatures up to 550C. The 96 alumina packaging system composed of chip-level packages and PCBs has been successfully tested with high temperature SiC discrete transistor devices at 500C for over 10,000 hours. In addition to tests in a laboratory environment, a SiC junction field-effect-transistor (JFET) with a packaging system composed of a 96 alumina chip-level package and an alumina printed circuit board was tested on low earth orbit for eighteen months via a NASA International Space Station experiment. In addition to packaging systems for electronics, a spark-plug type sensor package based on this high temperature interconnection system for high temperature SiC capacitive pressure sensors was also developed and tested. In order to further significantly improve the performance of packaging system for higher packaging density, higher operation frequency, power rating, and even higher temperatures, some fundamental material challenges must be addressed. This presentation will discuss previous development and some of the challenges in material science (technology) to improve high temperature dielectrics for packaging applications.

dielectric properties↗
NASA NTRS2016

Feldspathic Meteorites MIL 090034 and 090070: Late Additions to the Lunar Crust

Our studies of the Miller Range lunar meteorites MIL 090034, 090036, and 090070 show them to be a diverse suite of rocks from the lunar highlands hereafter referred to as MIL 34, MIL 36, and MIL 70, resp. MIL34 and MIL70, the focus of this work, are crystalline melt breccias. Plagioclase compositions in both peak sharply around An96-97. Mg numbers of olivine vary from 58-65 with a few higher values. MIL36 is a regolith breccia. MIL 34 and MIL 70 have some of the highest Al2O3 abundances of lunar highland meteorites, indicating that they have among the largest modal abundances of plagioclase for lunar meteorites. They have lower Sc and Cr abundances than nearly all lunar highland meteorites except Dho 081, Dho 489 and Dho 733. MIL34 and MIL70 also have similar cosmic ray exposure (CRE) ages of approximately 1-2 Ma indicating they are launch paired. (MIL36 has a larger CRE age approximately greater than 70 Ma). Park et al. found a variation in Ar-Ar ages among subsamples of MIL 34 and MIL70, but preferred ages of 3500+/-110 Ma for the "Dark" phase of MIL 34 anorthite and 3520+/-30 Ma for the "Light" phase of MIL70. Bouvier et al. reported a Pb-Pb age of 3894+/-39 Ma for a feldspathic clast of MIL 34 and a similar age for a melt lithology. Here we reexamine the Rb-Sr and Sm-Nd isotopic data, which show complexities qualitatively consistent with those of the Ar-Ar and Pb-Pb data. The Sm-Nd data in particular suggest that the feldspathic compositions of MIL 34 and MIL 70 formed during initial lunar geochemical differentiation, and REE modeling suggests a relatively late-stage formation.

Nyquist, L. E.↗
NASA NTRS2016

High-Temperature, Perhaps Silicic, Volcanism on Mars Evidenced by Tridymite Detection in High-SiO2 Sedimentary Rock at Gale Crater, Mars

The Mars Science Laboratory (MSL) rover, Curiosity, has been exploring sedimentary rocks within Gale crater since landing in August, 2012. On the lower slopes of Aeolis Mons (a.k.a. Mount Sharp), drill powder was collected from a high-silica (74 wt% SiO2) outcrop named Buckskin (BK). It was a surprise to find that the Buckskin sample contained significant amounts of the relatively rare silica polymorph tridymite. We describe the setting of the Buckskin sample, the detection of tridymite by the MSL Chemistry and Mineralogy (CheMin) X-ray diffraction instrument, and detection implications. Geologic setting: The Buckskin outcrop is part of the Murray formation exposed in the Marias Pass area. The formation was previously studied by CheMin in the Pahrump Hills member [1] where three samples of drill fines were analyzed (Confidence Hills (CH), Mojave2 (MJ) and Telegraph Peak (TP) [2]). Assuming approximately horizontal bedding, the Buckskin outcrop is approx.15 m stratigraphically above the bottom of the Pahrump Hills member. Mudstone, generally characterized by fine lamination, is the dominant depositional facies [1]. Buckskin Mineralogical and Chemical Composition: The CheMin instrument and XRD pattern analysis procedures have been previously discussed [3-6]. The diffraction pattern used for quantitative XRD analysis (Fig. 1) is the sum of the first 4 of 45 diffraction images. The remaining images are all characterized by both on-ring and off-ring diffraction spots that we attributed to poor grain motion and particle clumping. Coincident with particle clumping was a significant decrease in the intensity of the tridymite diffraction peaks (Fig. 2a). The derived mineralogical composition of the crystalline component (derived from the first 4 diffraction images) is given in Table 1. The tridymite is well-crystalline and its pattern is refined as monoclinic tridymite (Fig 1). Mineral chemical compositions were derived from XRD unit cell parameters or obtained from stoichiometry. The XRD-calculated amorphous component was 50 +/- 15 wt%. We constrained the value to 60 wt% because it is the minimum value necessary to give a positive Al2O3 concentration for the amorphous component using APXS data for the post-sieve dump pile (Table 2). The amorphous component has high SiO2 (approx.77 wt%) and high anion (SO3+P2O5+Cl ~10 wt%) concentrations. Calculation shows that a cation-anion balance is achieved if the cations in the amorphous component except SiO2 and TiO2, which do not readily form salts, are assumed to be present as amorphous mixed-cation sulfates, phosphates, and chlorides (or perchlorates/ chlorates).

Morris, R. V.↗
NASA NTRS2016

Low Temperature Rhombohedral Single Crystal SiGe Epitaxy on c-plane Sapphire

Current best practice in epitaxial growth of rhombohedral SiGe onto (0001) sapphire (Al2O3) substrate surfaces requires extreme conditions to grow a single crystal SiGe film. Previous models described the sapphire surface reconstruction as the overriding factor in rhombohedral epitaxy, requiring a high temperature Al-terminated surface for high quality films. Temperatures in the 850-1100 C range were thought to be necessary to get SiGe to form coherent atomic matching between the (111) SiGe plane and the (0001) sapphire surface. Such fabrication conditions are difficult and uneconomical, hindering widespread application. This work proposes an alternative model that considers the bulk sapphire structure and determines how the SiGe film nucleates and grows. Accounting for thermal expansion effects, calculations using this new model show that both pure Ge and SiGe can form single crystal films in the 450-550 C temperature range. Experimental results confirm these predictions, where x-ray diffraction and atomic force microscopy show the films fabricated at low temperature rival the high temperature films in crystallographic and surface quality. Finally, an explanation is provided for why films of comparable high quality can be produced in either temperature range.

Duzik, Adam J.↗
NASA NTRS2016

Characterization of Candidate Materials for Remote Recession Measurements of Ablative Heat Shield Materials

A method of remotely measuring surface recession of a material sample in a plasma flow through emission spectroscopy of the post shock layer was characterized through experiments in the NASA Langley HYMETS arc jet facility. Different methods for delivering the seed products into the Phenolic Impregnated Carbon Ablator (PICA) material samples were investigated. Three samples were produced by seeding the PICA material with combinations of Al, Si, HfO2, VB2, Al2O3, SiO2, TiC, HfC, NaCl, and MgCl2 through infusing seed materials into a core of PICA, or through encapsulating seed material in an epoxy disk, mechanically bonding the disk to a PICA sample. The PICA samples seeded with the candidate tracers were then tested at surface temperatures near 2400 K under low pressure air plasma. The emission of Al, Ti, V, Na, and Mg in the post-shock layer was observed in the UV with a high resolution imaging spectrometer viewing the whole stagnation line from the side, and from UV to NIR with a fiber-coupled miniaturized spectrometer observing the sample surface in the wavelength range from 200 nm to 1,100 nm from the front through a collimator. Al, Na, and Mg were found to be emitting in the post-shock spectra even before the recession reached the seeding depth - therefore possibly characterizing the pyrolysis process rather than the recession itself. The appearance of Ti and V emission in the spectra was well correlated with the actual recession which was monitored through a video of the front surface of the sample. The applicability of a seed material as an indicator for recession appears to be related to the melting temperature of the seed material. Future parametric studies will be carried out in low power plasma facilities at the University of Kentucky.

Butler, Bradley D.↗
NASA NTRS2016

Relating FTS Catalyst Properties to Performance

During the reporting period June 23, 2011 to August 31, 2013, CAER researchers carried out research in two areas of fundamental importance to the topic of cobalt-based Fischer-Tropsch Synthesis (FTS): promoters and stability. The first area was research into possible substitute promoters that might be used to replace the expensive promoters (e.g., Pt, Re, and Ru) that are commonly used. To that end, three separate investigations were carried out. Due to the strong support interaction of γ-Al2O3 with cobalt, metal promoters are commonly added to commercial FTS catalysts to facilitate the reduction of cobalt oxides and thereby boost active surface cobalt metal sites. To date, the metal promoters examined have been those up to and including Group 11. Because two Group 11 promoters (i.e., Ag and Au) were identified to exhibit positive impacts on conversion, selectivity, or both, research was undertaken to explore metals in Groups 12 - 14. The three metals selected for this purpose were Cd, In, and Sn. At a higher loading of 25%Co on alumina, 1% addition of Cd, In, or Sn was found to-on average-facilitate reduction by promoting a heterogeneous distribution of cobalt consisting of larger lesser interacting cobalt clusters and smaller strongly interacting cobalt species. The lesser interacting species were identified in TPR profiles, where a sharp low temperature peak occurred for the reduction of larger, weakly interacting, CoO species. In XANES, the Cd, In, and Sn promoters were found to exist as oxides, whereas typical promoters (e.g., Re, Ru, Pt) were previously determined to exist in an metallic state in atomic coordination with cobalt. The larger cobalt clusters significantly decreased the active site density relative to the unpromoted 25%Co/Al2O3 catalyst. Decreasing the cobalt loading to 15%Co eliminated the large non-interacting species. The TPR peak for reduction of strongly interacting CoO in the Cd promoted catalyst occurred at a measurably lower temperature than in the unpromoted catalyst. Nevertheless, the Co clusters remained slightly larger, on average, in comparison with the unpromoted 15%Co/Al2O3 reference catalyst. None of the promoted catalysts (i.e., with Cd, In, or Sn) exhibited surface Co0 site densities higher than that of the unpromoted catalyst. In activity testing, the activities were even much lower than what was expected from the H2-TPD results. Two possible explanations were proposed: (1) the promoters may be located on the surfaces of cobalt particles, blocking surface Co0 but being able to desorb hydrogen or (2) the promoters may facilitate Co oxidation during FTS, as previously observed by Huffman and coworkers when K was added to cobalt catalysts.

Zirconia↗