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Focused Ion Beam Recovery of Hypervelocity Impact Residue in Experimental Craters on Metallic Foils

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Focused Ion Beam Recovery of Hypervelocity Impact Residue in Experimental Craters on Metallic Foils Focused ion beam recovery of hypervelocity impact residue in experimental craters on metallic foils Item Type Article; text Authors Graham, G. A.; Teslich, N.; Dai, Z. R.; Bradley, J. P.; Kearsley, A. T.; Hörz, F. Citation Graham, G. A., Teslich, N., Dai, Z. R., Bradley, J. P., Kearsley, A. T., & Hörz, F. (2006). Focused ion beam recovery of hypervelocity impact residue in experimental craters on metallic foils. Meteoritics & Planetary Science, 41(2), 159-165. DOI 10.1111/j.1945-5100.2006.tb00200.x Publisher The Meteoritical Society Journal Meteoritics & Planetary Science Rights Copyright © The Meteoritical Society Download date 24/09/2021 15:59:42 Item License http://rightsstatements.org/vocab/InC/1.0/ Version Final published version Link to Item http://hdl.handle.net/10150/656097 Meteoritics & Planetary Science 41, Nr 2, 159–165 (2006) Abstract available online at http://meteoritics.org Focused ion beam recovery of hypervelocity impact residue in experimental craters on metallic foils G. A. GRAHAM*1, N. TESLICH2, Z. R. DAI2, J. P. BRADLEY1, A. T. KEARSLEY3, and F. H÷RZ4 1Institute of Geophysics and Planetary Physics, Lawrence Livermore National Laboratory, Livermore, California 94551, USA 2Chemistry and Materials Science, Lawrence Livermore National Laboratory, Livermore, California 94551, USA 3Department of Mineralogy, The Natural History Museum, London, SW7 5BD, UK 4Astromaterials Research Office, NASA Johnson Space Center, Houston, Texas 77058, USA *Corresponding author. E-mail: [email protected] (Received 04 November 2005; revision accepted 01 December 2005) Abstract–The Stardust sample return capsule returned to Earth in January 2006 with primitive debris collected from comet 81P/Wild-2 during the flyby encounter in 2004. In addition to the cometary particles embedded in low-density silica aerogel, there are microcraters preserved in the aluminum foils (1100 series; 100 μm thick) that are wrapped around the sample tray assembly. Soda lime spheres (∼49 μm in diameter) have been accelerated with a light gas gun into flight-grade aluminum foils at 6.35 km s−1 to simulate the capture of cometary debris. The experimental craters have been analyzed using scanning electron microscopy (SEM) and X-ray energy dispersive spectroscopy (EDX) to locate and characterize remants of the projectile material remaining within the craters. In addition, ion beam– induced secondary electron imaging has proven particularly useful in identifying areas within the craters that contain residue material. Finally, high-precision focused ion beam (FIB) milling has been used to isolate and then extract an individual melt residue droplet from the interior wall of an impact. This has enabled further detailed elemental characterization that is free from the background contamination of the aluminum foil substrate. The ability to recover “pure” melt residues using FIB will significantly extend the interpretations of the residue chemistry preserved in the aluminum foils returned by Stardust. INTRODUCTION exposed to an interstellar dust stream during parts of the outbound cruise phase (Brownlee et al. 2003). The cometary The study of comets is fundamental to understanding and interstellar dust particles were primarily captured in low- early solar system processes (e.g., Brownlee 2003; Hanner density, highly porous silica aerogel tiles (Tsou et al. 2003). A 2003). To date, much of the knowledge of the composition of number of papers have dealt with the technique issues of specific comets is from remote or in situ analysis (e.g., Kissel material recovery from deep penetration tracks in aerogel et al. 1986; Kissel et al. 2004). Yet the most definitive generated by laboratory simulations or by low-Earth orbit characterization can only really be achieved by using the (LEO) space exposure in order to prepare for Stardust’s return diverse range of analytical instruments that are currently (e.g., Graham et al. 2004; Westphal et al. 2004; Ishii et al. available in the laboratory (Zolensky et al. 2000). Some 2005a, 2005b). interplanetary dust particles (IDPs) have already been linked The STA that holds the individual aerogel tiles is to cometary sources based on their mineralogical and optical wrapped with aluminum foils 100 μm thick (1100 series). The spectroscopy properties (Bradley and Brownlee 1986; space-exposed surfaces of these foils will also retain a record Bradley et al. 1999). However, it has not proven possible to of the hypervelocity encounters with both interstellar and define a specific parent body source. cometary particle populations. Previous studies of metallic In January 2004, the successful flyby of NASA’s Stardust surfaces exposed in space, e.g., those from the Long Duration spacecraft with comet 81P/Wild-2 resulted in the capture of Exposure Facility (LDEF), showed evidence of micrometer- abundant cometary debris (Brownlee et al. 2004; Tuzzolino et size craters as a result of meteoroid or orbital debris collisions al. 2004). In addition to the primary mission goal of the comet (e.g., Bernhard et al. 1993). Using analyses of impact residue flyby, the reverse side of the sample tray assembly (STA) was chemistry preserved within the craters, it was possible to 159 © The Meteoritical Society, 2006. Printed in USA. 160 G. A. Graham et al. derive the original impactor composition (e.g., Bernhard et al. The impact penetrations and residue material that are 1993; Brownlee et al. 1993). In addition to SEM/EDX discussed in this paper are from JSC shot #2382, a shot that studies, novel replication and residue recovery techniques accelerated soda lime glass spheres (43–54 μm in diameter) enabled detailed TEM studies of the meteoroid debris into the aluminum foil target at 6.35 km s−1. The velocity was (Teetsov and Bradley 1986; Bradley et al. 1986; Brownlee et measured using laser occultation methods and IR photo al. 1993). These techniques will be employed on the Stardust diodes for determination of the sabot pieces. Additionally, the foil samples. However, it is important to explore the new velocity of the projectiles impacting the foil was measured analytical capabilities that are now available for careful using an impact flash detector. Typically sabot velocity and selection, preparation, and manipulation of specifically projectile velocity agree to better than 1%. located micrometer-size material. Here we report on the use of focused ion beam microscopy to extract residue material Imaging and Microanalysis from an impact preserved in aluminum foils to simulate potential Stardust recovery. The foil target from JSC shot #2382 was initially imaged using a Leica MZ16 stereomicroscope fitted with a Leica ANALYTICAL METHODS DC500 12 mega-pixel CCD camera. The entire foil (25 × 25 mm) was attached to a large diameter pin-stub using Light Gas Gun Simulations conductive carbon paint. It was then imaged, analyzed and subjected to precision ion milling using an FEI Nova 600 dual A number of metallic foils that have previously been beam microscope comprising of a Ga+ liquid metal source exposed in low-Earth-orbit (LEO) as part of either dedicated focused ion beam (FIB) and field emission gun scanning experiments (such as those on LDEF) or as a target-of- electron microscope (FESEM). The dual beam microscope opportunity (e.g., on the Solar Maximum satellite) could have was fitted with an EDAX Genesis energy dispersive X-ray been used to develop and test capabilities for recovery and (EDX) spectrometer and an Omniprobe tungsten needle analysis of impacted material (e.g., Bradley et al. 1986; nanomanipulator. The secondary electron imaging was Bernhard et al. 1993). As meteoroid impacts on space- performed at 5 kV with a beam current of 0.15 nA and the exposed surfaces are likely to have occurred at velocities EDX single-point spot analysis and mapping were performed between 10–20 km s−1 (e.g., Brownlee et al. 1993), they are at 15–20 kV with a beam current of 0.26 nA. The FIB imaging not a representative analogue for the Stardust encounter and milling was carried out at 30 kV with a beam current velocity of ∼6 km s−1. As a result, a comprehensive shot ranging from 30–1000 pA. Imaging and elemental analysis of program was set up to provide analogous materials for extracted residue were performed using 200 kV FEI Tecnai laboratory investigation to support the interpretation of G2 F20 UT (scanning) transmission electron microscope Stardust samples. (TEM) fitted with an EDAX EDX spectrometer and FEI TIA The laboratory simulation experiments described in this spectral processing software. paper were performed using the small caliber (5 mm bore) two-stage light gas gun (LGG) at the Johnson Space Center RESULTS (JSC) in Houston, Texas. Glass spheres of known size range (Kearsley et al. 2006) and meteoritic materials (e.g., crushed SEM/EDX Imaging and Analysis Allende) were used as projectiles for calibration studies. Rather than accelerate individual particles, a “shotgun” From the secondary electron imaging of the foil target, approach is utilized by loading multiple projectiles into the we determined that the crater diameter ranged from 214 μm to small central cavity of a four-piece serrated sabot. The four 223 μm (Fig. 1a). The impact craters studied had completely sabot quadrants were designed to separate radially during free penetrated the 100 μm 1100 series foil and terminated in the flight, yet allow a substantial fraction of the projectile 6061 aluminum plate. As a result, the observed impacts have ensemble to remain on straight trajectories and to ultimately steep sidewalls and flat bottom morphologies (Figs. 1a and reach the target site. 2a). The reduction in the cratering efficiency as a result of the The LGG at JSC is fitted with a number of flapper valves, shock reverberation of the foil and plate leads to lower crater mechanical apertures, and a sabot catcher system that diameters than the predicted value (∼236 μm crater diameter) minimize the contamination so that only those projectiles that from the calibration plot by Kearsley et al.
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