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NASA NTRS2013

Materials Science Research Rack Onboard the International Space Station

The Materials Science Research Rack (MSRR) is a research facility developed under a cooperative research agreement between NASA and ESA for materials science investigations on the International Space Station (ISS). MSRR was launched on STS-128 in August 2009 and currently resides in the U.S. Destiny Laboratory Module. Since that time, MSRR has logged more than 1000 hours of operating time. The MSRR accommodates advanced investigations in the microgravity environment on the ISS for basic materials science research in areas such as solidification of metals and alloys. The purpose is to advance the scientific understanding of materials processing as affected by microgravity and to gain insight into the physical behavior of materials processing. MSRR allows for the study of a variety of materials, including metals, ceramics, semiconductor crystals, and glasses. Materials science research benefits from the microgravity environment of space, where the researcher can better isolate chemical and thermal properties of materials from the effects of gravity. With this knowledge, reliable predictions can be made about the conditions required on Earth to achieve improved materials. MSRR is a highly automated facility with a modular design capable of supporting multiple types of investigations. The NASA-provided Rack Support Subsystem provides services (power, thermal control, vacuum access, and command and data handling) to the ESA-developed Materials Science Laboratory (MSL) that accommodates interchangeable Furnace Inserts (FI). Two ESA-developed FIs are presently available on the ISS: the Low Gradient Furnace (LGF) and the Solidification and Quenching Furnace (SQF). Sample Cartridge Assemblies (SCAs), each containing one or more material samples, are installed in the FI by the crew and can be processed at temperatures up to 1400C. ESA continues to develop samples with 14 planned for launch and processing in the near future. Additionally NASA has begun developing SCAs to support US PIs and their partners. The first of these Flight SCAs are being developed for investigations to support research in the areas of crystal growth and liquid phase sintering. Subsequent investigations are in various stages of development. US investigations will include a ground test program in order to distinguish the particular effects of the absence of gravity.

Reagan, Shawn↗
NASA NTRS2016

Materials Science Research Rack Onboard the International Space Station

The Materials Science Research Rack (MSRR) is a research facility developed under a cooperative research agreement between NASA and ESA for materials science investigations on the International Space Station (ISS). MSRR was launched on STS-128 in August 2009 and currently resides in the U.S. Destiny Laboratory Module. Since that time, MSRR has logged more than 1400 hours of operating time. The MSRR accommodates advanced investigations in the microgravity environment on the ISS for basic materials science research in areas such as solidification of metals and alloys. The purpose is to advance the scientific understanding of materials processing as affected by microgravity and to gain insight into the physical behavior of materials processing. MSRR allows for the study of a variety of materials, including metals, ceramics, semiconductor crystals, and glasses. Materials science research benefits from the microgravity environment of space, where the researcher can better isolate chemical and thermal properties of materials from the effects of gravity. With this knowledge, reliable predictions can be made about the conditions required on Earth to achieve improved materials. MSRR is a highly automated facility with a modular design capable of supporting multiple types of investigations. The NASA-provided Rack Support Subsystem provides services (power, thermal control, vacuum access, and command and data handling) to the ESA-developed Materials Science Laboratory (MSL) that accommodates interchangeable Furnace Inserts (FI). Two ESA-developed FIs are presently available on the ISS: the Low Gradient Furnace (LGF) and the Solidification and Quenching Furnace (SQF). Sample Cartridge Assemblies (SCAs), each containing one or more material samples, are installed in the FI by the crew and can be processed at temperatures up to 1400C. ESA continues to develop samples with 14 planned for launch and processing in the near future. Additionally NASA has begun developing SCAs to support US PIs and their partners. The first of these Flight SCAs are being developed for investigations to support research in the areas of crystal growth and liquid phase sintering. Subsequent investigations are in various stages of development. US investigations will include a ground test program in order to distinguish the particular effects of the absence of gravity.

Reagan, Shawn↗
NASA NTRS2016

Materials Science Research Rack Onboard the International Space Station

The Materials Science Research Rack (MSRR) is a research facility developed under a cooperative research agreement between NASA and ESA for materials science investigations on the International Space Station (ISS). MSRR was launched on STS-128 in August 2009 and currently resides in the U.S. Destiny Laboratory Module. Since that time, MSRR has logged more than 1400 hours of operating time. The MSRR accommodates advanced investigations in the microgravity environment on the ISS for basic materials science research in areas such as solidification of metals and alloys. The purpose is to advance the scientific understanding of materials processing as affected by microgravity and to gain insight into the physical behavior of materials processing. MSRR allows for the study of a variety of materials, including metals, ceramics, semiconductor crystals, and glasses. Materials science research benefits from the microgravity environment of space, where the researcher can better isolate chemical and thermal properties of materials from the effects of gravity. With this knowledge, reliable predictions can be made about the conditions required on Earth to achieve improved materials. MSRR is a highly automated facility with a modular design capable of supporting multiple types of investigations. The NASA-provided Rack Support Subsystem provides services (power, thermal control, vacuum access, and command and data handling) to the ESA-developed Materials Science Laboratory (MSL) that accommodates interchangeable Furnace Inserts (FI). Two ESA-developed FIs are presently available on the ISS: the Low Gradient Furnace (LGF) and the Solidification and Quenching Furnace (SQF). Sample Cartridge Assemblies (SCAs), each containing one or more material samples, are installed in the FI by the crew and can be processed at temperatures up to 1400degC. ESA continues to develop samples with 14 planned for launch and processing in the near future. Additionally NASA has begun developing SCAs to support US PIs and their partners. The first of these Flight SCAs are being developed for investigations to support research in the areas of crystal growth and liquid phase sintering. Subsequent investigations are in various stages of development. US investigations will include a ground test program in order to distinguish the particular effects of the absence of gravity.

Reagan, S. E.↗
NASA NTRS2019

New Perspectives of Ancient Mars: Mineral Diversity and Crystal Chemistry at Gale Crater, Mars from the CheMin X-Ray Diffractometer

The Mars Science Laboratory Curiosity rover arrived at Mars in August 2012 with a primary goal of characterizing the habitability of ancient and modern environments. Curiosity landed in Gale crater to study a sequence of ~3.5 Ga old sedimentary rocks that, based on orbital visible/near-infrared reflectance spectra, contain secondary minerals that suggest deposition and/or alteration in liquid water. The sedimentary sequence that comprises the lower slopes of Mount Sharp within Gale crater may preserve a dramatic shift on early Mars from a relatively warm and wet climate to a cold and dry climate based on a transition from smectite-bearing strata to sulfate-bearing strata. The rover is equipped with cameras and geochemical and mineralogical instruments to examine the sedimentology and identify compositional changes within the stratigraphy. These observations provide information about variations in depositional and diagenetic environments over time. The Chemistry and Mineralogy (CheMin) instrument is one of two internal laboratories on Curiosity and includes a transmission X-ray diffractometer (XRD) and X-ray fluorescence (XRF) spectrometer with a Co-K source. CheMin measures loose sediment samples scooped from the surface and drilled rock powders. The XRD provides quantitative mineralogy of scooped and drilled samples to a detection limit of ~1 wt.%. Curiosity has traversed >20 km since landing and has primarily been exploring the site of a predominantly ancient lake environment fed by groundwater and streams emanating from the crater rim. Results from CheMin demonstrate an incredible diversity in the mineralogy of fluvio-lacustrine rocks that signify variations in source rock composition, sediment transport mechanisms, and depositional and diagenetic fluid chemistry. Abundant trioctahedral smectite and magnetite at the base of the section may have formed from low-salinity pore waters with a circumneutral pH within lake sediments. A transition to dioctahedral smectite, hematite, and Ca-sulfate going up section suggests a change to more saline and oxidative aqueous conditions within the lake waters themselves and/or within diagenetic fluids. The primary minerals detected in fluvio-lacustrine samples by CheMin also suggest diversity in the igneous source regions for the sediments, where abundant pyroxene and plagioclase in most samples suggest a basaltic protolith, but sanidine and pyroxene in one sample may have been sourced from a potassic trachyte, and tridymite and sanidine in another sample may have been transported from a rhyolitic source. Crystal chemistry of major phases in each sample have been calculated from refined unit-cell parameters, providing further constraints on aqueous alteration processes and igneous protoliths for the sediments. Perhaps one of the biggest mysteries revealed by the CheMin instrument is the high abundance of X-ray amorphous materials (15 to 73 wt.%) in all samples measured to date. X-ray amorphous materials were detected by CheMin based on the observation of broad humps in XRD patterns. How these materials formed, their composition, and why they persist near the martian surface remain a topic of debate. The sedimentology and composition of the rocks analyzed by Curiosity demonstrate that habitable environments persisted intermittently on the surface or in the subsurface of Gale crater for perhaps more than a billion years.

Rampe, E. B.↗
NASA NTRS2020

Asteroid Cooling Rates Indicated by K-Feldspar Exsolution Textures in H4 Ordinary Chondrites

Undisturbed thermal metamorphism in ordinary chondrite (OC) asteroids, produced through the radioactive decay of 26Al, is expected to result in an onion-shell-like structure. In such a structure, the inner layers of the asteroid experience more extensive thermal metamorphism, as represented by higher petrologic type, than the exterior layers. Furthermore, cooling rates are expected to be slower for OCs of high petrologic type than those of low petrologic type. However, cooling rates determined using metallographic methods and pyroxene diffusion are inconsistent with onion-shell-style cooling and have resulted in new models. These models argue for the disruption of the asteroid after peak metamorphism followed by reaccretion into a rubble pile. Improved constraints on cooling rates would provide a better understanding of the timing and scale of disruptive events. Feldspar microtextures are another tool that can be used to determine asteroid cooling rates. In OC chondrules, plagioclase is present as either a primary phase, or a secondary phase forming from the crystallization of mesostasis glass through petrologic type 4, followed by chemical and textural equilibration. Potas-sium feldspar is observed in petrologic types 3.6-6, as either patches or lamellae exsolved from albite in a perthite texture, often near pores or fractures. Exsolution occurs most commonly, and most extensively, in petrologic type 4. Because the feldspar exsolution wavelength is related to the rate at which grains cooled from the solvus temperature, determined from the mineral’s bulk composition, the chondrite cooling rate can be measured from regions of exsolution. We have previously reported the perthite exsolution cooling rate of Avanhandava, an H4 chondrite, to be 1 °C per 1-4 months over a temperature interval of 765-670 °C. A peristerite exsolution texture was also present in the Na-rich lamellae for which we estimated a cooling rate of 1 °C in 103-104 years from 570-540 °C. Overall, the cooling rates determined from Avanhandava are consistent with pyroxene diffusion (fast cooling at high temperatures) and metallographic rates (slow cooling at low temperatures), hence with the rubble pile model of disruption and reaccretion. Here, we characterize feldspar microtextures in four additional H4 chondrites to test the consistency of feldspar cooling rates across a range of samples. We show that all H4s are similar and support rubble pile models.

Lewis, J. A.↗
NASA NTRSDate not supplied

Nylon-11 Nanowires Embedded in Flexible Substrates for Piezoelectric Transducers

Nylon-11 nanowires have been fabricated in flexible track-etched polymer templates. Customized fabrication equipment was employed to realize an air-flow and gravity assisted template-wetting synthesis technique. X-ray diffraction analysis suggests that the strength of the piezoelectric phase of the nanowire crystals is directly proportional to the air-flow.

piezoelectric↗
NASA NTRSDate not supplied

Using Mineralogy to Interpret Martian Geologic History

The surface mineralogy of Mars is key to interpreting the planet’s geologic history and constraining when and where Mars may have been habitable to microbial life. Orbital mineralogical data from infrared spectrometers collected over the last two decades have demonstrated that Mars is more than a basaltic planet. Thermal infrared (TIR) emission spectrometers have identified regional variations in igneous minerals, iron oxides, and chloride salts, showing evidence for magmatic evolution and aqueous alteration. Orbital visible/shortwave infrared reflectance spectra provide detailed information about the aqueous history of Mars through the identification of clay minerals, sulfates, carbonates, zeolites, and amorphous materials in ancient ~3-4-billion-year-old terrains. Mineralogical data from rovers allow us to better characterize mineral formation mechanisms by identifying mineral assemblages and placing them in geologic context using outcrop- to grain-scale images. TIR and Mössbauer data from the Mars Exploration Rovers helped identify an ancient dune-interdune playa environment with multiple episodes of groundwater at Meridiani Planum and volcanism-induced hydrothermalism at Gusev crater. The CheMin X-ray diffractometer on the Mars Science Laboratory Curiosity rover in Gale crater is the first fully quantitative mineralogical instrument sent to another planetary surface. CheMin data allow the quantification of minerals and X-ray amorphous materials with a mineral detection limit of <1 wt.% and provide crystal chemistry of major phases from refined unit-cell parameters. CheMin has revealed local mineralogical changes in ancient sedimentary rocks not seen from orbit and helped identify habitable environments. Throughout the 600+ m of vertical stratigraphy studied so far, changes in clay mineralogy, Fe-oxides/oxyhydroxides, sulfates, and carbonates demonstrate a long history of surface and groundwater at Gale crater with variable salinity, pH, Eh, and temperature. Recent CheMin data document a decrease in clay minerals and an increase in sulfate minerals in younger strata that corresponds with a change from fluvio-lacustrine to eolian depositional environments, potentially documenting a change to a drier climate across the planet.

E. B. Rampe↗
NASA NTRS2024

Understanding Mercury’s Magmatic History: Geochemical Affinity, Compatibility, & Volatility Changes Due to Reduction

Mercury’s depletion in O and abundance of S substituting in as S2- has fundamental effects on the physicochemical properties of minerals and melts because O2- is the dominant rock-forming anion. These changes exert a first order effect on planetary body evolution, including the initial distribution of elements, crystallization paths, stability of phases, and mineral chemistry. Experimental and empirical data have revealed that most nominally lithophile elements become more chalcophile and/or siderophile at reducing conditions, which can be visualized through a re-interpreted Goldschmidt classification table prepared for McCubbin & Anzures’s Treatises of Geochemistry 3rd edition chapter under review. Additionally, the S bonding environment influences Mercurian phase equilibria by decreasing the stability of forsterite and anorthite while increasing the stability of enstatite, silica, and albite through re-projection of silicate ternaries.

Brendan Anthony Anzures↗
NASA NTRS1998

Advanced thermoelectric materials with enhanced crystal lattice structure and methods of preparation

New skutterudite phases including Ru.sub.0.5 Pd.sub.0.5 Sb.sub.3, RuSb.sub.2 Te, and FeSb.sub.2 Te, have been prepared having desirable thermoelectric properties. In addition, a novel thermoelectric device has been prepared using skutterudite phase Fe.sub.0.5 Ni.sub.0.5 Sb.sub.3. The skutterudite-type crystal lattice structure of these semiconductor compounds and their enhanced thermoelectric properties results in semiconductor materials which may be used in the fabrication of thermoelectric elements to substantially improve the efficiency of the resulting thermoelectric device. Semiconductor materials having the desired skutterudite-type crystal lattice structure may be prepared in accordance with the present invention by using powder metallurgy techniques. Measurements of electrical and thermal transport properties of selected semiconductor materials prepared in accordance with the present invention, demonstrated high Hall mobilities and good Seebeck coefficients. These materials have low thermal conductivity and relatively low electrical resistivity, and are good candidates for low temperature thermoelectric applications.

Fleurial, Jean-Pierre↗
NASA NTRS1984

The effect of tantalum and carbon on the structure/properties of a single crystal nickel-base superalloy

The microstructure, phase chemistry, and creep and hot tensile properties were studied as a function of tantalum and carbon levels in Mar-M247 type single crystal alloys. Microstructural studies showed that several types of carbides (MC, M23C6 and M5C) are present in the normal carbon (0.10 wt % C) alloys after heat treatment. In general, the composition of the MC carbides changes from titanium rich to tantalum rich as the tantalum level in the alloy increases. Small M23C6 carbides are present in all alloys. Tungsten rich M6C carbides are also observed in the alloy containing no tantalum. No carbides are present in the low carbon (0.01 wt % C) alloy series. The morphology of gamma prime is observed to be sensitive to heat treatment and tantalum level in the alloy. Cuboidal gamma prime is present in all the as cast structures. After heat treatment, the gamma prime precipitates tend to have a more spheroidal like morphology, and this tendency increases as the tantalum level decreases. On prolonged aging, the gamma prime reverts back to a cuboidal morphology or under stress at high temperatures, forms a rafted structure. The weight fraction and lattice parameter of the spheroidal gamma prime increases with increasing tantalum content. Changes in the phase chemistry of the gamma prime matrix and gamma prime have also been analyzed using phase extraction techniques. The partitioning ratio decreases for tungsten and aluminum and increases for tantalum as the tantalum content increases for both alloy series; no significant changes occur in the partitioning ratios of the other alloying elements. A reduction in secondary creep rate and an increase in rupture time result from increasing the tantalum content and decreasing the carbon level.

Nguyen, H. C.↗
NASA NTRS2006

Fluorescent Approaches to High Throughput Crystallography

We have shown that by covalently modifying a subpopulation, less than or equal to 1%, of a macromolecule with a fluorescent probe, the labeled material will add to a growing crystal as a microheterogeneous growth unit. Labeling procedures can be readily incorporated into the final stages of purification, and the presence of the probe at low concentrations does not affect the X-ray data quality or the crystallization behavior. The presence of the trace fluorescent label gives a number of advantages when used with high throughput crystallizations. The covalently attached probe will concentrate in the crystal relative to the solution, and under fluorescent illumination crystals show up as bright objects against a dark background. Non-protein structures, such as salt crystals, will not incorporate the probe and will not show up under fluorescent illumination. Brightly fluorescent crystals are readily found against less bright precipitated phases, which under white light illumination may obscure the crystals. Automated image analysis to find crystals should be greatly facilitated, without having to first define crystallization drop boundaries as the protein or protein structures is all that shows up. Fluorescence intensity is a faster search parameter, whether visually or by automated methods, than looking for crystalline features. We are now testing the use of high fluorescence intensity regions, in the absence of clear crystalline features or "hits", as a means for determining potential lead conditions. A working hypothesis is that kinetics leading to non-structured phases may overwhelm and trap more slowly formed ordered assemblies, which subsequently show up as regions of brighter fluorescence intensity. Preliminary experiments with test proteins have resulted in the extraction of a number of crystallization conditions from screening outcomes based solely on the presence of bright fluorescent regions. Subsequent experiments will test this approach using a wider range of proteins. The trace fluorescently labeled crystals will also emit with sufficient intensity to aid in the automation of crystal alignment using relatively low cost optics, further increasing throughput at synchrotrons.

Pusey, Marc L.↗
NASA NTRS2007

Gravity Probe B Timing System and Roll Phase Determination

An oven-controlled crystal oscillator at 16.368 MHz provides clock signals to all GP-B components and synchronizes the data collection, transmission and processing. The sampled science data signals are stamped with the vehicle time, a counter of the 10Hz data strobe divided down from the clock. The GPS receiver supplies an external reference for time transfer between the vehicle time and coordinated universal time. Ground and space flight tests show the time transfer error is within 1 microsecond. The time latency between the effective sample time of science signals and the stamped vehicle time is verified to 1 ms in the ground tests. The GP-B satellite is controlled to roll with a period of 77.5 sec about an axis along the direction to the guide star to average out the disturbance torques fixed to the body of the satellite and reduce the gyroscope readout noise. The roll phase is determined on the ground to high accuracy with the telemetry data from two star trackers and used in the data analysis to separate the drifts of gyroscope spin axes in the orbital plane and perpendicular to the orbital plane. The flight data shows that the roll phase is controlled to within 40 arcsec with a measurement uncertainty of 7 arcsec.

Jie, Li↗
NASA NTRS2016

Rheological Properties of Quasi-2D Fluids in Microgravity

Freely suspended smectic films of sub-micrometer thickness and lateral extensions of several millimeters are used to study thermally driven convection and diffusion in the film plane. The experiments were performed during a six minute microgravity phase of a TEXUS suborbital rocket flight (Texus 52, launched April 27, 2015). The project served as a preliminary test for a planned ISS Experiment with liquid crystal films (OASIS), and in addition it provided new experimental data on smectic films exposed to in-plane thermal gradients.We find an attraction of the smectic material towards the cold edge of the film in a temperature gradient, similar to a Soret effect. This process is reversed when this edge is heated up again. Thermal convection driven by two thermocontacts in the film is practically absent, even at temperature gradients up to 10 Kmm, thermally driven convection sets in when the hot post reaches the transition temperature to the nematic phase.An additional experiment was performed under microgravity conditions to test the stability of liquid crystal bridges in different smectic phases.

microgravity↗
NASA NTRS2004

Novel Microstructures for Polymer-Liquid Crystal Composite Materials

There are a number of interface-dominated composite materials that contain a liquid crystalline (LC) phase in intimate contact with an isotropic phase. For example, polymer- dispersed liquid crystals, used in the fabrication of windows with switchable transparency, consist of micron size LC droplets dispersed in an isotropic polymer matrix. Many other types of liquid crystal composite materials can be envisioned that might have outstanding optical properties that could be exploited in novel chemical sensors, optical switches, and computer displays. This research project was based on the premise that many of these potentially useful LC composite materials can only be fabricated under microgravity conditions where gravity driven flows are absent. In the ground-based research described below, we have focused on a new class of LC composites that we call thermotropic- lyotropic liquid crystal systems (TLLCs). TLLCs consist of nanosize droplets of water dispersed in an LC matrix, with surfactants at the interface that stabilize the structure. By varying the type of surfactant one can access almost an infinite variety of unusual LC composite microstructures. Due to the importance of the interface in these types of systems, we have also developed molecular simulation models for liquid crystals at interfaces, and made some of the first measurements of the interfacial tension between liquid crystals and water.

Magda, Jules J.↗
NASA NTRS2000

Growth of Megaspherulites In a Rhyolitic Vitrophyre

Megaspherulites occur in the middle zone of a thick sequence of rhyolitic vitrophyre that occupies a small, late Eocene to early Oligocene volcanic-tectonic basin near Silver Cliff, Custer County, Colorado. Diameters of the megaspherulites range from 0.3 m to over 3.66 m, including a clay envelope. The megaspherulites are compound spherulites. consisting of an extremely large number (3.8 x 10(exp 9) to 9.9 x 10(exp 9)) of individual growth cones averaging 3 mm long by 1.25 mm wide at their termination. They are holocrystalline, very fine- to fine-grained, composed of disordered to ordered sanidine (orthoclase) and quartz, and surrounded by a thin K-feldspar, quartz rich rind, an inner clay layer with mordenite, and an outer clay layer composed wholly of 15 A montmorillonite. Whole rock analyses of the megaspherulites show a restricted composition from their core to their outer edge, with an average analyses of 76.3% SiO2, 0.34% CaO, 2.17% Na2O, 6.92% K2O, 0.83% H2O+ compared to the rhyolitic vitrophyre from which they crystallize with 71.07% SiO2, 0.57% CaO, 4.06% Na2O,4.l0% K2O, and 6.40% H2O+. The remaining oxides of Fe2O3 (total Fe), A12O3, MnO,MgO, TiO2, P2O5, Cr2O3, and trace elements show uniform distribution between the megaspherulites and the rhyolitic vitrophyre. Megaspherulite crystallization began soon after the rhyolitic lava ceased to flow as the result of sparse heterogeneous nucleation, under nonequilibrium conditions, due to a high degree of undercooling, delta T. The crystals grow with a fibrous habit which is favored by a large delta T ranging between 245 C and 295 C, despite lowered viscosity, and enhanced diffusion due to the high H2O content, ranging between 5% and 7%. Therefore, megaspherulite growth proceeded in a diffusion controlled manner, where the diffusion, rate lags behind the crystal growth rate at the crystal-liquid interface, restricting fibril lengths and diameters to the 10 micron to 15 micron and 3 micron and 8 micron ranges respectively. Once diffusion reestablishes itself at the crystallization front, a new nucleation event occurs at the terminated tips of the fibril cones and a new cone begins to develop with a similar orientation (small angle branching) to the earlier cones. During crystallization, these fibril cones impinge upon each other, resulting in fibril cone-free areas. These cone-free areas consist of coarser, fine-grained phases, dominated by quartz, which crystallized from the melt as it accumulated between the crystallizing K-feldspar fibrils of the cones. The anhydrous nature of the disordered to ordered sanidine (orthoclase) and quartz, suggests that water in the vitrophyre moved ahead of the crystallization front, resulting in a water rich fluid being enriched in Si, K, Na, Mg, Ca, Sr, Ba, and Y. The clay layers associated with the megaspherulites are therefore, the result of the deuteric alteration between the fractionated water and the vitrophyre, as indicated by the presence of the minerals mordenite and montmorillonite. This silica rich fluid also resulted in the total silicification of the megaspherulites within the upper 3 m of the vitrophyre.

Smith, Robert K.↗