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NASA NTRS1999

Friction and Wear Properties of Selected Solid Lubricating Films

To evaluate commercially developed solid film lubricants for aerospace bearing applications, we investigated the friction and wear behavior of bonded molybdenum disulfide (MoS2), magnetron-sputtered MoS2 and ion-plated silver films in sliding contact with 6-mm-diameter American Iron and Steel Institute (AISI) 440 C stainless steel balls. Unidirectional sliding friction experiments were conducted with a load of 5.9 N (600 g), a mean Herizian contact pressure of 0.79 GPa maximum 1.19 GPa), and a sliding velocity of 0.2 m/s at room temperature in three environments: ultrahigh vacuum (7x10 (exp -7Pa)), humid air (approx. 20 percent humidity), and dry nitrogen (less than 1 percent humidity). The resultant films were characterized by scanning electron microscopy, energy-dispersive x-ray spectroscopy, and surface profilometry. Marked differences in friction and wear resulted front the environmental conditions and the film materials. The main criteria for judging the performance were coefficient of friction and wear rate, which had to be less than 0.3 and on the order of 10 (exp -6mm exp 3/Nm or less), respectively. The bonded MoS2 and magnetron-sputtered MoS2 films met the criteria in all three environments. Also, the wear rates of the counterpart AISI 440 C stainless steel balls met that criterion in all three environments. The ion-plated silver films met the criteria only in ultrahigh vacuum. In ultrahigh vacuum the bonded MoS2 films were superior. In humid air the bonded MoS2 films had higher coefficient of friction and shorter wear life than did the magnetron-sputtered MoS2 films. The ion-plated silver films had a high coefficient of friction in humid air but relatively low coefficients of friction in the nonoxidative environments. Adhesion and plastic deformation played important roles in all three environments. All sliding involved adhesive transfer of materials.

Miyoshi, Kazuhisa↗

NASA NTRS1990

Nature and origin of interstellar diamond from the Allende CV3 meteorite

Data and experimental evidence which support the contention that the C delta diamonds may result from grain-grain collisions in supernova shocks in the interstellar medium are presented. Fragments of the Allende CV3 chondrite were acid-treated. A whitish powder was obtained. For the Analytical Electron Microscopy (AEM) a small drop of ethanol suspension was transferred onto holey carbon support films on 3 mm EM grids. The AEM was performed on transmission-thin fragments of the material which overlay holes in the film, to eliminate interference from the substrate. Electron Spectroscopy for Chemical Analysis (ESCA) was performed on a large aliquot of C. Diamond was identified by selected area electron diffraction. Scanning Transmission Electron Microscope / Energy Dispersive X-ray (STEM-EDS) microanalyses of the C delta diamond, using a light-element detector, show that oxygen and possibly nitrogen are the only impurities consistently present. ESCA spectra from bulk C delta material confirm the presence of N at a level of 0.35 percent or less. Under UV irradiation a yellow-red fluorescence is observed, consistent with that of natural diamonds containing substitutional N. Electron Energy Loss Spectra (EELS) were recorded at 2 eV resolution from the C delta diamond, high pressure synthetic diamond, a diamond film produced in a low pressure plasma by chemical vapor deposition (CVD) on a heated silicon substrate (Roy, 1987), graphite, and amorphous arc sputtered carbon. Comparison of the carbon K edge shape and fine structure shows the Allende C delta phase to be largely diamond, but with a significant pre-edge absorption feature indicative of transitions of C 1s electrons into pi asterisk orbitals which are absent in the purely sp(3)-bonded diamond but present in graphite and amorphous carbon.

Blake, David↗

NASA NTRS1998

Tribometer for Lubrication Studies in Vacuum

The NASA Lewis Research Center has developed a new way to evaluate the liquid lubricants used in ball bearings in space mechanisms. For this evaluation, a liquid lubricant is exercised in the rolling contact vacuum tribometer shown in the photo. This tribometer, which is essentially a thrust bearing with three balls and flat races, has contact stresses similar to those in a typical preloaded, angular contact ball bearing. The rotating top plate drives the balls in an outward-winding spiral orbit instead of a circular path. Upon contact with the "guide plate," the balls are forced back to their initial smaller orbit radius; they then repeat this spiral orbit thousands of times. The orbit rate of the balls is low enough, 2 to 5 rpm, to allow the system to operate in the boundary lubrication regime that is most stressful to the liquid lubricant. This system can determine the friction coefficient, lubricant lifetime, and species evolved from the liquid lubricant by tribodegradation. The lifetime of the lubricant charge is only few micrograms, which is "used up" by degradation during rolling. The friction increases when the lubricant is exhausted. The species evolved by the degrading lubricant are determined by a quadrupole residual gas analyzer that directly views the rotating elements. The flat races (plates) and 0.5-in.-diameter balls are of a configuration and size that permit easy post-test examination by optical and electron microscopy and the full suite of modern surface and thin-film chemical analytical techniques, including infrared and Raman microspectroscopy and x-ray photoelectron spectroscopy. In addition, the simple sphere-on-a-flat-plate geometry allows an easy analysis of the contact stresses at all parts of the ball orbit and an understanding of the frictional energy losses to the lubricant. The analysis showed that when the ball contacts the guide plate, gross sliding occurs between the ball and rotating upper plate as the ball forced back to a smaller orbit radius. The friction force due to gross sliding is sensed by the piezoelectric force transducer behind the guide plate and furnishes the coefficient of friction for the system. This tribometer has been used to determine the relative lifetimes of Fomblin Z-25, a lubricant often used in space mechanisms, as a function of the material of the plates against which it was run. The balls were 440C steel in all cases; the plate materials were aluminum, chromium (Cr), 440C steel (17 wt % Cr), and 4150 steel (1 wt % Cr). As shown in the bar graph, the lifetime is greatest for the plate material with least chromium, thus implicating chromium as a tribochemically active element attacking Fomblin Z-25.

Pepper, Stephen V.↗

NASA NTRSDate not supplied

Contamination, Transportation or Transmutation in LENR Material Analyses

LENR experiments using various loading and triggering mechanisms rely on a variety of elemental and isotopic assays to determine LENR effects. These assays include optical microscopy, Scanning Electron Microscopy with Energy Dispersive X-Ray Analysis (SEM/EDX), X-Ray Photoelectron Spectroscopy (XPS) and Transmission Electron Microscopy (TEM). All of these methods observe the surface of a material. By dissolving or vaporizing the sample, Inductively Coupled Plasma Optical Element Spectroscopy (ICP-OES) can determine elemental composition (ppb) or with mass spectroscopy, isotopes (ICP/MS). One can use a focused ion beam (FIB) to cut open a sample and observe the “cut” with either SEM/EDX, or Time-of-Flight Secondary Ion Mass Spectroscopy (TOF-SIMS). High Purity Gamma Ray Spectroscopy (HPGe) and alpha/ beta Liquid Scintillator spectroscopy can be used. We’ve employed these assay methods in our NASA GRC research under both the Advanced Energy Conversion and Lattice Confinement Fusion Projects. However, there are limitations associated with each of these methods ranging from handling contamination, instrumental limitations including sensitivity and field of view, and sample preparation.

Low Energy Nuclear Reactions↗

NASA NTRSDate not supplied

The MOCHII ISS National Laboratory: The First Spacecraft Based Scanning Electron Microscope

Introduction: Scanning electron microscopy (SEM) in concert with element identification by energy dispersive Xray (EDX) spectroscopy has become an indispensable tool in the analyses of extraterrestrial materials. Nevertheless, to-date, SEM-EDX instrumentation has remained purely in the purview of terrestrial laboratories due to their size, complexity, and operational requirements. However, in January 2022 a miniaturized SEM-EDX called MOCHII became the first successful space-based instrument of its kind, following its deployment onboard the International Space Station (ISS). It represents the culmination of nearly 40 years of technological development. We have performed an on-orbit study with MOCHII with the goal of evaluating its potential as the progenitor of a new generation of spacecraftbased instruments for use in future manned and robotic planetary exploration missions. Out goal has been to validate the on-orbit investigation of samples relevant to astromaterials and astrobiology. We have performed in-situ analyses on standards and a freshly fractured fragment of the Martian meteorite Allan Hills 84001 which was first analyzed, prior to launch, using an engineering MOCHII ground unit located at Johnson Space Center in Houston. Results of both imaging and compositional analyses substantiates the utility of remote SEM-EDX analyses in low Earth orbit (LEO).

Miniature Scanning Electron Microscope↗

NASA NTRS1992

Viscosity determinations of some frictionally generated silicate melts: Implications for slip zone rheology during impact-induced faulting

Analytical scanning electron microscopy, using combined energy dispersive and wavelength dispersive spectrometry, was used to determine the major-element compositions of some natural and artificial glasses and their crystalline equivalents derived by the frictional melting of acid to intermediate protoliths. The major-element compositions are used to calculate the viscosities of their melt precursors using the model of Shaw at temperatures of 800-1400 C, with Fe(2+)/Fe(tot) = 0.5 and for 1-3 wt percent H2O. These results are then modified to account for suspension effects in order to determine viscosities. The results have implications for the generation of pseudotachylitic breccias as seen in the basement lithologies of the Sudbury and Vredefort structures and possibly certain dimict lunar breccias. Many of these breccias show similarities with the more commonly developed pseudotachylite fault and injection veins seen in endogenic fault zones that typically occur in thicknesses of a few centimeters or less. The main difference is one of scale: Impact-induced pseudotachylite breccias can attain several meters in thickness. This would suggest that they were generated under exceptionally high slip rates and hence high strain rates and that the friction melts generated possessed extremely low viscosities.

Spray, John G.↗

NASA NTRS1987

Soft x ray window encapsulant for HgI2 detectors

HgI2 is an excellent semiconductor material for a low energy, room temperature x-ray spectrometer. The high values of the atomic numbers for its constituent elements gives high x-ray and gamma ray stopping power. The band gap of HgI2 is significantly higher than other commonly used semiconductors. Owing to the large value band gap, the leakage current for HgI2 devices is smaller, thus allowing low noise performance. Devices fabricated from HgI2 crystals have demonstrated energy resolution sufficient to distinguish the x-ray emission from the neighboring elements on the periodic table. Also the power requirements of HgI2 are very low. These characteristics make a HgI2 spectrometer an ideal component in a satellite based detection system. Unfortunately, HgI2 crystals tend to deteriorate with time, even if protected by standard semiconductor encapsulants. This degradation ruins the performance of the device in terms of its energy resolution and pulse amplitude. The degrading mechanism is believed to be material loss occurring from below the electrodes, due to high vapor pressure of HgI2 at room temperature. To address this major obstacle to rapid expansion of HgI2 technology, a research program aimed at improving device stability by encapsulation with inert polymeric materials was carried out. The program focused specifically on optimizing the encapsulant materials and their deposition techniques. The principal objectives for this program were device encapsulation, device testing, and accelerated testing to ensure very long term stability of these high resolution sensors. A variety of encapsulants were investigated with the selection criteria based on their chemical diffusion barrier properties, mechanical stability, reactivity, and morphology of encapsulant films. The investigation covered different classes of encapsulants including solvent based encapsulants, vapor deposited encapsulants, and plasma polymerized encapsulants. A variety of characterization techniques were employed to examine their effectiveness in stabilizing HgI2 devices; these included permeability evaluation, vacuum and heat testing, scanning electron microscopy (SEM) as well as studying the detector performance of coated detectors. The plasma polymerized films appear to have entirely solved the HgI2 degradation problem. Another achievement of this program was the development of an accelerated testing technique which correlates extremely well with long term tesing.

Entine, G.↗

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↗

NASA NTRSDate not supplied

Determining Surface Exposure Ages of Regolith Grains in Lunar Core Sample 73002 By Investigating Solar Particle Irradiation Damage

Space weathering causes the surface soils of airless bodies like the Moon to be micro-structurally and chemically altered by exposure to micrometeoroid bombardment and solar wind irradiation. These alterations accumulate in surface grains with continued residence in the uppermost millimeters of regolith. Low energy solar wind ions (largely H+ and He+) produce a layer of radiation damage as they become implanted in grain surfaces. Also present are solar energetic particle (SEP) tracks, which are nanoscale lineations within grain interiors formed by heavy, high-energy ions (mainly Fe group nuclei) penetrating up to millimeters below the surface. Recent work has determined that the width of solar wind-damaged rims on anorthite and olivine, and their respective SEP track densities are correlated with each other and with grain surface exposure age. Core sample 73002, recently released under the Apollo Next Generation Sample Analysis (ANGSA) Program, has provided an opportunity to study material collected from the light mantle formation in the Taurus-Littrow Valley during Apollo 17. The light mantle is thought to have been deposited vial and slide originating from the neighboring South Massif. Spectral analysis of bulk core soils found a plagioclase rich composition, confirming a highlands origin of the formation. Spectral profiles and ferromagnetic resonance (FMR) measurements of bulk soils sampled at cm-intervals from 73002 indicate that regolith up to~9.5 cm in depth have maturity indices consistent with longer durations of surface processing than samples deeper in the core. Thus, this upper ~9 cm layer likely represents the maximum extent of an in-situ reworking zone which may have persisted over 5 to 17million years. Here we present an analysis of grain exposure ages within the in-situ reworking zone of 73002derived from SEP track density measurements via transmission electron microscopy.

J A McFadden↗

NASA NTRS2026

Microstructural Evolution and Mechanical Properties of LP-DED NASA HR-1 – A Hydrogen Resistant AM Superalloy for Space Propulsion Applications

The National Aeronautics and Space Administration (NASA) has actively pursued metal additive manufacturing (AM) technologies for spaceflight applications since the late 2000s. AM offers transformative advantages in cost, schedule, part consolidation, and design flexibility. Among the various AM techniques, laser powder directed energy deposition (LP-DED) is particularly well suited for fabricating complex geometries with fine feature resolution. In propulsion systems that utilize high-pressure gaseous hydrogen—such as liquid hydrogen rocket engines—hydrogen environment embrittlement (HEE) presents a serious threat to material performance 1,2 . Mechanical property degradation under these conditions can compromise component reliability, especially under cyclic loading. To address this challenge, NASA developed NASA HR-1 (Hydrogen Resistant-1) as a solution for liquid rocket engine components operating in hydrogen-rich environments, using the LP-DED technique 3-9 . A key component in a liquid rocket engine is the exhaust nozzle, which is typically regeneratively cooled (regen) due to the high heat flux. NASA HR-1 was specifically developed for regen nozzle applications using hydrogen as a propellant, providing resistance to HEE, a critical issue for many materials. The AM version of NASA HR-1 was also formulated to achieve high ultimate tensile strength, along with high yield strength and ductility in this environment 5,6 . Low-cycle fatigue (LCF) is another important consideration in nozzle design, as components are expected to endure multiple starts and missions. Additionally, the LP-DED version of the alloy exhibits improved thermal conductivity compared to its wrought counterpart, which benefits nozzle cooling. Overall, NASA HR-1 offers an excellent balance of high strength, HEE resistance, LCF performance, thermal conductivity, and ductility to meet the demanding requirements of channel-cooled nozzles and other components used with hydrogen and other propellants. The LP-DED–processed NASA HR-1 requires several post-processing heat treatment steps to achieve the material properties desirable for its intended application 6 . These steps include stress relief, homogenization, solution annealing, and aging for precipitation hardening. The stress relief treatment mitigates residual stresses accumulated during the LP-DED process and minimizes the potential for distortion. Homogenization, a common step for AM materials, reduces elemental segregation and promotes recrystallization to develop a more equiaxed grain structure. The subsequent solution annealing treatment heats the part to a solid solution temperature to dissolve the undesirable η-phase that forms during cooling from homogenization, followed by rapid cooling to retain an η-phase–free microstructure. Finally, aging promotes precipitation of the strengthening γ′ phase in the alloy. The integration of compositional design and optimized thermal processing enables high-quality LP-DED NASA HR-1 components with excellent microstructural and mechanical stability. Improved chemical and microstructure homogeneity enhances ductility and fatigue resistance—both critical for safe and reliable operation in high-pressure hydrogen environments. NASA has successfully fabricated and hot-fire tested multiple subscale and full-scale channel wall nozzles using LP-DED NASA HR-1 5,6, 9-14 . These efforts included process refinements to support thin-wall construction and various channel geometries. Throughout development, several key observations emerged. After homogenization, the as-built columnar grain structure transforms into a fully equiaxed microstructure. However, subsequent treatments—such as solution annealing and aging—result in changes that are more difficult to track. The grain structure remains largely unchanged, and the γ′ precipitates, typically 5–10 nm in diameter, are beyond the resolution of scanning electron microscopy (SEM). While transmission electron microscopy (TEM) can resolve these fine precipitates, TEM sample preparation is time-consuming and difficult for LP-DED material. As an alternative, differential scanning calorimetry (DSC) offers a useful, qualitative approach to monitor precipitate evolution throughout different stages of heat treatment. The overall goal is to improve the understanding of how heat treatment affects the microstructure and mechanical performance of LP-DED NASA HR-1. This paper presents heat treatment design considerations, microstructural characterization, mechanical testing – including tensile and LCF testing in both air and hydrogen environments.

Superalloy↗

NASA NTRS1995

Natural and orbital debris particles on LDEF's trailing and forward-facing surfaces

Approximately 1000 impact craters on the Chemistry of Meteoroid Experiment (CME) have been analyzed by means of Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Analysis (EDXA) to determine the compositional make-up of projectile residues. This report completes our systematic survey of gold and aluminum surfaces exposed at the trailing-edge (A03) and forward-facing (A11) LDEF sites, respectively. The major categories for the projectile residues were (1) natural, with diverse subgroups such as chondritic, monomineralic silicates, and sulfides, and (2) man made, that were classified into aluminum (metallic or oxide) and miscellaneous materials (such as stainless steel, paint flakes, etc). On CME gold collectors on LDEF's trailing edge approximately 11 percent of all craters greater than 100 micron in diameter were due to man-made debris, the majority (8.6 percent) caused by pure aluminum, approximately 31.4 percent were due to cosmic dust, while the remaining 58 percent were indeterminate via the analytical techniques utilized in this study. The aluminum surfaces located at the A11 forward-facing site did not permit analysis of aluminum impactors, but approximately 9.4 percent of all craters were demonstratably caused by miscellaneous debris materials and approximately 39.2 percent were the result of natural particles, leaving approximately 50 percent which were indeterminate. Model considerations and calculations are presented that focus on the crater-production rates for features greater than 100 micron in diameter, and on assigning the intermediate crater population to man-made or natural particles. An enhancement factor of 6 in the crater-production rate of natural impactors for the 'forward-facing' versus the 'trailing-edge' CME collectors was found to best explain all observations (i.e., total crater number(s), as well as their computational characteristics). Enhancement factors of 10 and 4 are either too high or too low. It is also suggested that approximately 45 percent of all craters greater than 100 micron in diameter are caused by man-made impactors on the A11 surfaces. This makes the production rate for craters greater than 100 micron in diameter, resulting from orbital debris, a factor of 40 higher on the forward-facing sides as opposed to the trailing-edge direction.

Hoerz, Friedrich↗

NASA NTRS2023

Mineralogical, Elemental, and Tomographic Reconnaissance Investigation for CLPS (METRIC)

METRIC is a robotic science laboratory that can determine the mineralogy, elemental chemistry, micromorphology, and thermophysical properties of planetary regolith. The METRIC suite comprises METRIC XRD/F, an X-ray diffraction/X-ray fluorescence instrument that can determine the mineralogy and elemental chemistry of regolith samples; METRIC XCT, a micro X-ray computed tomography instrument that can be used to evaluate grain/crystallite sizes and textures; METRIC IRS, an imaging spectrometer mounted on a rover that can determine mineralogy and thermophysical properties at the landing site; and a pneumatic sample collection, processing, distribution system developed by Honeybee Robotics. The payload elements could be deployed on a static lander or a rover. Data returned from the METRIC payload would inform origin, formation, and evolution of rocky planetary bodies. METRIC XRD/F draws on heritage from the CheMin instrument on the Mars Science Laboratory (MSL) Curiosity rover [1], with a few important improvements. Like CheMin, METRIC XRD/F operates in transmission geometry and uses piezoelectric actuators on sample cells in a tuning fork geometry to induce convective grain motion of the regolith to create a randomly oriented powder. MSL CheMin uses an energy-sensitive CCD to collect XRD patterns and XRF spectra simultaneously from the same sample cell, resulting in qualitative XRF data. METRIC XRD/F uses two different sample cells, one optimized for XRD and one optimized for XRF, and a silicon drift detector to detect fluoresced X-rays. This improvement to the XRF capabilities provides quantitative geochemical data of major elements down to Z = 11 and allows for the detection of minor and trace elements that are critical for evaluating geologic evolution of the Moon (e.g., P and Th). Modest improvements to the XRD geometry and hardware allow for better angular resolution and the ability to distinguish between members of the pyroxene group. METRIC XCT uses the same geometry and much of the same hardware as METRIC XRD/F, where a CCD would capture images of a regolith sample in a 3 mm diameter sample tube that is rotated 360° in steps <1°. Image brightness can be used to infer compositional data, where brighter materials indicate a higher Z, much like scanning electron microscopy. Data from METRIC XCT complement those from METRIC XRD/F. Particle size, shape, and texture can provide petrologic and provenance information, whereas vesicle size and morphology in volcanic or impact melt lithologies can inform cooling rates. METRIC IRS is a hyperspectral thermal imager that can be mounted to a lander or rover to provide mineralogical data from the broader landing site and help determine whether the samples analyzed by METRIC XRD/F and XCT are representative. The METRIC IRS spectral range (8–14 μm) and resolution (10.8 cm-1) allow for quantitative mineralogy from modelling Reststrahlen bands of major rock-forming minerals (e.g., silicates, phosphates). Radiance cubes can be processed and modelled with an onboard high-performance computer to determine mineral abundances of plagioclase, high-Ca pyroxene, pigeonite, orthopyroxene, olivine, and glass. Regolith samples can be acquired, processed, and delivered to the X-ray instruments via multiple sample handling systems, but the pneumatic sampling systems developed by Honeybee Robotics [e.g., 2] are best suited for relatively low-cost missions that are being competed for the Moon (e.g., NASA’s Payloads and Research Investigations for the Surface of the Moon program). There are pneumatic sampling systems that collect surface material and other systems that pneumatically drill up to ~1 m below the surface, providing material that has not been space weathered and has not been affected by the lander’s exhaust. [1] Blake, D. F., Vaniman, D., Achilles, C., Anderson, R., Bish, D., et al. (2012). Space Sci. Rev. 170, 341-478. https://doi.org/10.1007/s11214-012-9905-1. [2] Zacny, K., Betts, B., Hedlund, M., Long, P., Gramlich, M., Tura, K., Chu, P., Jacob, A., Garcia, A. (2014). IEEE Aerospace Conference, 3-7 March 2014, Big Sky, MT, U.S.A.

X-ray diffraction↗

NASA NTRS2022

Atomic-Scale Structure and Non-Stoichiometry of Meteoritic Hibonite: A Transmission Electron Microscope Study

Hibonite (CaAl_12O_19) is a common refractory mineral in Ca-Al-rich inclusions (CAIs) in primitive meteorites. Transmission electron microscope (TEM) studies have identified enigmatic planar defects in different occurrences of hibonite in the Allende meteorite that give rise to strong streaking along c* in electron diffraction patterns. Atomic resolution high-angle annular dark-field (HAADF) imaging and energy-dispersive X-ray (EDX) analyses were used to determine the nature and origin of these planar features. HAADF images of hibonite grains reveal lamellar intergrowths of common 1.6 nm spacing, and less commonly 2.0 and 2.5 nm spacings, interspersed in stoichiometric hibonite showing 1.1 nm (002) spacing. Stoichiometric hibonite consists of alternating Ca-containing (“R”) and spinel-structured (“S”) blocks stacked in a sequence RS. In contrast, the 1.6 nm layers result from a doubled S block such that the stacking sequence is RSS, while in the widest defect observed, the stacking sequence is RSSSS. These intergrowths are epitaxial and have coherent, low-strain boundaries with the host hibonite Meteoritic hibonite shows common Ti and Mg substitution for Al in its structure. Atomic-resolution EDX maps of hibonite grains in the Allende CAI confirm the preferred site occupancy of Mg on tetragonal M3 sites in S blocks and of Ti on trigonal bipyramidal M2 and octahedral M4 sites in R blocks. Mg is highly concentrated, but Ti is absent in the planar defects where wider S blocks show Al-rich compositions compared to stoichiometric MgAl_2O_4 spinel. Therefore, Mg likely played the major role in the formation and metastability of planar defects in hibonite. Electron energy loss spectroscopy data from the Ti L_2,3 edge show the presence of mixed Ti oxidation states with ~ 15–20% of Ti as Ti^(3+) in hibonite, suggesting a direct substitution of Ti^(3+) ↔ Al^(3+) in hibonite. The remaining ~ 80–85% of Ti is present as Ti^(4+) and corresponding EDX analyses are consistent with the well-known coupled substitution 2Al^(3+) ↔ Ti^(4+) + Mg^(2+) being the major mechanism for Ti and Mg substitution in hibonite. The formation of planar defects in hibonite occurred during high-temperature nebular condensation or melting/crystallization processes. The occurrence of non-stoichiometric hibonite in the Allende CAI deviates from the mineral formation sequence predicted from equilibrium condensation models. Overall, our atomic resolution TEM observations signify non-equilibrium, kinetic-controlled crystal growth during the high-temperature formation of refractory solids in the early solar nebula.

hibonite↗

NASA NTRSDate not supplied

Microwave Structure Construction Capability Year One Accomplishments

The Microwave Structure Construction Capability (MSCC) element, part of the Moon to Mars Planetary Autonomous Construction Project (MMPACT) was initiated in 2020. MSCC is responsible for creating horizontal and vertical infrastructure on the moon using microwave energy. Microwave energy was selected since it is the only method to volumetrically heat the regolith. All other sintering/melting methods rely on thermal conduction through the very low conductivity surface, resulting in an inefficient process. Advances were achieved in materials characterization and understanding, microwave sintering in vacuum, and microwave design and analyses. Two dielectric property testing systems have been developed at Radiance Technologies and JPL. These will examine dielectric properties at cryogenic temperatures and over a broad frequency range. Permittivity and permeability testing at -60 ̊C in vacuum from 0.05 to 3 GHz has been generated at JPL. Additional modifications will be made to go to -190 ̊C (LN2). Radiance Technologies created a test system to measure dielectric properties at greater than 10 GHz and initiated work on developing a vacuum capable, portable test system to measure dielectric properties of Apollo regolith and simulants from 100 MHz to 18 GHz. These tests are to identify optimal heating frequencies and protocols. During microwave sintering at about 1100 ̊C, volatiles were creating difficulty in achieving a reasonably dense specimen. Due to processing in vacuum and the nature of the lunar regolith, some volatiles and porosity are expected. However, the Earth produced simulants have non-lunar materials in them that create volatiles that aren’t representative of lunar regolith. Therefore, a five month effort was conducted to establish a heat treat method to remove these non-lunar materials. Tests were conducted using TGA mass spectrometry, heating in vacuum and conducting mass spectrometry, dielectric and DTA, Raman, BET, particle size analysis, morphological analysis, carbon and sulfur chemical content determination and microscopy. The process has been scaled-up to 6 kg batch size and undergoing evaluation. A 36 kg batch size is the target for JSC-1A and other limited availability simulants. These calcining protocols will be standard for NASA and beyond. MSCC has also created scalable processes for fabricating synthetic lunar materials. Processes to fabricate Anorthite (plagioclase CaAl2Si2O8), Diopside (pyroxene CaMgSi₂O₆), and Enstatite (pyroxene Mg2Si2O6) have been generated. These materials will enable generation of microwave sintering models to bound various composition ranges anticipated on the Moon, therefore mitigating the need for a precise simulant with respect to location on the Moon. Successful microwave sintering in air using a horn applicator was demonstrated. All previous microwave vacuum sintering in the literature was at small scale and in a contained enclosure thus taking advantage of reflections. This is the first to use a lunar like microwave applicator to sinter ceramic in a bed as it would be done on the Moon. Small scale and inert sintering were conducted to assist in developing protocols with quicker turnaround times than larger scale testing. Testing has anchored thermal analysis predicting heat flow in vacuum during microwave sintering. Thermal conductivity testing was also initiated. Microwave coupling to the regolith has been modeled by multiple organizations and with different software packages. At least six horn designs and applicator configurations for both magnetron and solid state sources are being examined. Optimal simulant container designs for microwaves have also been generated. The power and electronics design for the solid state microwave system has been initiated. Concept designs for a lander based microwave sintering have been evaluated.

microwave↗