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All sourcesNASA NTRSDOE OSTI
NASA NTRS2016

Fabricating with Crystalline Si to Improve Superconducting Detector Performance

We built and measured radio-frequency (RF) loss tangent, tan d, evaluation structures using float-zone quality silicon-on-insulator (SOI) wafers with 5 µ m thick device layers. Superconducting Nb components were fabricated on both sides of the SOI Si device layer. Our main goals were to develop a robust fabrication for using crystalline Si (c-Si) dielectric layers with superconducting Nb components in a wafer bonding process and to confirm that tan d with c-Si dielectric layers was reduced at RF frequencies compared to devices fabricated with amorphous dielectrics, such as SiO2 and SixNy, where tan d ~ 10-3. Our primary test structure used a Nb coplanar waveguide (CPW) readout structure capacitively coupled to LC resonators, where the capacitors were defined as parallel-plate capacitors on both sides of a c-Si device layer using a wafer bonding process with benzocyclobutene (BCB) wafer bonding adhesive. Our control experiment, to determine the intrinsic tan d in the SOI device layer without wafer bonding, also used Nb CPW readout coupled to LC resonators; however, the parallel-plate capacitors were fabricated on both sides of the Si device layer using a deep reactive ion etch (DRIE) to access the c-Si underside through the buried oxide and handle Si layers in the SOI wafers. We found that our wafer bonded devices demonstrated F· d = (8 ± 2) × 10-5, where F is the filling fraction of two-level states (TLS). For the control experiment, F· d = (2.0 ± 0.6) × 10-5, and we discuss what may be degrading the performance in the wafer bonded devices as compared to the control devices.

Beyer, A D↗
NASA NTRS2016

Fabricating with Crystalline Si to Improve Superconducting Detector Performance

We built and measured radio-frequency (RF) loss tangent, tan δ, evaluation structures using float-zone quality silicon-on-insulator (SOI) wafers with 5 μm thick device layers. Superconducting Nb components were fabricated on both sides of the SOI Si device layer. Our main goals were to develop a robust fabrication for using crystalline Si (c-Si) dielectric layers with superconducting Nb components in a wafer bonding process and to confirm that tan δ with c-Si dielectric layers was reduced at RF frequencies compared to devices fabricated with amorphous dielectrics, such as SiO2 and SixNy, where tan δ ~ 10(exp -3). Our primary test structure used a Nb coplanar waveguide (CPW) readout structure capacitively coupled to LC resonators, where the capacitors were defined as parallel-plate capacitors on both sides of a c-Si device layer using a wafer bonding process with benzocyclobutene (BCB) wafer bonding adhesive. Our control experiment, to determine the intrinsic tan δ in the SOI device layer without wafer bonding, also used Nb CPW readout coupled to LC resonators; however, the parallel-plate capacitors were fabricated on both sides of the Si device layer using a deep reactive ion etch (DRIE) to access the c-Si underside through the buried oxide and handle Si layers in the SOI wafers. We found that our wafer bonded devices demonstrated F· δ = (8 +/- 2) × 10(exp -5), where F is the filling fraction of two-level states (TLS). For the control experiment, F· δ = (2.0 +/- 0.6) × 10(exp -5), and we discuss what may be degrading the performance in the wafer bonded devices as compared to the control devices.

Beyer, A. D↗
NASA NTRS2004

Deformation, Stress Relaxation, and Crystallization of Lithium Silicate Glass Fibers Below the Glass Transition Temperature

The deformation and crystallization of Li(sub 2)O (center dot) 2SiO2 and Li(sub 2)O (center dot) 1.6SiO2 glass fibers subjected to a bending stress were measured as a function of time over the temperature range -50 to -150 C below the glass transition temperature (Tg). The glass fibers can be permanently deformed at temperatures about 100 C below T (sub)g, and they crystallize significantly at temperatures close to, but below T,, about 150 C lower than the onset temperature for crystallization for these glasses in the no-stress condition. The crystallization was found to occur only on the surface of the glass fibers with no detectable difference in the extent of crystallization in tensile and compressive stress regions. The relaxation mechanism for fiber deformation can be best described by a stretched exponential (Kohlrausch-Williams-Watt (KWW) approximation), rather than a single exponential model.The activation energy for stress relaxation, Es, for the glass fibers ranges between 175 and 195 kJ/mol, which is considerably smaller than the activation energy for viscous flow, E, (about 400 kJ/mol) near T, for these glasses at normal, stress-free condition. It is suspected that a viscosity relaxation mechanism could be responsible for permanent deformation and crystallization of the glass fibers below T,

Ray, Chandra S.↗
NASA NTRS1997

Geochemistry of approximately 1.9 Ga sedimentary rocks from northeastern Labrador, Canada

Fifty-eight rock chips from fifteen samples of sedimentary rocks from the Ramah Group (approximately 1.9 Ga) in northeastern Labrador, Canada, were analyzed for major and minor elements, including C and S, to elucidate weathering processes on the Earth's surface about 1.9 Ga ago. The samples come from the Rowsell Harbour, Reddick Bight, and Nullataktok Formations. Two rock series, graywackes-gray shales of the Rowsell Harbour, Reddick Bight and Nullataktok Formations, and black shales of the Nullataktok Formation, are distinguishable on the basis of lithology, mineralogy, and major and trace element chemistry. The black shales show lower concentrations than the graywackes-gray shales in TiO2 (0.3-0.7 wt% vs. 0.7-1.8 wt%), Al2O3 (9.5-20.1 wt% vs. 13.0-25.0 wt%), and sigma Fe (<1 wt% vs. 3.8-13.9 wt% as FeO). Contents of Zr, Th, U, Nb, Ce, Y, Rb, Y, Co, and Ni are also lower in the black shales. The source rocks for the Ramah Group sediments were probably Archean gneisses with compositions similar to those in Labrador and western Greenland. The major element chemistry of source rocks for the Ramah Group sedimentary rocks was estimated from the Al2O3/TiO2 ratios of the sedimentary rocks and the relationship between the major element contents (e.g., SiO2 wt%) and Al2O3/TiO2 ratios of the Archean gneisses. This approach is justified, because the Al/Ti ratios of shales generally retain their source rock values; however, the Zr/Al, Zr/Ti, and Cr/Ni ratios fractionate during the transport of sediments. The measured SiO2 contents of shales in the Ramah Group are generally higher than the estimated SiO2 contents of source rocks by approximately 5 wt%. This correction may also have to be applied when estimating average crustal compositions from shales. Two provenances were recognized for the Ramah Group sediments. Provenance I was comprised mostly of rocks of bimodal compositions, one with SiO2 contents approximately 45 wt% and the other approximately 65 wt%, and was the source for most sedimentary rocks of the Ramah Group, except for black shales of the Nullataktok Formation. The black shales were apparently derived from Provenance II that was comprised mostly of felsic rocks with SiO2 contents approximately 65 wt%. Comparing the compositions of the Ramah Group sedimentary rocks and their source rocks, we have recognized that several major elements, especially Ca and Mg, were lost almost entirely from the source rocks during weathering and sedimentation. Sodium and potassium were also leached almost entirely during the weathering of the source rocks. However, significant amounts of Na were added to the black shales and K to all the rock types during diagenesis and/or regional metamorphism. The intensity of weathering of source rocks for the Ramah Group sediments was much higher than that of typical Phanerozoic sediments, possibly because of a higher PCO2 in the Proterozoic atmosphere. Compared to the source rock values, the Fe3+/Ti ratios of many of the graywackes and gray shales of the Ramah Group are higher, the Fe2+/Ti ratios are lower, and the sigma Fe/Ti ratios are the same. Such characteristics of the Fe geochemistry indicate that these sedimentary rocks are comprised of soils formed by weathering of source rocks under an oxygen-rich atmosphere. The atmosphere about 1.9 Ga was, therefore, oxygen rich. Typical black shales of Phanerozoic age exhibit positive correlations between the organic C contents and the concentrations of S, U, and Mo, because these elements are enriched in oxygenated seawater and are removed from seawater by organic matter in sediments. However, such correlations are not found in the Ramah Group sediments. Black shales of the Ramah Group contain 1.7-2.8 wt% organic C, but are extremely depleted in sigma Fe (<1 wt% as FeO), S (<0.3 wt%), U (approximately l ppm), Mo (<5 ppm), Ni (<2 ppm), and Co (approximately 0 ppm). This lack of correlation, however, does not imply that the approximately 1.9 Ga atmosphere-ocean system was anoxic. Depletion of these elements from the Ramah Group sediments may have occurred during diagenesis.

Non-NASA Center↗
NASA NTRS2023

An Improved Hf Vapor Etching Apparatus for Stardust Particle Extraction

Introduction: The NASA Stardust mission captured thousands of particles from the Jupiter-family comet 81P/Wild 2 in a collector composed of aluminum foil and blocks of silica aerogel [1]. To date, most Wild 2 particles available for study are relatively large and coherent particles extracted individually from the ends of hollow, carrot-shaped impact tracks produced during impact into aerogel. However, >65% of the impacting mass can be found in the ‘bulb’ of the track, including nearly all of the <1 μm size fraction [2]. This fraction contains organic-rich material and is likely to include presolar grains, representing a critical opportunity to constrain the organic and presolar inventory of primitive outer solar system materials. However, the small size and susceptibility of this fraction to melting or alteration during capture poses significant analytical challenges. Previous attempts to extract and concentrate fine-grained material from the bulb of Stardust tracks have attempted to develop techniques that efficiently destroy aerogel and leave impactor particles relatively unharmed. The low density and high porosity of silica aerogel makes it more susceptible to attack by etching with hydrofluoric acid (HF) [3] or CF4 plasma ashing [4] than collected cometary silicates. Previous studies of HF vapor etching used HF solutions varying between 5 to 49% and noted that at high concentrations and etch rates, a liquid droplet was produced according to the etching reaction 4HF + SiO2 → SiF4 (g) + 2H2O [3]. SiF4 readily decomposes into HF and silicic acid in water, which has the potential to alter the freed cometary silicates. The plasma ashing technique avoids production of a liquid droplet and minimizes damage to embedded silicates but requires specialized equipment [4]. In this abstract, we present recent improvements to the HF etching procedure with the aim of constructing an etching chamber capable of slowly etching silica aerogel using small quantities of dilute HF. The etching chamber can be assembled using readily available materials.

Stardust↗
NASA NTRS1996

Atomic Oxygen Durability of Second Surface Silver Microsheet Glass Concentrators

Second surface silver microsheet glass concentrators are being developed for potential use in future solar dynamic space power systems. Traditional concentrators are aluminum honeycomb sandwich composites with either aluminum or graphite epoxy face sheets, where a reflective aluminum layer is deposited onto an organic leveling layer on the face sheet. To protect the underlying layers, a SiO2 layer is applied on top of the aluminum reflective layer. These concentrators may be vulnerable to atomic oxygen degradation due to possible atomic oxygen attack of the organic layers at defect sites in the protective and reflective coatings. A second surface microsheet glass concentrator would be inherently more atomic oxygen durable than these first surface concentrators. In addition, a second surface microsheet glass concentrator design provides a smooth optical surface and allows for silver to be used as a reflective layer, which would improve the reflectivity of the concentrator and the performance of the system. A potential threat to the performance of second surface microsheet glass concentrators is atomic oxygen attack of the underlying silver at seams and edges or at micrometeoroid and debris (MMD) impacts sites. Second surface silver microsheet glass concentrator samples were fabricated and tested for atomic oxygen durability. The samples were iteratively exposed to an atomic oxygen environment in a plasma asher. Samples were evaluated for potential degradation at fabrication seams, simulated MMD impact sites, and edges. Optical microscopy was used to evaluate atomic oxygen degradation. Reflectance was obtained for an impacted sample prior to and after atomic oxygen exposure. After an initial atomic oxygen exposure to an effective fluence of approx. 1 x 10(exp 21) atoms/cm(exp 2), oxidation of the silver at defect sites and edges was observed. Exposure to an additional approx. 1 x 10(exp 21) atoms/cm(exp 2) caused no observed increase in oxidation. Oxidation at an impact site caused negligible changes in reflectance. In all cases oxidation was found to be confined to the vicinity of the seams, impact sites, edges or defect sites. Asher to in-space atomic oxygen correlation issues will be addressed.

deGroh, Kim K.↗
NASA NTRSDate not supplied

Tin-Essako 001: A Metal-Rich Ureilite?

Introduction: Metal-rich achondrites include a variety of types, and likely have a variety of origins. Models range from gravitational mixing at the core-mantle boundaries of differentatiated asteroids, to complex impact mixing scenarios. We describe a new type of metal-rich achondrite that might be the first metal-rich ureilite. Sample: Tin-Essako (TE) 001 (~4.3 g) was found in Mali in 2020 and purchased by Jay Piatek in 2021. It was classified as a metal-rich ungrouped achondrite, with olivine and oxygen isotope (d18O=8.2810‰, d17O=3.718‰, avg. 3) compositions suggesting affinity to ureilites [1]. We studied one polished section (~187.7 mm2) of TE 001. Petrography: TE 001 consists of ~60% metal and 40% silicates, heterogeneously distributed. The metal is largely fresh, but iron oxides (presumably terrestrial) occur along one edge and in some patches and veins in the interior. The silicates are dominantly olivine (≥90%), with melt-textured areas of plagioclase + Si-rich glass. Minor phases include chromite and carbon. Olivine occurs as rounded grains (up to ~2.5 mm) in metal, commonly with rims of melt-textured plagioclase + glass. Olivine also occurs in more massive areas having a “honeycomb” texture, with rounded olivine “cells” surrounded by an interstitial network of reduced olivine riddled with tiny metal grains, plus melt-textured plagioclase + Si-rich glass. Chromite occurs as subhedral to rounded grains; smaller grains (30-250 mm) are included in olivine and a few larger grains (400-500 mm) are isolated within metal. A carbon phase occurs as lacy-textured rims around olivine grains in metal, or small patches within metal. Mineral Compositions: The olivine (excluding interstitial areas) is Fo 73.9±0.5, with 0.25±0.02 wt.% CaO, 0.31±0.01 wt% Cr2O3, 0.01 wt.% NiO, and molar Fe/Mn=49.8±2.2 (53 analyses). Olivine in interstitial areas has Fo up to at least 91. Smaller chromite grains have Fe# (molar Fe/[Fe+Mg]) = 0.54±0.01, Cr# (molar Cr/[Cr+Al]) = 0.52±0.01, 0.52±0.02 wt.% V2O3 and 0.21±0.04 wt% ZnO (28 analyses). One larger grain is zoned from Fe# = 0.45, Cr# =0.52 to Fe# = 0.40, Cr# =0.57, and contains thin Al-rich lamellae not resolved by EMPA. One irregularly shaped patch of chromite included in olivine has Fe# =0.26 and contains no ZnO. Plagioclase laths are An ~53-60, with ≤0.01 wt.% K2O. Glass contains 75-76 wt% SiO2 and ~16 wt% Al2O3. The metal contains 5.2±0.2 wt% Ni, 0.46±0.02 wt.% Co, and 0.01±0.01 wt.% Cr, with Si and P below detection (168 analyses). Discussion: The olivine + chromite assemblage in TE 001 is similar to the most ferroan ureilites (Fo ~75-79 [2]), as are the oxygen isotopes [1]. The presence of a carbon phase supports this, although the identity of this phase (graphite as in ureilites?) remains to be determined. The “honeycomb” textured areas, in particular, the presence of olivine “reduction rims,” resemble shock-smelted olivine areas in ureilites [3], but interstitial melt-textured plagioclase laths + glass like those in TE 001 have not been reported in such (or any) ureilites. Olivine in TE 001 is marginally more ferroan than in the most FeO-rich ureilite, with Fe-Mg-Mn composition offset from the trend of olivine + low-Ca pyroxene ureilites similar to augite-bearing ureilites [4]. CaO and Cr2O3 contents are in the range of those in ureilite olivine [ ] , though Cr2O3 is at the extreme low end of the range [5]. Chromites (except the unusual one) have similar Fe# to the most ferroan primary chromites in ureilites [2], but distinctly lower Cr# (0.52 vs. 0.71). Metal compositions are with the range for metal in ureilites [7]. The absence of pyroxene and sulfide, and the high abundance of metal in TE 001, are unlike ureilites. One possibility is that a ferroan, chromite-bearing, pyroxene-poor ureilite was invaded (possibly due to impact) by a metallic liquid (low S content suggests very high temperature), resulting in complete melting of pyroxene and smelting of olivine, with rapid recrystallization of melted silicate as plagioclase + glass. Alternatively, a pre-existing metal-rich ureilite assemblage may have been impact melted. Additional types of data will be obtained to evaluate these hypotheses (i.e., is the metal indigenous?) and assess affinity to ureilites.

olivine↗
NASA NTRS2012

Optical and Scanning Electron Microscopy of the Materials International Space Station Experiment (MISSE) Spacecraft Silicone Experiment

Under a microscope, atomic oxygen (AO) exposed silicone surfaces are crazed and seen as "islands" separated by numerous crack lines, much analogous to mud-tile cracks. This research characterized and compared the degree of AO degradation of silicones by analyzing optical microscope images of samples exposed to low Earth orbit (LEO) AO as part of the Spacecraft Silicone Experiment. The Spacecraft Silicone Experiment consisted of eight DC 93-500 silicone samples exposed to eight different AO fluence levels (ranged from 1.46 to 8.43 10(exp 21) atoms/sq cm) during two different Materials International Space Station Experiment (MISSE) missions. Image analysis software was used to analyze images taken using a digital camera. To describe the morphological degradation of each AO exposed flight sample, three different parameters were selected and estimated: (1) average area of islands was determined and found to be in the 1000 to 3100 sq mm range; (2) total length of crack lines per unit area of the sample surface were determined and found to be in the range of 27 to 59 mm of crack length per sq mm of sample surface; and (3) the fraction of sample surface area that is occupied by crack lines was determined and found to be in the 25 to 56 percent range. In addition, average crack width can be estimated from crack length and crack area measurements and was calculated to be about 10 mm. Among the parameters studied, the fraction of sample surface area that is occupied by crack lines is believed to be most useful in characterizing the degree of silicone conversion to silicates by AO because its value steadily increases with increasing fluence over the entire fluence range. A series of SEM images from the eight samples exposed to different AO fluences suggest a complex sequence of surface stress due to surface shrinkage and crack formation, followed by re-distribution of stress and shrinking rate on the sample surface. Energy dispersive spectra (EDS) indicated that upon AO exposure, carbon content on the surface decreased relatively quickly at the beginning, to 32 percent of the pristine value for the least exposed sample in this set of experiments (1.46 10(exp 21) atoms/sq cm), but then decreased slowly, to 22 percent of the pristine value for the most exposed sample in this set of experiment (8.43 10(exp 21) atoms/sq cm). The oxygen content appears to increase at a slower rate. The least and most AO exposed samples were, respectively, 52 and 150 percent above the pristine values. The silicone samples with the greater AO exposure (7.75 10(exp 21) atoms/sq cm and higher) appear to have a surface layer which contains SiO2 with perhaps small amounts of unreacted silicone, CO and CO2 sealed inside.

Hung, Ching-cheh↗