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NASA NTRS2006

X-Ray Detector Research at MSFC for Space Applications

NASA's Vision for Space Exploration has specific goals aimed at exploring the Solar System. This vision, under presidential mandate includes landing humans on the moon before the end of the next decade, paving the way for eventual journeys to Mars and beyond. The first missions to the moon will be in the form of both Orbiters and Landers, with the goal of paving the way for human return. One of the instruments we are currently working on,in collaboration with Brookhaven National Laboratory, is a lunar orbiter fluorescent x-ray spectrometer to finely map the light elements (down to Carbon) on surface of the moon. Funded NASA s Planetary Instrument Definition and Development Program the instrument is based on silicon drift detector arrays read out by custom ASICs. These offer the promise of high spectral resolution, necessary for resolving weak lines against a strong background continuum, and very low power requirements, necessary for large areas (greater than 500 square centimeters) required for future lunar missions. Further, the inherent radiation hardness of these detectors makes them ideal candidates for exploring the Jovian system, where the harsh radiation environment from Jupiter s radiation belts creates unfavorable detector conditions. Looking beyond our solar system, in the hard x-ray regime (20-80keV.), we are studying Cadmium-Zinc-Telluride pixilated detectors as feasible candidates for focal plane detectors of a hard x-ray telescope. This energy region bridges the gap between thermal and non-thermal x-ray emission from astronomical sources, will allow us to better understand supernovae nucleosynthesis (such as through the Ti-44 lines at 68keV and 78keV), Active Galactic Nuclei and other compact objects, more completely. The detectors that we are characterizing are 2mm in thickness and are pixilated with a 16x16 array of 300 micrometer pitch pixels (50micometer gap). These detectors are designed at Rutherford Appleton Laboratory, material is from eV Products, and polymer flip-chip assembly was performed by a commercial vendor. An energy resolution of 2.0% at 60keV (or better) should allow us to sufficiently distinguish lines of interest from background continuum, and the detector spatial resolution should be fine enough to over-sample the focal spot from the x-ray focusing optics by about a factor of two. Full technical details of these developments will be presented.

Gaskin, Jessica↗
NASA NTRS2016

Application of X-Ray Pulsar Navigation: A Characterization of the Earth Orbit Trade Space

The potential for pulsars as a navigation source has been studied since their discovery in 1967. X-ray pulsar navigation (XNAV) is a celestial navigation system that uses the consistent timing nature of x-ray photons from milli-second pulsars (MSP) to perform space navigation. By comparing the detected arrival of x-ray photons to a reference database of expected pulsar lightcurve timing models, one can infer a range and range rate measurement based on light time delay. Much of the challenge of XNAV comes from the faint signal, availability, and distant nature of pulsars. This is a study of potential pulsar XNAV measurements to measure extended Kalman filter (EKF) tracking performance with a wide trade space of bounded Earth orbits, using a simulation of existing x-ray detector space hardware. An example of an x-ray detector for XNAV is the NASA Station Explorer for X-ray Timing and Navigation (SEXTANT) mission, a technology demonstration of XNAV set to perform on the International Space Station (ISS) in late 2016early 2017. XNAV hardware implementation is driven by trajectory and environmental influences which add noise to the x-ray pulse signal. In a closed Earth orbit, the radiation environment can exponentially increase the signal noise from x-ray pulsar sources, decreasing the quality and frequency of measurements. The SEXTANT mission in particular improves on the signal to noise ratio by focusing an array of 56 x-ray silicon drift detectors at one pulsar target at a time. This reduces timing glitches and other timing noise contributions from ambient x-ray sources to within a 100 nanosecond resolution. This study also considers the SEXTANT scheduling challenges inherent in a single target observation. Finally, as the navigation sources are now relatively inertial targets, XNAV measurements are also subject to periods of occultation from various celestial bodies. This study focuses on the characterization of these drivers in closed Earth orbits and is not a tuning analysis of the EKF. The study shows that the closed Earth orbit for XNAV performance is reliant on the orbit semi-major axis and eccentricity as well as orbit inclination. These parameters are the primary drivers of pulsar measurement availability and significantly influence the natural spacecraft orbit dynamics. Sensitivity to initial orbit determination error growth due to the scarcity of XNAV measurements within an orbital period require appropriate timing of initial XNAV measurements. The orbit angles of argument of perigee and right ascension of the ascending node, alongside the other orbit parameters, complete the initial cadence of XNAV measurements. The performance of initial XNAV measurements then propagates throughout the experimental period. The study provides a basis to missions who wish to consider XNAV as a potential navigation source in a closed Earth orbit design. It provides a family of orbit trajectories as well as other modeling considerations needed to effectively evaluate if XNAV is an effective navigation source for a potential mission. As an EKF is sensitive to a linearized estimated state, this study has a direct benefit of providing effective XNAV measurements to maintain spacecraft tracking, independent of other navigation sources. In the particular use case of the SEXTANT mission, it also provides a novel scheduling algorithm which addresses the need to prioritize and manage pulsar observations for effective navigation.

PULSAR↗
NASA NTRS2016

Application of X-Ray Pulsar Navigation: A Characterization of the Earth Orbit Trade Space

The potential for pulsars as a navigation source has been studied since their discovery in 1967. X-ray pulsar navigation (XNAV) is a celestial navigation system that uses the consistent timing nature of x-ray photons from millisecond pulsars (MSP) to perform space navigation. By comparing the detected arrival of x-ray photons to a reference database of expected pulsar light-curve timing models, one can infer a range and range rate measurement based on light time delay. Much of the challenge of XNAV comes from the faint signal, availability, and distant nature of pulsars. This is a study of potential pulsar XNAV measurements to measure extended Kalman filter (EKF) tracking performance with a wide trade space of bounded Earth orbits, using a simulation of existing x-ray detector space hardware. An example of an x-ray detector for XNAV is the NASA Station Explorer for X-ray Timing and Navigation (SEXTANT) mission, a technology demonstration of XNAV set to perform on the International Space Station (ISS) in late 2016early 2017. XNAV hardware implementation is driven by trajectory and environmental influences which add noise to the x-ray pulse signal. In a closed Earth orbit, the radiation environment can exponentially increase the signal noise from x-ray pulsar sources, decreasing the quality and frequency of measurements. The SEXTANT mission in particular improves on the signal to noise ratio by focusing an array of 56 x-ray silicon drift detectors at one pulsar target at a time. This reduces timing glitches and other timing noise contributions from ambient x-ray sources to within a 100 nanosecond resolution. This study also considers the SEXTANT scheduling challenges inherent in a single target observation. Finally, as the navigation sources are now relatively inertial targets, XNAV measurements are also subject to periods of occultation from various celestial bodies. This study focuses on the characterization of these drivers in closed Earth orbits and is not a tuning analysis of the EKF. The study shows that the closed Earth orbit for XNAV performance is reliant on the orbit semi-major axis and eccentricity as well as orbit inclination. These parameters are the primary drivers of pulsar measurement availability and significantly influence the natural spacecraft orbit dynamics. Sensitivity to initial orbit determination error growth due to the scarcity of XNAV measurements within an orbital period require appropriate timing of initial XNAV measurements. The orbit angles of argument of perigee and right ascension of the ascending node, alongside the other orbit parameters, complete the initial cadence of XNAV measurements. The performance of initial XNAV measurements then propagates throughout the experimental period. The study provides a basis to missions who wish to consider XNAV as a potential navigation source in a closed Earth orbit design. It provides a family of orbit trajectories as well as other modeling considerations needed to effectively evaluate if XNAV is an effective navigation source for a potential mission. As an EKF is sensitive to a linearized estimated state, this study has a direct benefit of providing effective XNAV measurements to maintain spacecraft tracking, independent of other navigation sources. In the particular use case of the SEXTANT mission, it also provides a novel scheduling algorithm which addresses the need to prioritize and manage pulsar observations for effective navigation.

x-ray↗
NASA NTRS2012

Experimental Validation of Pulse Phase Tracking for X-Ray Pulsar Based

Pulsars are a form of variable celestial source that have shown to be usable as aids for autonomous, deep space navigation. Particularly those sources emitting in the X-ray band are ideal for navigation due to smaller detector sizes. In this paper X-ray photons arriving from a pulsar are modeled as a non-homogeneous Poisson process. The method of pulse phase tracking is then investigated as a technique to measure the radial distance traveled by a spacecraft over an observation interval. A maximum-likelihood phase estimator (MLE) is used for the case where the observed frequency signal is constant. For the varying signal frequency case, an algorithm is used in which the observation window is broken up into smaller blocks over which an MLE is used. The outputs of this phase estimation process were then looped through a digital phase-locked loop (DPLL) in order to reduce the errors and produce estimates of the doppler frequency. These phase tracking algorithms were tested both in a computer simulation environment and using the NASA Goddard Space flight Center X-ray Navigation Laboratory Testbed (GXLT). This provided an experimental validation with photons being emitted by a modulated X-ray source and detected by a silicon-drift detector. Models of the Crab pulsar and the pulsar B1821-24 were used in order to generate test scenarios. Three different simulated detector trajectories were used to be tracked by the phase tracking algorithm: a stationary case, one with constant velocity, and one with constant acceleration. All three were performed in one-dimension along the line of sight to the pulsar. The first two had a constant signal frequency and the third had a time varying frequency. All of the constant frequency cases were processed using the MLE, and it was shown that they tracked the initial phase within 0.15% for the simulations and 2.5% in the experiments, based on an average of ten runs. The MLE-DPLL cascade version of the phase tracking algorithm was used in the varying frequency case. This resulted in tracking of the phase and frequency by the DPLL outputs in both the simulation and experimental environments. The crab pulsar was experimentally tested with a trajectory with a higher acceleration. In this case the phase error tended toward zero as the observation extended to 250 seconds and the doppler frequency error tended to zero in under 100 seconds.

Experimental↗
NASA NTRS1972

Methods of measurement for semiconductor materials, process control, and devices

Activities directed toward the development of methods of measurement for semiconductor materials, process control, and devices are described. Topics investigated include: measurements of transistor delay time; application of the infrared response technique to the study of radiation-damaged, lithium-drifted silicon detectors; and identification of a condition that minimizes wire flexure and reduces the failure rate of wire bonds in transistors and integrated circuits under slow thermal cycling conditions. Supplementary data concerning staff, standards committee activities, technical services, and publications are included as appendixes.

Bullis, W. M.↗
NASA NTRS1972

Advanced technical developments in support of scientific experiments in space

A technique was developed for preparing solid state, lithium-drifted silicon detectors. Hollow cylindrical detectors were built and tested for possible use as anticoincidence shields to replace conventional plastic scintillators and photomultipliers. A fission cell was developed for the Pioneer F/G instruments and the IMP I subsystem. An electron current detector was developed for Jovian belt measurements of electron flux. A number of circuits and semiconductor devices was also developed.

Lamport, J. E.↗
NASA NTRS1982

Carbon and oxygen X-ray line emission from the interstellar medium

A soft X-ray, 0.3-1.0 keV spectrum from a 1 sr region which includes a portion of the North Polar Spur, obtained by three rocketborne lithium-drifted silicon detectors, shows the C V, C VI, O VII and O VIII emission lines. The spectrum is well fitted by a two-component, modified Kato (1976) model, where the coronal emission is in collisional equilibrium, with interstellar medium and North Polar Spur temperatures of 1.1 and 3.8 million K, respectively.

Schnopper, H. W.↗
NASA NTRS2009

Modern Material Analysis Instruments Add a New Dimension to Materials Characterization and Failure Analysis

Modern analytical tools can yield invaluable results during materials characterization and failure analysis. Scanning electron microscopes (SEMs) provide significant analytical capabilities, including angstrom-level resolution. These systems can be equipped with a silicon drift detector (SDD) for very fast yet precise analytical mapping of phases, as well as electron back-scattered diffraction (EBSD) units to map grain orientations, chambers that admit large samples, variable pressure for wet samples, and quantitative analysis software to examine phases. Advanced solid-state electronics have also improved surface and bulk analysis instruments: Secondary ion mass spectroscopy (SIMS) can quantitatively determine and map light elements such as hydrogen, lithium, and boron - with their isotopes. Its high sensitivity detects impurities at parts per billion (ppb) levels. X-ray photo-electron spectroscopy (XPS) can determine oxidation states of elements, as well as identifying polymers and measuring film thicknesses on coated composites. This technique is also known as electron spectroscopy for chemical analysis (ESCA). Scanning Auger electron spectroscopy (SAM) combines surface sensitivity, spatial lateral resolution (10 nm), and depth profiling capabilities to describe elemental compositions of near and below surface regions down to the chemical state of an atom.

Panda, Binayak↗
NASA NTRS2013

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 NTRS2014

The Neutron Star Interior Composition Explorer (NICER)

The Neutron Star Interior Composition Explorer (NICER) is an approved NASA Explorer Mission of Opportunity dedicated to the study of the extraordinary gravitational, electromagnetic, and nuclear‐physics environments embodied by neutron stars. Scheduled to be launched in 2016 as an International Space Station payload, NICER will explore the exotic states of matter, using rotation‐resolved spectroscopy of the thermal and non‐thermal emissions of neutron stars in the soft (0.2‐12 keV) X‐ray band. Grazing‐incidence "concentrator" optics coupled with silicon drift detectors, actively pointed for a full hemisphere of sky coverage, will provide photon‐counting spectroscopy and timing registered to GPS time and position, with high throughput and relatively low background. The NICER project plans to implement a Guest Observer Program, which includes competitively selected user targets after the first year of flight operations. I will describe NICER and discuss ideas for potential Be/X‐ray binary science.

Wilson-Hodge, Colleen A.↗
NASA NTRS2016

Miniature X-Ray Solar Spectrometer: A Science-Oriented, University 3U CubeSat

The miniature x-ray solar spectrometer is a three-unit CubeSat developed at the Laboratory for Atmospheric and Space Physics at the University of Colorado, Boulder. Over 40 students contributed to the project with professional mentorship and technical contributions from professors in the Aerospace Engineering Sciences Department at University of Colorado, Boulder and from Laboratory for Atmospheric and Space Physics scientists and engineers. The scientific objective of the miniature x-ray solar spectrometer is to study processes in the dynamic sun, from quiet sun to solar flares, and to further understand how these changes in the sun influence the Earth's atmosphere by providing unique spectral measurements of solar soft x-rays. The enabling technology providing the advanced solar soft x-ray spectral measurements is the Amptek X123, a commercial off-the-shelf silicon drift detector. The Amptek X123 has a low mass (approx. 324 g after modification), modest power consumption (approx. 2.50 W), and small volume (6.86 x 9.91 x 2.54 cm), making it ideal for a CubeSat. This paper provides an overview of the miniature x-ray solar spectrometer mission: the science objectives, project history, subsystems, and lessons learned, which can be useful for the small-satellite community.

Mason, James P.↗
NASA NTRS2016

Performance of NICER Flight X-Ray Concentrator

Neutron star Interior Composition ExploreR (NICER) is a NASA instrument to be onboard International Space Station, which is equipped with 56 pairs of an X-ray concentrator (XRC) and a silicon drift detector for high timing observations. The XRC is based on an epoxy replicated thin aluminum foil X-ray mirror, similar to those of Suzaku and ASTRO-H (Hitomi), but only a single stage parabolic grazing incidence optic. Each has a focal length of 1.085 m and a diameter of 105 mm, with 24 confocally aligned parabolic shells. Grazing incident angles to individual shells range from 0.4 to 1.4 deg. The flight 56 XRCs have been completed and successfully delivered to the payload integration. All the XRC was characterized at the NASA/GSFC 100-m X-ray beamline using 1.5 keV X-rays (some of them are also at 4.5 keV). The XRC performance, effective area and point spread function, was measured by a CCD camera and a proportional counter. The average effective area is about 44 sq cm at 1.5 keV and about 18 sq cm at 4.5 keV, which is consistent with a micro-roughness of 0.5 nm from individual shell reflectivity measurements. The XRC focuses about 91% of X-rays into a 2mm aperture at the focal plane, which is the NICER detector window size. Each XRC weighs only 325 g. These performance met the project requirement. In this paper, we will present summary of the flight XRC performance as well as co-alignment results of the 56 XRCs on the flight payload as it is important to estimate the total effective for astronomical observations.

X-ray concentrator↗
NASA NTRS2020

Design and construction of the X-ray instrumentation onboard the HaloSat CubeSat

HaloSat is the first mission funded by NASA’s Astrophysics Division to use the CubeSat platform. Using three co-aligned silicon drift detectors, the HaloSat observatory measures soft (0.4 to 7 keV) x-ray emission from sources of diffuse emission such as the hot, gaseous halo of the Milky Way. We describe the design and construction of the science payload on HaloSat and the reasoning behind many of the choices. As a direct result of the design choices and adherence to best practices during construction, the HaloSat science payload continues to perform well after more than one year on-orbit.

Daniel M. LaRocca↗
NASA NTRSDate not supplied

A Transmission Electron Microscopy Study of a Refractory Metal Grain from a Calcium-Aluminum-Rich Inclusion in the Leoville CV3 Chondrite

Introduction: Calcium-aluminum-rich inclusions (CAIs) are an important component of chondritic meteorites. They can contain materials that are thermodynamically predicted and isotopically age dated to be among the first-formed solids in our solar system [1-5]. Observed in some CAIs are micron to sub-micron sized inclusions rich in Fe, Ni, and high-Z elements such as Pt, Os, Ir and W, in the form of refractory metal nuggets (RMNs), fremdlinges, and ‘nugget like objects’ (NLOs) [1,6]. Refractory siderophile elements such as Os, Ir and Ru are thermodynamically predicted to condense at temperatures well in excess of the major CAI phases such as melilite, perovskite, spinel and hibonite [2,7-9]. These refractory metal inclusions in CAIs can therefore serve as probes into the thermodynamic landscape of the early solar protoplanetary disk. Here we report on a refractory grain identified in a CAI of the Leoville CV3 chondrite. This work is part of an ongoing effort to gain insight into the thermochemistry of the early solar system through systematic analyses of the structure and chemistry of various components in CAIs [10-13]. Sample and Analytical Techniques: A fluffy type A CAI (Fig. 1A) was identified in a section of the Leoville, CV3 chondrite (Center for Meteorite Studies, Arizona State University collection, #821_C_3) using a JOEL-JXA 8530F electron microprobe at Arizona State University. Backscattered electron (BSE) imaging and energy-dispersive X-ray spectroscopy (EDS) were used to identify refractory metal grains in the CAI using a Thermo Fisher (formerly FEI) Helios NanoLab 660 G3 focused-ion-beam scanning-electron microscope (FIBSEM) located at the Kuiper Materials Imaging and Characterization Facility (KMICF) at the Lunar and Planetary Laboratory, University of Arizona. The FIB is equipped with an EDAX EDS system. We selected one of the larger (micron-sized) refractory metal grains, designated as ‘Spud’ (Fig. 1B) for further analysis. ‘Spud’ was extracted and thinned to electron transparency (<100 nm) using the FIB-SEM located in KMICF, following methods described by [14- 15]. The FIB section was analyzed using a 200 keV Hitachi HF5000 scanning transmission electron microscope (S/TEM) located at KMICF. The HF5000 is equipped with cold-field emission gun, 3rd-order spherical aberration corrector for STEM imaging, and an Oxford Instruments X-Max N 100 TLE energydispersive spectroscopy (EDS) system with dual 100 mm2 windowless silicon-drift detectors (Ω = 2.0 sr). Selected-area electron-diffraction (SAED) patterns were acquired to aid in determination of crystallinity and phase. Results: The mineralogy, texture, and morphology of the CAI are consistent with that of a fluffy type A (FTA) CAI [16]. BSE imaging at high magnifications revealed grains with high contrast, indicative of compositions rich in elements of higher atomic number relative to surrounding material. These high-Z grains have sizes that range from ∼250 nm to 4 µm. EDS analyses confirm that the bright grains are metal-rich inclusions. A minor fraction of the grains are composed of only Fe and Ni, but the majority (∼60%) of the identified inclusions also contained various refractory siderophiles including Os, Ru, Zr, Ir and Mo. EDS analysis on the FIB-SEM of Spud shows that it contains Fe, Ni, Mo and Ru. High-angle annular dark-field (HAAFD) imaging and EDS mapping in the TEM (Fig. 2) show that Spud occurs in melilite (Ca1.9Al1.99Si1.06O7). Spud contains a subhedral to anhedral morphology and is compositionally heterogenous (polyphasic, Fig. 2). Local spatial correlation occurs among Fe, Ni, and Pt, and also among Os, Ru, and Mo. SAED patterns show that the Fe-Ni-Pt, Fe-Os-Mo-Ru and Fe-Pt regions are crystalline. Discussion: CAIs can contain various types of inclusions rich in Fe, Ni and refractory siderophiles such as Os, Ru, W and Pt [1]. RMNs are micron-sized, single phase alloy grains and can contain Os, Ir, Ru and Rh [1,7,17]. NLOs are also micron-sized inclusions, but contain two phases, a refractory metal, and an oxide [6]. Fremdlinge are the largest of such inclusions (tens of microns in size) and are complex aggregates of Fe-Ni alloy, silicates, oxides, and sulfides [1,17]. While the size of Spud matches previous descriptions of RMNs and NLOs, Spud is neither a single-phase alloy like RMNs, nor does it contain one metal phase and one oxide like NLOs. Spud does not match the above described categories of refractory metal inclusions. The presence of refractory siderophiles such as Mo, Os, Ru, and Pt suggests a high-temperature origin. Thermodynamic modelling by [7] indicates condensation temperatures of 1917 K, 1693 K, 1613 K and 1415 K for Os, Mo, Ru and Pt respectively. These models also show that following the initial condensation of a refractory metal, alloying of solutes such as Fe, Ni and W, occurs in levels proportional to their partial pressures in the surrounding gas. Such alloying occurs at temperatures above the condensation temperatures of common CAI phases such as melilite (1529 K), perovskite (1441 K), spinel (197 K) and forsterite (1354 K) [2]. The polyphasic nature of Spud could be the result of such high-temperature alloying, possibly shortly after the condensation of Mo and Ru at 1693 K and 1613 K respectively. That Spud occurs as an inclusion is consistent with it having formed prior to and at temperature above that of its host melilite in this FTA CAI, which is qualitatively consistent with such prior thermodynamic modeling. Further, the polyphasic nature of Spud is similar to refractory grains from a FTA CAI in the Northwest Africa (NWA) 8323, CV3 chondrite [11-13]. These data suggest that such refractory metal grains could have been widespread in the inner and early solar protoplanetary disk and represent some of the earliest formed solids to have condensed. Acknowledgments: Research and instrumentation supported by NASA grants #NNX12AL47G, #NNX15AJ22G and #80NSSC19K0509, and NSF grants #1531243 and #0619599. Fig 2. STEM data on ‘Spud’. HAADF Image (Top) False-color EDS Maps (Bottom) References: [1] MacPherson G. J. (2014) T. of Geochem. Vol I: Met. And Cosmochem. Processes, 139-179. [2] Lodders K. (2003) ApJ, 591, 1220-1247. [3] Ebel D. S. (2006) Met. & the Early S. Sys. II., 253- 277. [4] Amelin Y. (2002) Science, 297, 1678-1683. [5] Connelly J.N. et.al. (2012) Science, 338, 651-655. [6] Schwander D. et al. (2015) GCA, 18, 70-87. [7] Palme H. and Wlotzka F. (1976) EPSL, 33, 45-60. [8] Berg T. et al. (2009) ApJ, 702, 172-176. [9] Liffman K. et al. (2021) Icarus, 221, 89-105. [10] Zega T.J. et al. (2021) PSJ, 2, 115. [11] Ramprasad T. et al. (2020) LPSC LI, Abstract #2472. [12] Ramprasad T. et al. (2021) Microscopy & Microanalysis, S1, 2792-2794. [13] Ramprasad T. et al. (2021) 84th MetSoc, Abstract #6123. [14] Zega T.J. et al. (2007) MAPS, 42, 1373-1386. [15] Ramprasad T. et al. (2022) MAPS, in revision. [16] Grossman L. (1975), GCA, 39, 433-454. [17] El Goresy A. et al. (1978) LPSC IX, Abstract#1100

T. Ramprasad↗
NASA NTRSDate not supplied

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.

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