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

METRIC comprises a suite of two instruments in a Lunar lander that perform X-ray diffraction (XRD) for mineral structure, X-ray fluorescence (XRF) for elemental composition, and X-ray Micro Computed Tomography (XCT) for 3D internal micromorphology. The instruments are accompanied by optical-near IR cameras to provide local geologic context. The Honeybee Robotics PlanetVac pneumatic sampling and transfer system [1],positioned on a lander footpad, will deliver sieved regolith to the X-ray instruments for analysis. The instrument suite is intended for delivery to the lunar surface on a Commercial Lunar Payload Services (CLPS) lander. The METRICXRD/F instrument draws on heritage from the Mars Science Laboratory CheMin instrument [2] and improves upon the design in multiple ways [3]. Like CheMin, Rietveld refinement and full-pattern fitting of METRIC XRD data can identify minerals at a detection limit of ~1 wt.%, quantify their abundances when present at >3 wt.%, and determine mineral composition (e.g., Fo#in olivine) from lattice parameters for minerals present at >5 wt.%[4,5]. An optimized XRF geometry provides for improved detection and quantification of major, minor and trace elements. The METRIC XCT instrument is a miniaturized X-ray Computed Tomography scanner[6]. Lunar regolith is delivered to a 3 mm diameter, 10 mm long graphite tube inside the instrument. The tube is rotated through 360°in 0.9deg.incrementsand a divergent point source X-ray beam is directed through the material. A Charge Coupled Device (CCD)records attenuation images whose brightness and contrast area function of average atomic number and density. Quantitative data, including particle and void sizes, 3D particle shape parameters, modal volumes and pore geometry can be derived from the resulting 3D reconstructions(voxel resolution: 30 μm). Crystal morphologies derived from METRIC XCT data complement the bulk mineralogy determined by the METRIC XRD/F and provide a measure of grain size distribution for the different phases. Taken together, the METRIC instrument suite determines crystal structure, elemental composition and morphology, three principal characteristics of geological materials that are highly useful in determining the origin and subsequent processing of lunar regolith.

Moon↗

X-ray fluorescence and XANES spectroscopy revealed diverse potassium chemistries and colocalization with phosphorus in the ectomycorrhizal fungus Paxillus ammoniavirescens

Ectomycorrhizal (ECM) fungi play a major role in forest ecosystems and managed tree plantations. Particularly, they facilitate mineral weathering and nutrient transfer towards colonized roots. Among nutrients provided by these fungi, potassium (K) has been understudied compared to phosphorus (P) or nitrogen (N). The ECM fungus Paxillus ammoniavirescens is a generalist species that interacts with the root of many trees and can directly transfer K to them, including loblolly pine. However, the forms of K that ECM fungi can store is still unknown. Here, we used synchrotron potassium X-ray fluorescence (XRF) and K-edge X-ray Absorption Near Edge Structure (XANES) spectroscopy on P. ammoniavirescens growing in axenic conditions to investigate the K chemistries accumulating in the center and the edge of the mycelium. We observed that various K forms accumulated in different part of the mycelium, including K-nitrate (KNO 3 ), K-C-O compounds (such as K-tartrate K 2 (C 4 H 4 O 6 ) and K-oxalate (K 2 C 2 O 4 )), K-S and K-P compounds. Saprotrophic fungi have been shown to excrete carboxylic acids, which in turn play a role in soil mineral weathering. Our finding of several K counter-ions to carboxylic acids may suggest that, besides their direct transfer to colonized roots, K ions can also be involved in the production of compounds necessary for sourcing nutrients from their surrounding environment by ECM fungi. Additionally, this work reveals that XANES spectroscopy can be used to identify the various forms of K accumulating in biological systems.

Ectomycorrhizal symbiosis↗

Fluorescent Approaches to High Throughput Crystallography

X-ray crystallography remains the primary method for determining the structure of macromolecules. The first requirement is to have crystals, and obtaining them is often the rate-limiting step. The numbers of crystallization trials that are set up for any one protein for structural genomics, and the rate at which they are being set up, now overwhelm the ability for strictly human analysis of the results. Automated analysis methods are now being implemented with varying degrees of success, but these typically cannot reliably extract intermediate results. By covalently modifying a subpopulation, 51%, of a macromolecule solution 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. The covalently attached probe will concentrate in the crystal relative to the solution, and under fluorescent illumination the crystals show up as bright objects against a dark background. As crystalline packing is more dense than amorphous precipitate, the fluorescence intensity can be used as a guide in distinguishing different types of precipitated phases, even in the absence of obvious crystalline features, widening the available potential lead conditions in the absence of clear hits. Non-protein structures, such as salt crystals, will not incorporate the probe and will not show up under fluorescent illumination. Also, brightly fluorescent crystals are readily found against less fluorescent precipitated phases, which under white light illumination may serve to obscure the crystals. Automated image analysis to find crystals should be greatly facilitated, without having to first define crystallization drop boundaries and by having the protein or protein structures all that show up. 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. This presentation will focus on the methodology for fluorescent labeling, the crystallization results, and the effects of the trace labeling on the crystal quality.

Pusey, Marc L.↗

Fluorescent Approaches to High Throughput Crystallography

X-ray crystallography remains the primary method for determining the structure of macromolecules. The first requirement is to have crystals, and obtaining them is often the rate-limiting step. The numbers of crystallization trials that are set up for any one protein for structural genomics, and the rate at which they are being set up, now overwhelm the ability for strictly human analysis of the results. Automated analysis methods are now being implemented with varying degrees of success, but these typically can not reliably extract intermediate results. By covalently modifying a subpopulation, less than or = 1%, of a macromolecule solution 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. The covalently attached probe will concentrate in the crystal relative to the solution, and under fluorescent illumination the crystals show up as bright objects against a dark background. As crystalline packing is more dense than amorphous precipitate, the fluorescence intensity can be used as a guide in distinguishing different types of precipitated phases, even in the absence of obvious crystalline features, widening the available potential lead conditions in the absence of clear "hits." Non-protein structures, such as salt crystals, will not incorporate the probe and will not show up under fluorescent illumination. Also, brightly fluorescent crystals are readily found against less fluorescent precipitated phases, which under white light illumination may serve to obscure the crystals. Automated image analysis to find crystals should be greatly facilitated, without having to first define crystallization drop boundaries and by having the protein or protein structures all that show up. 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. This presentation will focus on the methodology for fluorescent labeling, the crystallization results, and the effects of the trace labeling on the crystal quality.

Pusey, Marc L.↗

Fluorescent Approaches to High Throughput Crystallography

X-ray crystallography remains the primary method for determining the structure of macromolecules. The first requirement is to have crystals, and obtaining them is often the rate-limiting step. The numbers of crystallization trials that are set up for any one protein for structural genomics, and the rate at which they are being set up, now overwhelm the ability for strictly human analysis of the results. Automated analysis methods are now being implemented with varying degrees of success, but these typically cannot reliably extract intermediate results. By covalently modifying a subpopulation, less than or = 1%, of a macromolecule solution 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 a macromolecules purification. The covalently attached probe will concentrate in the crystal relative to the solution, and under fluorescent illumination the crystals will show up as bright objects against a dark background. As crystalline packing is more dense than amorphous precipitate, the fluorescence intensity can be used as a guide in distinguishing different types of precipitated phases, even in the absence of obvious crystalline features, widening the available potential lead conditions in the absence of clear "bits." Non-protein structures, such as salt crystals, will not incorporate the probe and will not show up under fluorescent illumination. Also, brightly fluorescent crystals are readily found against less fluorescent precipitated phases, which under white light illumination may serve to obscure the crystals. Automated image analysis to find crystals should be greatly facilitated, without having to first define crystallization drop boundaries and by having the protein or protein structures all that show up. 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. This presentation will focus on the methodology for fluorescent labeling, the crystallization results, and the effects of the trace labeling on the crystal quality.

Minamitani, Elizabeth Forsythe↗

Micro-XRF for In Situ Geological Exploration of Other Planets

In situ analysis of rock chemistry is a fundamental tool for exploration of planets. To meet this need, a high-spatial-resolution micro x-ray fluorescence (Micro-XRF) instrument was developed that is capable of determining the elemental composition of rocks (elements Na U) with 100 microns spatial resolution, thus providing insight to the composition of features as small as sand grains and individual laminae. The resulting excitation beam is of sufficient intensity that high signal-to-noise punctual spectra are acquired in seconds to a few minutes using an Amptek Silicon Drift Detector (SDD). The instrument features a tightly focused x-ray tube and HVPS developed by Moxtek that provides up to 200 micro-A at 10 to 50 keV, with a custom polycapillary optic developed by XOS Inc. and integrated into a breadboard Micro-XRF (see figure). The total mass of the complete breadboard instrument is 2.76 kg, including mounting hardware, mounting plate, camera, laser, etc. A flight version of this instrument would require less than 5W nominal power and 1.5 kg mass. The instrument includes an Amptek SDD that draws 2.5 W and has a resolution of 135 to 155 eV FWHM at 5.9 keV. It weighs 180 g, including the preamplifier, digital pulse processor, multichannel analyzer, detector and preamp power supplies, and packaging. Rock samples are positioned relative to the instrument by a three-axis arm whose position is controlled by closed-loop translators (mimicking the robotic arm of a rover). The distance from the source to the detector is calculated from the position of a focused laser beam on the sample as imaged by the camera. The instrument enables quick scans of major elements in only 1 second, and rapid acquisition (30 s) of data with excellent signal-to-noise and energy resolution for trace element analysis

Wade, Lawrence A.↗

NASA Tech Briefs, September 2012

Topics covered include: Beat-to-Beat Blood Pressure Monitor; Measurement Techniques for Clock Jitter; Lightweight, Miniature Inertial Measurement System; Optical Density Analysis of X-Rays Utilizing Calibration Tooling to Estimate Thickness of Parts; Fuel Cell/Electrochemical Cell Voltage Monitor; Anomaly Detection Techniques with Real Test Data from a Spinning Turbine Engine-Like Rotor; Measuring Air Leaks into the Vacuum Space of Large Liquid Hydrogen Tanks; Antenna Calibration and Measurement Equipment; Glass Solder Approach for Robust, Low-Loss, Fiber-to-Waveguide Coupling; Lightweight Metal Matrix Composite Segmented for Manufacturing High-Precision Mirrors; Plasma Treatment to Remove Carbon from Indium UV Filters; Telerobotics Workstation (TRWS) for Deep Space Habitats; Single-Pole Double-Throw MMIC Switches for a Microwave Radiometer; On Shaft Data Acquisition System (OSDAS); ASIC Readout Circuit Architecture for Large Geiger Photodiode Arrays; Flexible Architecture for FPGAs in Embedded Systems; Polyurea-Based Aerogel Monoliths and Composites; Resin-Impregnated Carbon Ablator: A New Ablative Material for Hyperbolic Entry Speeds; Self-Cleaning Particulate Prefilter Media; Modular, Rapid Propellant Loading System/Cryogenic Testbed; Compact, Low-Force, Low-Noise Linear Actuator; Loop Heat Pipe with Thermal Control Valve as a Variable Thermal Link; Process for Measuring Over-Center Distances; Hands-Free Transcranial Color Doppler Probe; Improving Balance Function Using Low Levels of Electrical Stimulation of the Balance Organs; Developing Physiologic Models for Emergency Medical Procedures Under Microgravity; PMA-Linked Fluorescence for Rapid Detection of Viable Bacterial Endospores; Portable Intravenous Fluid Production Device for Ground Use; Adaptation of a Filter Assembly to Assess Microbial Bioburden of Pressurant Within a Propulsion System; Multiplexed Force and Deflection Sensing Shell Membranes for Robotic Manipulators; Whispering Gallery Mode Optomechanical Resonator; Vision-Aided Autonomous Landing and Ingress of Micro Aerial Vehicles; Self-Sealing Wet Chemistry Cell for Field Analysis; General MACOS Interface for Modeling and Analysis for Controlled Optical Systems; Mars Technology Rover with Arm-Mounted Percussive Coring Tool, Microimager, and Sample-Handling Encapsulation Containerization Subsystem; Fault-Tolerant, Real-Time, Multi-Core Computer System; Water Detection Based on Object Reflections; SATPLOT for Analysis of SECCHI Heliospheric Imager Data; Plug-in Plan Tool v3.0.3.1; Frequency Correction for MIRO Chirp Transformation Spectroscopy Spectrum; Nonlinear Estimation Approach to Real-Time Georegistration from Aerial Images; Optimal Force Control of Vibro-Impact Systems for Autonomous Drilling Applications; Low-Cost Telemetry System for Small/Micro Satellites; Operator Interface and Control Software for the Reconfigurable Surface System Tri-ATHLETE; and Algorithms for Determining Physical Responses of Structures Under Load.

Source record↗

Low- to Mid-Latitude X-Ray Emission from Jupiter

The Chandra X-ray Observatory (CXO) observed Jupiter during the period 2003 February 24-26 for approx.40 hours (4 Jupiter rotations), using both the spectroscopy array of the Advanced CCD Imaging Spectrometer (ACIS-S) and the imaging array of the High-Resolution Camera (HRC-I). Two ACIS-S exposures, each approx.8.5 hr long, were separated by an HRC-I exposure of approx.20 hr. The low- to mid-latitude non-auroral disk X-ray emission is much more spatially uniform than the auroral emission. However, the low- to mid-latitude X-ray count rate shows a small but statistically significant hour angle dependence, and is higher in regions of relatively low surface magnetic field strength, confirming ROSAT results. In addition, the spectrum from the low surface field region shows an enhancement in the energy band 1.14- 1.38 keV, perhaps partly due to line emission from that region. Correlation of surface magnetic field strength with count rate is not found for the 2000 December HRC-I data, at a time when solar activity was high. The low- to mid-latitude disk X-ray count rate observed by the HRC-I in the 2003 February observation is about 50% of that observed in 2000 December, roughly consistent with a decrease in the solar activity index (F10.7 cm flux) by a similar amount over the same time period. The low- to mid-latitude X-ray emission does not show any oscillations similar to the -45 minute oscillations sometimes seen from the northern auroral zone. The temporal variation in Jupiter's non-auroral X-ray emission exhibits similarities to variations in solar X-ray flux observed by GOES and TIMED/SEE. The two ACIS-S 0.3-2 keV low- to mid-latitude X-ray spectra are harder than the auroral spectrum, and are different from each other at energies above 0.7 keV, showing variability in Jupiter s non-auroral X-ray emission on a time scale of a day. The 0.3-2.0 keV X-ray power emitted at low- to mid-latitudes is 0.21 GW and 0.39 GW for the first and second ACIS-S exposures, respectively. We suggest that X-ray emission from Jupiter's disk may be largely generated by solar X-rays resonantly and fluorescently scattered in its upper atmosphere, especially at times of high incident solar X-ray flux. However, the correlation of higher count rate with low surface magnetic-field strength indicates the presence of some secondary component, possibly ion precipitation from radiation belts closer to the planet than elsewhere at low- to mid-latitudes.

Bhardwaj, Anil↗

Low- to Middle-Latitude X-Ray Emission from Jupiter

The Chandra X-ray Observatory (CXO) observed Jupiter during the period 24-26 February 2003 for approx. 40 hours (4 Jupiter rotations), using both the spectroscopy array of the Advanced CCD Imaging Spectrometer (ACIS-S) and the imaging array of the High-Resolution Camera (HRC-I). Two ACIS-S exposures, each -8.5 hours long, were separated by an HRC-I exposure of approx. 20 hours. The low- to middle-latitude nonauroral disk X-ray emission is much more spatially uniform than the auroral emission. However, the low- to middle-latitude X-ray count rate shows a small but statistically significant hour angle dependence and depends on surface magnetic field strength. In addition, the X-ray spectra from regions corresponding to 3-5 gauss and 5-7 gauss surface fields show significant differences in the energy band 1.26-1.38 keV, perhaps partly due to line emission occurring in the 3-5 gauss region but not the 5-7 gauss region. A similar correlation of surface magnetic field strength with count rate is found for the 18 December 2000 HRC-I data, at a time when solar activity was high. The low- to middle-latitude disk X-ray count rate observed by the HRC-I in the February 2003 observation is about 50% of that observed in December 2000, roughly consistent with a decrease in the solar activity index (F10.7 cm flux) by a similar amount over the same time period. The low- to middle-latitude X-ray emission does not show any oscillations similar to the approx. 45 min oscillations sometimes seen from the northern auroral zone. The temporal variation in Jupiter's nonauroral X-ray emission exhibits similarities to variations in solar X-ray flux observed by GOES and TIMED/SEE. The two ACIS-S 0.3-2.0 keV low- to middle-latitude X-ray spectra are harder than the auroral spectrum and are different from each other at energies above 0.7 keV, showing variability in Jupiter's nonauroral X-ray emission on a timescale of a day. The 0.3-2.0 keV X-ray power emitted at low to middle latitudes is 0.21 GW and 0.39 GW for the first and second ACIS-S exposures, respectively. We suggest that X-ray emission from Jupiter's disk may be largely generated by the scattering and fluorescence of solar X rays in its upper atmosphere, especially at times of high incident solar X-ray flux. However, the dependence of count rate on surface magnetic-field strength may indicate the presence of some secondary component, possibly ion precipitation from radiation belts close to the planet.

Bhardwaj, Anil↗

Measuring X-Ray Emission Line Shapes in Neutral Species for XRISM Calibration

Space X-ray spectrometers such as the Resolve instrument on XRISM require precise calibration in order to interpret the spectra of astrophysical objects. Key components of the calibration are the energy scale and the core line spread function, both of which vary with photon energy. A major issue in the calibration of high-resolution spectrometers is locating good calibrators with well-known and stable intrinsic line shapes. Neutral fluorescence is widely used, but inner-shell transitions in neutral atoms often exhibit complex, poorly documented line shapes that vary with excitation conditions. Here, in this study, we present empirical measurements of K-shell transitions in neutral O and F below 1 keV using an engineering model XRISM calorimeter array, an electron bombardment modulated X-ray source, and an electron beam ion trap (EBIT) to provide a precise energy reference. In addition, we report measurements of the Mo Lα complex with the transition-edge microcalorimeter spectrometer (TEMS), which reveal strong satellite structure and sensitivity of the line shape to the incident exciting spectrum. Together, these results demonstrate the need for empirical line-shape models, highlight the nonstationary nature of neutral fluorescence features, and define a path toward developing transfer standards for XRISM and future precision instruments such as Athena/X-IFU.

Astronomy and AstroPhysics↗

Novel Applications of Focused Ion Beam Technique for Planetary Sample Analyses

We are using innovative FIB techniques to prepare samples of planetary materials for different types of coordinated analyses using ion microprobes, synchrotron beamlines, and specialized transmission electron microscopy (TEM) techniques. In these cases, the FIB sample preparation is the critical step in enabling these specialized analyses. We discuss several examples below utilizing the FEI Quanta3D instrument at the NASA Johnson Space Center. Trace element analyses utilizing synchrotron x-ray fluorescence. The trace element content of mineral grains in comet dust provides important clues on their formation and processing in the early solar system. We preformed coordinated analyses of a comet dust particle that had been prepared using ultramicrotomy for TEM analysis. Following the TEM analyses, we extracted a 70 nm thick section from a region of the carbon (C) film of the TEM grid, for additional analyses. A carbon ring ~2-3 μm thick was deposited on top of the C film using the FIB. The C film on the outer rim of the ring was milled away using various patterns to uniformly release the stresses on the film, preventing rupture and collapse, and was attached to the micromanipulator needle. We then isolated the ring completely and transferred the section to a silicon sample holder for analysis using the HXN (hard X-ray nanoprobe) beamline at NSLSII at Brookhaven National Lab. Coordinated Analyses of Presolar Grains. Rare sub-m presolar grains that originate in evolved stars and supernovae, occur in primitive astromaterials and are identified by their exotic isotopic compositions. Coordinated analyses of these grains using NanoSIMS, TEM, and other techniques on the same grain is enabled by innovative FIB sample preparation. In order to obtain subsequent isotopic analyses of Mg and Fe, contributions from surrounding grains were minimized. We precisely deposited a protective cap of Pt on top of the grain to preserve the grain of interest and then milled away about 5 μm diameter of the surrounding material. Following the isotopic analyses, the spindle was extracted and thinned to electron transparency for TEM microstructural analyses. In situ heating TEM experiments on lunar samples. We extracted a FIB thin section from Apollo 17 lunar rock 76015. To avoid ion-beam damage, e-beam deposition was used to deposit the first 500 nm of the C strap, followed by ion beam-assisted deposition of ~3 μm carbon. We performed an ex situ lift-out of the section and placed the section on one of the elements of a microelectromechanical systems (MEMS) - specialized heating substrate and attached the section to the substrate by depositing small C straps with the FIB. The heating chips utilize silicon nitride windows to support the samples and provide uniform heating while enabling TEM imaging. The heating chip was loaded into a Hitachi “Blaze” heating holder and analyzed using a Hitachi HF5000 at the University of Arizona.

Rahman, Z.↗

Applicability of Micro X-Ray Fluorescence Spectroscopy to Astromaterials Curation and Research

Introduction: The Astromaterials Acquisition and Curation Office at NASA’s Johnson Space Center (JSC) curates NASA’s astromaterial sample collections which includes: Apollo samples, Luna samples, Ant-arctic meteorites, cosmic dust particles, microparticle impacts into space-flown materials, Genesis solar wind atoms, Stardust comet Wild-2 particles, Stardust inter-stellar particles, Hayabusa asteroid Itokawa particles, Hayabusa 2 asteroid Ryugu particles, and future OSIRIS-Rex asteroid Bennu particles (landing in Sep-tember, 2023) [1–3]. To enhance JSC’s advanced cu-ration capabilities, we have recently installed a high-performance micro-X-ray fluorescence (µXRF) spec-trometer to assist in sample characterization through rapid, non-destructive, in-situ elemental analyses that do not require the sample preparation protocols (i.e., polishing and carbon-coating) commonly needed for electron beam analyses. With this new instrument, we are capable of detecting all elements down to carbon in a variable-pressure or He-purged chamber for anal-ysis of a wide range of sample types. Here we describe the instrumental set-up, capabilities, and applicability of µXRF analysis to astromaterials curation and re-search. Instrumentation and Methodology: The X-ray fluorescence and computed tomography lab (X-FaCT) lab at JSC is now equipped with a Bruker M4 Tornado Plus µXRF (Fig. 1). This system is an energy-dispersive x-ray spectrometer equipped with two 60 mm2 silicon drift detectors (SDD) that are able to be used simulta-neously for output count rates ~500,000 cps. New light element windows allow detecting and analyzing the entire elemental range from carbon to americium. Two x-ray tubes (micro-focus Rh with polycapillary lenses and W with collimators of 0.5, 1.0, 2.0, and 4.5 mm) with max excitation parameters of 50 kV, 30 W and 50 kV, 40 W, respectively, allow for more flexibility of the analysis of high energy lines. The motorized X-Y-Z stage has a mapping range of 190 x 160 mm and can support samples up to 7 kg (~15.5 lbs) and a height of 120 mm [4]. Analytical modes include elemental analysis (down to ~20 µm spot size) via point, line, or area of bulk materials (rock surfaces, thin sections, thick sections, etc.) as well as coating analysis (determination of thickness and composition) of samples. This system has a variable vacuum chamber (1 mbar to 1 atm) that is also equipped with a He-purge system which accommodates vacuum sensitive samples while still allowing detection of light elements at atmospheric pressure. Utility and Applicability of µXRF in Astro-materials research and exploration science (ARES): Elemental analysis using µXRF is commonly em-ployed for both terrestrial and planetary geological science disciplines [5]. It is especially useful for analy-sis of astromaterials given the limited sample prepara-tion required, which is not feasible for certain materi-als. Here we show select applications of µXRF anal-yses of astromaterials that can, have, and will be done at JSC’s X-FaCT lab. Point analysis: In-situ spot analyses (~20 µm spot size) on a cut slab of Martian meteorite NWA 10922 allowed for the discovery, qualitative elemental analy-sis and determination of different feldspar minerals [6]. These point analyses served as an effective prelim-inary step for subsequent quantitative analyses. Ana-lytical standards can be employed for more accurate quantification of µXRF spot analyses. Area analysis: This analytical mode measures all detectable elements (from C to Am) at each pixel (>5 µm pixel size) in a user-defined area. The results are shown as elemental maps which can be extracted as 16-bit TIFF’s for further data processing. In Fig. 2. we show elemental distribution maps of the high-Ti basalt 73001,531 that have been processed using ImageJ software. From these maps you can accurately and quickly (this map took ~50 mins.) identify mineral components, such as pyroxene, plagioclase, oxides, and phosphates, compositional zoning, and mineral textures. Detection of high-Z phases: µXRF techniques are es-pecially effective at analyzing trace minerals with high-atomic-number (high-Z) elements because the high-energy characteristic X-rays used (relative to SEM EDS) allow for mapping of K lines in elements up to La (typically SEM maps use L X-ray lines for elements >Zn, and these can often have interferences). Thus, µXRF is especially suited for identifying minerals like zircon, baddeleyite, REE-rich phosphates, Fe-rich met-als, oxides, sulfides, and phosphides [4]. In Fig. 3 we show elemental distribution maps for 73001,530 where we are able to correlate the original video image with, Zr, Si, Y and Hf elemental maps together identi-fying the location of a zircon. In this location you would expect lower Si compared to surrounding mate-rial, as well as higher Zr, Y, and Hf content compared to surrounding material, all of which is confirmed by our XRF ele-mental distribution maps (Figure 2.) Conclusions: The new M4 Tornado Plus µXRF within the Astromaterials Acquisition and Curation office at NASA JSC allows for rapid and non-destructive elemental analysis of astromaterials with limited or no sample preparation. µXRF analyses pro-vide crucial compositional knowledge for the prelimi-nary examination and curation of astromaterials. This instrument enhances the advanced curation capabili-ties in the X-FaCT laboratory at JSC by allowing pro-ductive, cohesive, and non-destructive multi-modal x-ray analyses on astromaterial samples, which is neces-sary for the comprehensive curation and study of our current and future astromaterial collections. Addition-ally, µXRF can provide complimentary information to researchers for studies on astromaterials. References: [1] Allen, C. et al., (2011). Chemie De Erde Geochemistry, 71, 1-20. [2] McCubbin, F. M. et al., (2016) 47th LPSC, abstract #2668 [3] Zeigler, R. A. et al., (2017) 48th LPSC, abstract #2772 [4] Bruker User Manual [5] Young et al., (2016) Appl. Geochemistry, 72, 77-87 [6] Mor-ris, R. V. et al., (2023) 54th LPSC.

E W O'Neal↗

Local halide heterogeneity drives surface wrinkling in mixed-halide wide-bandgap perovskites

Compositional heterogeneity in wide-bandgap (1.8 - 2.1 eV) mixed-halide perovskites is a key bottleneck in the processing of high-quality solution-processed thin films and prevents their application in efficient multijunction solar cells. Notably, mixed-cation (formamidinium-methylammonium) wide-bandgap perovskite films are prone to form micrometer-scale wrinkles which can interfere with the smooth surfaces ideal for multijunction devices. Here, we study the formation dynamics of wrinkled mixed-halide perovskite films and its impact on the local composition and optoelectronic properties. We use in situ X-ray scattering during perovskite film formation to show that crystallization of bromide-rich perovskites precedes that of mixed-halide phases in wrinkled films cast using an antisolvent-based process. Using nanoscopic X­-ray fluorescence and hyperspectral photoluminescence imaging, we also demonstrate the formation of iodide- and bromide-rich phases in the wrinkled domains. This intrinsic spatial halide segregation results in an increased local bandgap variation and Urbach energy. Morphological disorder and compositional heterogeneity also aggravate the formation of sub-bandgap electronic defects, reducing photostability and accelerating light-induced segregation of iodide and bromide ions in thin films and solar cells.

36 MATERIALS SCIENCE↗

The comet rendezvous asteroid flyby mission

The Comet Rendezvous Asteroid Flyby Mission (CRAF) is described. After gravity assists from Venus and Earth, the spacecraft will fly by the asteroid 46 Hestia en route to a rendezvous with P/Tempel 2 in Nov. 1996, when the comet is near aphelion. The scientific experiments for the CRAF mission are: an imaging system; a visual and infrared mapping spectrometer; an infrared radiometer; a penetrator carrying a gamma-ray spectrometer, a scanning differential calorimeter and evolved gas analyzer, accelerometers, and temperature probes; a neutral gas and thermal ion mass spectrometer; a secondary ion mass spectrometer for analyzing dust, gas, and thermal ions; a scanning electron microscope and particle analyzer; an X-ray fluorescence and gas chromatographic analyzer for collected dust and ice samples; a dust counter and velocity analyzer; a retarding potential ion mass spectrometer; a supra-thermal ion mass spectrometer and electron analyzer; a magnetometer; and a coordinated radio, electron, and plasma wave analyzer.

Neugebauer, M.↗

Lunar scout missions: Galileo encounter results and application to scientific problems and exploration requirements

The Lunar Scout Missions (payload: x-ray fluorescence spectrometer, high-resolution stereocamera, neutron spectrometer, gamma-ray spectrometer, imaging spectrometer, gravity experiment) will provide a global data set for the chemistry, mineralogy, geology, topography, and gravity of the Moon. These data will in turn provide an important baseline for the further scientific exploration of the Moon by all-purpose landers and micro-rovers, and sample return missions from sites shown to be of primary interest from the global orbital data. These data would clearly provide the basis for intelligent selection of sites for the establishment of lunar base sites for long-term scientific and resource exploration and engineering studies. The two recent Galileo encounters with the Moon (December, 1990 and December, 1992) illustrate how modern technology can be applied to significant lunar problems. We emphasize the regional results of the Galileo SSI to show the promise of geologic unit definition and characterization as an example of what can be done with the global coverage to be obtained by the Lunar Scout Missions.

Head, J. W.↗

Precision Fe K-Alpha and Fe K-Beta Line Spectroscopy of the Seyfert 1.9 Galaxy NGC 2992 with Suzaku

We present detailed time-averaged X-ray spectroscopy in the 0.5-10 keV band of the Seyfert 1.9 galaxy NGC 2992 with the Suzaku X-ray Imaging Spectrometers (XIS). The source had a factor approximately 3 higher 2-10 keV flux (approximately 1.2 x l0(exp -11) erg per square cm per s) than the historical minimum and a factor approximately 7 less than the historical maximum. The XIS spectrum of NGC 2992 can be described by several components. There is a primary continuum, modeled as a power-law with a photon index of Gamma = 1.57(sup +0.06) (sup -0.03) that is obscured by a Compton-thin absorber with a column density of 8.01(sup +0.6) (sup -0.5)x l0 (exp 21) per square cm. . There is another, weaker, unabsorbed power-law component (modeled with the same slope as the primary), that is likely to be due to the primary continuum being electron-scattered into our line-of-sight by a region extended on a scale of hundreds of parsecs. We measure the Thomson depth of the scattering zone to be Tau = 0.072 +/- 0.021. An optically-thin thermal continuum emission component, which probably originates in the same extended region, is included in the model and yields a temperature and luminosity of KT = 0.656(sup +0.088) (sup -0.0.61) keV and approximately 1.2 +/- 0.4 x l0 (exp 40) erg per s respectively. We detect an Fe K emission complex which we model with broad and narrow lines and we show that the intensities of the two components are decoupled at a confidence level > 3 sigma. The broad Fe K alpha line has an equivalent width of 118(sup +32) (sup -61) eV and could originate in an accretion disk (with inclination angle greater than approximately 30 deg) around the putative central black hole. The narrow Fe K alpha line has an equivalent width of 1632(sup +47) (sup -26) eV and is unresolved (FWHM < 4630 km per s) and likely originates in distant matter. The absolute flux in the narrow line implies that the column density out of the line-of-sight could be much higher than measured in the line-of-sight, and that the mean (historically-averaged) continuum luminosity responsible for forming the line could be a factor of several higher than that measured from the data. We also detect the Fe K Beta line (corresponding to the narrow Fe K alpha line) with a high signal-to-noise ratio and describe a new robust method to constrain the ionization state of Fe responsible for the Fe K alpha and Fe K Beta lines that does not require any knowledge of possible gravitational and Doppler energy shifts affecting the line energies. For the distant line-emitting matter (e. g. the putative obscuring torus) we deduce that the predominant ionization state is lower than Fe VIII (at 99% confidence), conservatively taking into account residual calibration uncertainties in the XIS energy scale and theoretical and experimental uncertainties in the Fe K fluorescent line energies. From the limits on a possible Compton-reflection continuum it is likely that the narrow Fe K alpha and Fe K Beta lines originate in a Compton-thin structure.

Yaqoob, Tahir↗

Mapping alpha-Particle X-Ray Fluorescence Spectrometer (Map-X)

Many planetary surface processes (like physical and chemical weathering, water activity, diagenesis, low-temperature or impact metamorphism, and biogenic activity) leave traces of their actions as features in the size range 10s to 100s of micron. The Mapping alpha-particle X-ray Spectrometer ("Map-X") is intended to provide chemical imaging at 2 orders of magnitude higher spatial resolution than previously flown instruments, yielding elemental chemistry at or below the scale length where many relict physical, chemical, and biological features can be imaged and interpreted in ancient rocks.

CCD Camera↗

NASAs Evolvable Mars Campaign: Mars Moons Robotic Precursor

Human exploration missions to the moons of Mars are being considered within NASA's Evolvable Mars Campaign (EMC) as an intermediate step for eventual human exploration and pioneering of the surface of Mars. A range of mission architectures is being evaluated in which human crews would explore one or both moons for as little as 14 days or for as long as 500 days with a variety of orbital and surface habitation and mobility options being considered. Relatively little is known about the orbital, surface, or subsurface characteristics of either moon. This makes them interesting but challenging destinations for human exploration missions during which crewmembers must be able to effectively conduct scientific exploration without being exposed to undue risks due to radiation, dust, micrometeoroids, or other hazards. A robotic precursor mission to one or both moons will be required to provide data necessary for the design and operation of subsequent human systems and for the identification and prioritization of scientific exploration objectives. This paper identifies and discusses considerations for the design of such a precursor mission based on current human mission architectures. Objectives of a Mars' moon precursor in support of human missions are expected to include: 1) identifying hazards on the surface and the orbital environment at up to 50-km distant retrograde orbits; 2) collecting data on physical characteristics for planning of detailed human proximity and surface operations; 3) performing remote sensing and in situ science investigations to refine and focus future human scientific activities; and 4) prospecting for in situ resource utilization. These precursor objectives can be met through a combination or remote sensing (orbital) and in-situ (surface) measurements. Analysis of spacecraft downlink signals using radio science techniques would measure the moon's mass, mass distribution, and gravity field, which will be necessary to enable trajectory planning. Laser altimetry would precisely measure the moon's shape and improve the accuracy of radio science measurements. A telescopic imaging camera would map the moon at submeter resolution and photograph selected areas of interest at subcentimeter resolution and a visible and near-infrared (0.4-3.0 mm) imaging spectrograph would produce a global map of mineral composition variations at a resolution of tens of meters and maps of selected areas of interest at meter resolution. Additional remote sensing capabilities could include a thermal infrared imager (heat flow, thermal inertia, and grain size distributions), a gamma-ray and neutron detector (atomic composition), a ground-penetrating radar (internal structure), and a magnetometer and Langmuir probe (magnetic properties and plasma field). Once on the surface of Phobos or Deimos, necessary instrumentation would include a penetrometer (regolith compressive strength), a motion-imagery camera (to observe the penetrometer tests before, during, and after contact), a dust-adhesion witness plate and camera (dust levitation), a microimager (dust particle sizes and shapes), and an alpha-proton-X-ray, X-ray fluorescence, Mossbauer, or Raman spectrometer (atomic and mineral composition of surface materials) and an optional temperature probe (regolith thermal properties). A variety of robotic mission design options to enable both orbital and surface measurements are being considered that include fully integrated and modular approaches. In-situ measurements from at least one surface location would be required, with additional measurement locations possible through use of multiple landers, through propulsive relocation of a single lander, or through electromechanical surface translation by a walking or hopping lander vehicle, which could also serve to evaluate such mobility capabilities for subsequent human missions. Preliminary orbital analysis suggests that remote sensing would likely be performed while in a distant retrograde orbit around the target moon. Mission design options to enable characterization of both Mars’ moons in a single mission are also being studied.

Gernhardt, Michael L.↗