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Using Technology to Better Characterize the Apollo Sample Suite: A Retroactive PET Analysis and Potential Model for Future Sample Return Missions

From 1969-1972 the Apollo missions collected 382 kg of lunar samples from six distinct locations on the Moon. Studies of the Apollo sample suite have shaped our understanding of the formation and early evolution of the Earth-Moon system, and have had important implications for studies of the other terrestrial planets (e.g., through the calibration of the crater counting record) and even the outer planets (e.g., the Nice model of the dynamical evolution of the Solar System). Despite nearly 50 years of detailed research on Apollo samples, scientists are still developing new theories about the origin and evolution of the Moon. Three areas of active research are: (1) the abundance of water (and other volatiles) in the lunar mantle, (2) the timing of the formation of the Moon and the duration of lunar magma ocean crystallization, (3) the formation of evolved lunar lithologies (e.g., granites) and implications for tertiary crustal processes on the Moon. In order to fully understand these (and many other) theories about the Moon, scientists need access to "new" lunar samples, particularly new plutonic samples. Over 100 lunar meteorites have been identified over the past 30 years, and the study of these samples has greatly aided in our understanding of the Moon. However, terrestrial alteration and the lack of geologic context limit what can be learned from the lunar meteorites. Although no "new" large plutonic samples (i.e., hand-samples) remain to be discovered in the Apollo sample collection, there are many large polymict breccias in the Apollo collection containing relatively large (approximately 1 cm or larger) previously identified plutonic clasts, as well as a large number of unclassified lithic clasts. In addition, new, previously unidentified plutonic clasts are potentially discoverable within these breccias. The question becomes how to non-destructively locate and identify new lithic clasts of interest while minimizing the contamination and physical degradation of the samples.

Zeigler, R. A.↗

Heterogeneity Determination and Purification of Commercial Hen Egg-White Lysozyme

Hen egg-white lysozyme (HEWL) is widely used as a model protein, although its purity has not been adequately characterized by modern biochemical techniques. We have identified and quantified the protein heterogeneities in three commercial HEWL preparations by sodium dodecyl sulfate polyacrylamide gel electrophoresis with enhanced silver staining, reversed-phase fast protein liquid chromatography (FPLC) and immunoblotting with comparison to authentic protein standards. Depending on the source, the contaminating proteins totalled 1-6%(w/w) and consisted of ovotransferrin, ovalbumin, HEWL dimers, and polypeptides with approximate M(sub r) of 39 and 18 kDa. Furthermore, we have obtained gram quantities of electrophoretically homogeneous [> 99.9%(w/w)] HEWL by single-step semi-preparative scale cation-exchange FPLC with a yield of about 50%. Parallel studies of crystal growth kinetics, salt repartitioning and crystal perfection with this highly purified material showed fourfold increases in the growth-step velocities and significant enhancement in the structural homogeneity of HEWL crystals.

Thomas, B. R.↗

Triboluminescent Materials for Smart Optical Damage Sensors for Space Applications

There is a need to develop a new technique of damage detection for composites, which could detect cracking or delamination from any desired location within a material structure in real time. Recently, triboluminescent materials have been proposed as smart sensors of structural damage. To sense the damage, these materials can be epoxy bonded, coated in a polymer matrix, or embedded in a composite host structure. When the damage or fracture takes place in the host structure, the resultant fracture of triboluminescent crystals creates a light emission. This will warn in real time that structural damage has occurred. The triboluminescent emission of the candidate phosphor has to be bright enough that the light reaching from the point of fracture to the detector through a fiber optic cable is detectable. There are a large number of triboluminescent materials, but few satisfy the above criterion. The authors have synthesized an organic material known as Europium tetrakis (dibenzoylmethide) triethylammonium (EuD4TEA), which is a potential candidate for application as a damage sensor and could be made into a wireless sensor with the addition of microchip, antenna, and electronics. Preliminary results on the synthesis and characterization of this material are presented.

Aggarwal, M. D.↗

X-Ray Diffraction Wafer Mapping Method for Rhombohedral Super-Hetero-Epitaxy

A new X-ray diffraction (XRD) method is provided to acquire XY mapping of the distribution of single crystals, poly-crystals, and twin defects across an entire wafer of rhombohedral super-hetero-epitaxial semiconductor material. In one embodiment, the method is performed with a point or line X-ray source with an X-ray incidence angle approximating a normal angle close to 90 deg, and in which the beam mask is preferably replaced with a crossed slit. While the wafer moves in the X and Y direction, a narrowly defined X-ray source illuminates the sample and the diffracted X-ray beam is monitored by the detector at a predefined angle. Preferably, the untilted, asymmetric scans are of {440} peaks, for twin defect characterization.

Park, Yoonjoon↗

Extremum-seeking control for an Ultrasonic/Sonic Driller/Corer (USDC) driven at high-power

Future NASA exploration missions will increasingly require sampling, in-situ analysis and possibly the return of material to Earth for further tests. One of the challenges to addressing this need is the ability to drill using for low axial loading while operating from light weight platforms (e.g., lander, rover, etc.) as well as operate at planets with low gravity. For this purpose, the authors developed the Ultrasonic/Sonic Driller/Corer (USDC) jointly with Cybersonics Inc. Studies of the operation of the USDC at high power have shown there is a critical need to self-tune to maintain the operation of the piezoelectric actuator at resonance. Performing such tuning is encountered with difficulties and to address them an extremum-seeking control algorithm is being investigated. This algorithm is designed to tune the driving frequency of a time-varying resonating actuator subjected to both random and high-power impulsive noise disturbances. Using this algorithm the performance of the actuator is monitored on a time-scale that is compatible with its slowly time-varying physical characteristics. The algorithm includes a parameter estimator, which estimates the coefficients of a function that characterizes the quality factor of the USDC. Since the parameter estimator converges sufficiently faster than the time-varying drift of the USDC's physical parameters, the proposed extremum-seeking estimation and control algorithm is potentially applicable for use as a closed-loop health monitoring system. Specifically, this system may be programmed to automatically adjust the duty-cycle of the sinusoidal driver signal to guarantee that the quality factor of the USDC does not fall below a user-defined set-point. Such fault-tolerant functionality is especially important in automated drilling applications where it is essential not to inadvertently drive the piezoelectric ceramic crystals of the USDC beyond their capacities. The details of the algorithm and experimental results will be described and discussed in this paper.

Peek-seeking estimation and control↗

Ice Cloud Backscatter Study and Comparison with CALIPSO and MODIS Satellite Data

An invariant imbedding T-matrix (II-TM) method is used to calculate the single-scattering properties of 8-column aggregate ice crystals. The II-TM based backscatter values are compared with those calculated by the improved geometric-optics method (IGOM) to refine the backscattering properties of the ice cloud radiative model used in the MODIS Collection 6 cloud optical property product. The integrated attenuated backscatter-to-cloud optical depth (IAB-ICOD) relation is derived from simulations using a CALIPSO (Cloud-Aerosol Lidar and Infrared Pathfinder Satellite) lidar simulator based on a Monte Carlo radiative transfer model. By comparing the simulation results and co-located CALIPSO and MODIS (Moderate Resolution Imaging Spectroradiometer) observations, the non-uniform zonal distribution of ice clouds over ocean is characterized in terms of a mixture of smooth and rough ice particles. The percentage of the smooth particles is approximately 6 percent and 9 percent for tropical and mid-latitude ice clouds, respectively.

MODIS↗

Phosphate (U-Th)/He Thermochronology of Apollo 14 Melt Breccia 14311

Our ability to confidently characterize the impact history of the inner solar system is limited by discrepancies in radiometric dates and age interpretations for lunar rocks, impact melts, and recovered meteorites. It is therefore important to explore different thermally sensitive radiometric systems to unravel the timing and extent of the long term impact flux. Low-temperature thermochronology of lunar samples has the potential to provide more complementary geochronological datasets and further test dynamical models related to the evolution of the inner solar system (e.g., [1]). (U-Th)/He dating is based on the production of 4He atoms by radioactive alpha decay of U and Th (and to a lesser extent, Sm) in a crystal and the thermally activated volumetric diffusion of those 4He nuclides. At high temperatures, the crystal is an open system from which 4He can escape; at lower temperatures, 4He may be retained. This retention temperature depends on factors such as crystal structure and volume fraction of radiation damage in the crystal (e.g., [2, 3]), but is significantly lower for phosphate minerals compared to the diffusion of the radiogenic daughter products in other widely used chronometric systems (e.g., ~75°C in terrestrial apatite (U-Th)/He vs. ~500°C in apatite U-Th-Pb vs. ~900°C in zircon U-Th-Pb chronometry). Phosphate (U-Th)/He dating has been used to decipher peak temperatures and cooling rates related to terrestrial impact events (e.g., [4]). Pairing a low-temperature thermochronometer with higher-temperature approaches (i.e., a combined 207Pb-206Pb and (U-Th)/He approach), can therefore resolve multiple impact ages within a given sample or even grain. However, despite its potential, phosphate (U-Th)/He dating has not been reported on any lunar samples. Here we present the first lunar phosphate (U-Th)/He thermochronology on an Apollo 14 impact melt-breccia.

C A Diaz↗

Ionization induced damage in crystalline silicon

Close examination of the interaction of the energetic knock-on atoms with the local lattice environment reveals a damage mechanism which does satisfy the experimental data on proton irradiation of silicon. A proton-atom interaction with high energy transfer is considered where the proton path is delineated by a trail of ionization, and the silicon ion path is characterized by much heavier ionization terminating in a dense displacement cluster. At collision, many of the silicon electrons are stripped off, and the resulting energetic ion subsequently loses energy rapidly by Coulomb interaction with bound electrons. The rate of energy loss depends on the charge state and velocity of the knock-on ion. For ion energies in excess of 1 MeV, the intensity of ionization is sufficient to permit lattice atoms, stripped of their binding electrons, to reorient randomly before having an opportunity to recombine with electrons and re-establish the lattice. The path of a knock-on ion thus becomes a thin cylinder of amorphous material within the crystal. Amorphous silicon has a Fermi level closer to mid-band than does single crystal silicon, and a strong field therefore, results around this damaged region. The field produces a large depletion region, representing a very large capture cross section for minority carriers.

Meulenberg, A., Jr.↗

SAMS Acceleration Measurements on Mir from November 1995 to March 1996

The NASA Microgravity Science and Applications Division (MSAD) sponsors science experiments on a variety of microgravity carriers, including Orbiter missions and Russia's Mir space station. The MSAD sponsors the Space Acceleration Measurement System (SAMS) at the NASA Lewis Research Center (LERC) to support these science experiments by providing acceleration measurements to characterize the microgravity environment to which the experiments were exposed. The LeRC Principal Investigator Microgravity Services (PIMS) project supports principal investigations of microgravity science experiments as they evaluate the effects of varying acceleration levels on their experiments. In 1994, a SAMS unit was installed on the Mir space station. In a manner similar to Orbiter mission support, the SAMS unit supports science experiments from the U.S. and Russia by measuring the microgravity environment during experiment operations. Previous reports have summarized the SAMS data acquired during the period from September 1994 to November 1995. During the time period from November 1995 to March 1996, the primary SAMS-supported experiment was a Protein Crystal Growth (PCG) experiment. SAMS data were obtained during the PCG operations on Mir in accordance with the requirements specified by the PCG Principal Investigator. Also included in this data are mission events of interest, such as the undocking of STS-74 from Mir (November 1995) and the docking of Atlantis (STS-76) to Mir in March 1996. This report presents an overview of the SAMS data recorded in the interval from November 1995 to March 1996.

DeLombard, Richard↗

Vibration Isolation Technology (VIT) ATD Project

A fundamental advantage for performing material processing and fluid physics experiments in an orbital environment is the reduction in gravity driven phenomena. However, experience with manned spacecraft such as the Space Transportation System (STS) has demonstrated a dynamic acceleration environment far from being characterized as a 'microgravity' platform. Vibrations and transient disturbances from crew motions, thruster firings, rotating machinery etc. can have detrimental effects on many proposed microgravity science experiments. These same disturbances are also to be expected on the future space station. The Microgravity Science and Applications Division (MSAD) of the Office of Life and Microgravity Sciences and Applications (OLMSA), NASA Headquarters recognized the need for addressing this fundamental issue. As a result an Advanced Technology Development (ATD) project was initiated in the area of Vibration Isolation Technology (VIT) to develop methodologies for meeting future microgravity science needs. The objective of the Vibration Isolation Technology ATD project was to provide technology for the isolation of microgravity science experiments by developing methods to maintain a predictable, well defined, well characterized, and reproducible low-gravity environment, consistent with the needs of the microgravity science community. Included implicitly in this objective was the goal of advising the science community and hardware developers of the fundamental need to address the importance of maintaining, and how to maintain, a microgravity environment. This document will summarize the accomplishments of the VIT ATD which is now completed. There were three specific thrusts involved in the ATD effort. An analytical effort was performed at the Marshall Space Flight Center to define the sensitivity of selected experiments to residual and dynamic accelerations. This effort was redirected about half way through the ATD focusing specifically on the sensitivity of protein crystals to a realistic orbital environment. The other two thrusts of the ATD were performed at the Lewis Research Center. The first was to develop technology in the area of reactionless mechanisms and robotics to support the eventual development of robotics for servicing microgravity science experiments. This activity was completed in 1990. The second was to develop vibration isolation and damping technology providing protection for sensitive science experiments. In conjunction with the this activity, two workshops were held. The results of these were summarized and are included in this report.

Lubomski, Joseph F.↗

Li, B - Behavior in Lunar Basalts During Shock and Thermal Metamorphism: Implications for H2O in Martian Magmas

Introduction: The water-content of Martian magmas is a topic of debate among researchers. Some Martian basalts are characterized with melt inclusions of biotite, apatite and amphibole; phases typically associated with hydration reactions on Earth [1-3]. However, the H-content of melt inclusions from these basalts is low, and bulk-rock H2O-contents range from a meager 0.013 to 0.035 wt. % in Shergotty [4]. Nonetheless, researchers note that low present-day water contents do not preclude a once hydrous past [5]. Since light lithophile elements (LLE), such as Li and B, partition into aqueous fluids at T > 350 C, workers proposed that Li-B depletions in pyroxene rims of Nakhlite and Shergottite basalts reflect the loss of several weight percent water from Martian magmas during crystallization [6]. Since similar depletions were observed in pyroxene rims from completely dry lunar basalts, it is likely that alternative mechanisms also contribute to the distribution of elements such as Li and B [7]. Given that many Martian basalts have experienced considerable shock pressures (15-45 GPa), it is possible that shock and subsequent thermal metamorphism may have influenced the volatile element records of these basalts [8]. In order to better understand the distribution of Li and B, we are studying the effects of crystal chemistry, shock pressure, and thermal metamorphism in pyroxenes from lunar basalts. Below, we discuss results from experimentally shocked and thermally metamorphosed Apollo 11, 10017 (A-11) and Apollo 17, 75035 (A-17) basalts.

Chaklader, Johny↗

New Martian Meteorite Is One of the Most Oxidized Found to Date

As of 2013, about 60 meteorites from the planet Mars have been found and are being studied. Each time a new Martian meteorite is found, a wealth of new information comes forward about the red planet. The most abundant type of Martian meteorite is a shergottite; its lithologies are broadly similar to those of Earth basalts and gabbros; i.e., crustal igneous rocks. The entire suite of shergottites is characterized by a range of trace element, isotopic ratio, and oxygen fugacity values that mainly reflect compositional variations of the Martian mantle from which these magmas came. A newly found shergottite, NWA 5298, was the focus of a study performed by scientists within the Astromaterials Research and Exploration Science (ARES) Directorate at the Johnson Space Center (JSC) in 2012. This sample was found in Morocco in 2008. Major element analyses were performed in the electron microprobe (EMP) laboratory of ARES at JSC, while the trace elements were measured at the University of Houston by laser inductively coupled plasma mass spectrometry (ICPMS). A detailed analysis of this stone revealed that this meteorite is a crystallized magma that comes from the enriched end of the shergottite spectrum; i.e., trace element enriched and oxidized. Its oxidation comes in part from its mantle source and from oxidation during the magma ascent. It represents a pristine magma that did not mix with any other magma or see crystal accumulation or crustal contamination on its way up to the Martian surface. NWA 5298 is therefore a direct, albeit evolved, melt from the Martian mantle and, for its lithology (basaltic shergottite), it represents the oxidized end of the shergottite suite. It is thus a unique sample that has provided an end-member composition for Martian magmas.

Hui, Hejiu↗

Time development of a perturbed-spherical nucleus in a pure supercooled liquid. I - Power-law growth of morphological instabilities. II - Nonlinear development

The linear growth stage of the morphological instabilities developing at the liquid-solid interface during crystal growth from an axisymmetric spherical nucleus is analyzed. The corresponding growth rate parameters are calculated numerically, and it is shown that morphological instabilities for free growth evolve according to a power law in agreement with WKB results and contrary to an exponential law found in a quasi-stationary approximation. The time evolution of an arbitrary perturbed liquid-solid interface from a linear into the nonlinear stage is studied. The initial perturbations include the eigenfunctions for the linear problem, localized perturbations of the grain-boundary type, and a stochastic noise. It is shown that the perturbations grow and spread in a wavelike manner. The formation of a predendritic growth stage is characterized by establishment of constant values of tip radius and velocity.

Pines, V.↗

Investigation of Advanced Processed Single-Crystal Turbine Blade Alloys

This investigation studied the influence of thermal processing and microstructure on the mechanical properties of the single-crystal, nickel-based superalloys PWA 1482 and PWA 1484. The objective of the program was to develop an improved single-crystal turbine blade alloy that is specifically tailored for use in hydrogen fueled rocket engine turbopumps. High-gradient casting, hot isostatic pressing (HIP), and alternate heat treatment (HT) processing parameters were developed to produce pore-free, eutectic-free microstructures with different (gamma)' precipitate morphologies. Test materials were cast in high thermal gradient solidification (greater than 30 C/cm (137 F/in.)) casting furnaces for reduced dendrite arm spacing, improved chemical homogeneity, and reduced interdendritic pore size. The HIP processing was conducted in 40 cm (15.7 in.) diameter production furnaces using a set of parameters selected from a trial matrix study. Metallography was conducted on test samples taken from each respective trial run to characterize the as-HIP microstructure. Post-HIP alternate HT processes were developed for each of the two alloys. The goal of the alternate HT processing was to fully solution the eutectic gamma/(gamma)' phase islands and to develop a series of modified (gamma)' morphologies for subsequent characterization testing. This was accomplished by slow cooling through the (gamma)' solvus at controlled rates to precipitate volume fractions of large (gamma)'. Post-solution alternate HT parameters were established for each alloy providing additional volume fractions of finer precipitates. Screening tests included tensile, high-cycle fatigue (HCF), smooth and notched low-cycle fatigue (LCF), creep, and fatigue crack growth evaluations performed in air and high pressure (34.5 MPa (5 ksi)) hydrogen at room and elevated temperature. Under the most severe embrittling conditions (HCF and smooth and notched LCF in 34.5 MPa (5 ksi) hydrogen at 20 C (68 F), screening test results showed increases in fatigue life typically on the order of 1OX, when compared to the current Space Shuttle Main Engine (SSME) Alternate Turbopump (AT) blade alloy (PWA 1480).

Peters, B. J.↗

Isotopes of H, N, and O in H Chondrite Xenoliths

Brecciated H chrondites host a variety of xenoliths, including unshocked, phyllosilate-rich carbonaceous chondrites (CCs) [1-2]. The brecciated H chondrite Zag (H3-6) is one of two chondrites to host macroscopic (1 - 5mm), xenolithic crystals of halite (NaCl) with aqueous fluid inclusions and organics [3-4]. A ~1cm CC xenolith in Zag (Zag clast) also encloses halite in its matrix, linking the halite and the xenolith to the same parent object. The Zag clast has mineralogy similar to CI chondrites, but it has a unique bulk oxygen isotopic composition among all meteorites (Δ17O = 1.49 ± 0.04 ‰, 𝛿18O = 22.38 ± 0.17 ‰) and is therefore derived from a uniquely sampled parent object [5-6]. Organics have high bulk 𝛿D and 𝛿15N values with isotopic "hotspots" similar to organics in CR chondrites and Bells (C2-ung.) [6-7]. Bulk 𝛿15N is also similar to CRs and Bells [7]. We provide further isotopic characterization of the Zag clast to constrain the formation temperature and origin of its primary and secondary components.

Frank, D.↗

Evolution of Dendritic Extended 3D Patterns during Directional Solidification: Microgravity Experiments in DECLIC-DSI onboard ISS and Phase-field Modeling

To characterize the dynamical formation of three-dimensional (3D) arrays of dendrites under diffusive growth conditions, in situ monitoring of a series of experiments on a transparent succinonitrile – 0.46 wt% camphor model alloy was carried out under low gravity in the DECLIC Directional Solidification Insert onboard the International Space Station. These experiments offer continuous interface observation and enable the construction of space-time evolution maps of dendrite location and primary spacing during directional solidification. We present the evolution of dendritic extended 3D patterns for a large range of parameters displaying different levels of side branching in both experiments and phase-field simulations. The combined and separate effects of macroscopic interface curvature and crystal mis-orientation are evidenced and detailed. In addition, the aligned dendritic array caused by the invasion of dendrites formed at the edge of the crucible border is investigated.

Kaihua Ji↗

Characterization of physiochemical properties of polymeric and electrochemical materials for aerospace flight

Nickel-cadmium rechargeable batteries are a vital and reliable energy storage source for aerospace applications. As the demand for longer life and more reliable space batteries increases, the understanding and solving of cell aging factors and mechanisms become essential. Over the years, many cell designs and manufacturing process changes have been developed and implemented. Cells fabricated with various design features were life cycled in a simulated low-Earth orbit regime. Following the test program, a comprehensive electrochemical analysis of cell components was undertaken to study cell degradation mechanisms. Discharge voltage degradation or voltage plateau has been observed during orbit cycling, but, its cause and explanation have been the subject of much discussion. A Hg/HgO reference electrode was used to monitor the reference versus each electrode potential during the discharge of a cycled cell. The results indicate that the negative electrode was responsible for the voltage plateau. Cell analysis revealed large crystals of cadmium hydroxide on the surface of the negative electrode and throughout the separator.

Rock, M.↗

Ablative Rocket Deflector Testing and Computational Modeling

A deflector risk mitigation program was recently conducted at the NASA Stennis Space Center. The primary objective was to develop a database that characterizes the behavior of industry-grade refractory materials subjected to rocket plume impingement conditions commonly experienced on static test stands. The program consisted of short and long duration engine tests where the supersonic exhaust flow from the engine impinged on an ablative panel. Quasi time-dependent erosion depths and patterns generated by the plume impingement were recorded for a variety of different ablative materials. The erosion behavior was found to be highly dependent on the material s composition and corresponding thermal properties. For example, in the case of the HP CAST 93Z ablative material, the erosion rate actually decreased under continued thermal heating conditions due to the formation of a low thermal conductivity "crystallization" layer. The "crystallization" layer produced near the surface of the material provided an effective insulation from the hot rocket exhaust plume. To gain further insight into the complex interaction of the plume with the ablative deflector, computational fluid dynamic modeling was performed in parallel to the ablative panel testing. The results from the current study demonstrated that locally high heating occurred due to shock reflections. These localized regions of shock-induced heat flux resulted in non-uniform erosion of the ablative panels. In turn, it was observed that the non-uniform erosion exacerbated the localized shock heating causing eventual plume separation and reversed flow for long duration tests under certain conditions. Overall, the flow simulations compared very well with the available experimental data obtained during this project.

Allgood, Daniel C.↗