Analytical scanning and transmission electron microscopy of laboratory impacts on Stardust aluminum foils: Interpreting impact crater morphology and the composition of impact residues

Abstract— The known encounter velocity (6.1 kms^?1) and particle incidence angle (perpendicular) between the Stardust spacecraft and the dust emanating from the nucleus of comet Wild‐2 fall within a range that allows simulation in laboratory light‐gas gun (LGG) experiments designed to validate analytical methods for the interpretation of dust impacts on the aluminum foil components of the Stardust collector. Buckshot of a wide size, shape, and density range of mineral, glass, polymer, and metal grains, have been fired to impact perpendicularly on samples of Stardust Al 1100 foil, tightly wrapped onto aluminum alloy plate as an analogue of foil on the spacecraft collector. We have not yet been able to produce laboratory impacts by projectiles with weak and porous aggregate structure, as may occur in some cometary dust grains. In this report we present information on crater gross morphology and its dependence on particle size and density, the pre‐existing major‐ and trace‐element composition of the foil, geometrical issues for energy dispersive X‐ray analysis of the impact residues in scanning electron microscopes, and the modification of dust chemical composition during creation of impact craters as revealed by analytical transmission electron microscopy. Together, these observations help to underpin the interpretation of size, density, and composition for particles impacted on the Stardust aluminum foils.     

Comet 81P/Wild 2: The size distribution of finer (sub‐10 μm) dust collected by the Stardust spacecraft

Abstract– The fluence of dust particles <10 μm in diameter was recorded by impacts on aluminum foil of the NASA Stardust spacecraft during a close flyby of comet 81P/Wild 2 in 2004. Initial interpretation of craters for impactor particle dimensions and mass was based upon laboratory experimental simulations using projectiles less than >10 μm in diameter and the resulting linear relationship of projectile to crater diameter was extrapolated to smaller sizes. We now describe a new experimental calibration program firing very small monodisperse silica projectiles (470 nm–10 μm) at approximately 6 km s^?1. The results show an unexpected departure from linear relationship between 1 and 10 μm. We collated crater measurement data and, where applicable, impactor residue data for 596 craters gathered during the postmission preliminary examination phase. Using the new calibration, we recalculate the size of the particle responsible for each crater and hence reinterpret the cometary dust size distribution. We find a greater flux of small particles than previously reported. From crater morphology and residue composition of a subset of craters, the internal structure and dimensions of the fine dust particles are inferred and a “maximum‐size” distribution for the subgrains composing aggregate particles is obtained. The size distribution of the small particles derived directly from the measured craters peaks at approximately 175 nm, but if this is corrected to allow for aggregate grains, the peak in subgrain sizes is at <100 nm.     

Focused ion beam recovery of hypervelocity impact residue in experimental craters on metallic foils

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.     

Micron‐scale hypervelocity impact craters: Dependence of crater ellipticity and rim morphology on impact trajectory,projectile size,velocity, and shape

The interstellar collector on NASA's Stardust mission captured many particles from sources other than the interstellar dust stream. Impact trajectory may provide a means of discriminating between these different sources, and thus identifying/eliminating candidate interstellar particles. The collector's aerogel preserved a clear record of particle impact trajectory from the inclination and direction of the resultant tracks. However, the collector also contained aluminum foils and, although impact crater studies to date suggest only the most inclined impacts (>45° from normal) produce crater morphologies that indicate trajectory (i.e., distinctly elliptical), these studies have been restricted to much larger (mm and above) scales than are relevant for Stardust (μm). It is unknown how oblique impact crater morphology varies as a function of length scale, and therefore how well Stardust craters preserve details of impactor trajectory. Here, we present data from a series of impact experiments, together with complementary hydrocode modeling, that examine how crater morphology changes with impact angles for different‐sized projectiles. We find that, for our smallest spherical projectiles (2 μm diameter), the ellipticity and rim morphology provide evidence of their inclined trajectory from as little as 15° from normal incidence. This is most likely a result of strain rate hardening in the target metal. Further experiments and models find that variation in velocity and impactor shape complicate these trends, but that rim morphology remains useful in determining impact direction (where the angle of impact is >20° from normal) and may help identify candidate interstellar particle craters on the Stardust collector.     

Aerogel tracks made by impacts of glycine: Implications for formation of bulbous tracks in aerogel and the Stardust mission

Abstract– Impacts of small particles of soda‐lime glass and glycine onto low density aerogel are reported. The aerogel had a quality similar to the flight aerogels carried by the NASA Stardust mission that collected cometary dust during a flyby of comet 81P/Wild 2 in 2004. The types of track formed in the aerogel by the impacts of the soda‐lime glass and glycine are shown to be different, both qualitatively and quantitatively. For example, the soda‐lime glass tracks have a carrot‐like appearance and are relatively long and slender (width to length ratio <0.11), whereas the glycine tracks consist of bulbous cavities (width to length ratio >0.26). In consequence, the glycine particles would be underestimated in diameter by a factor of 1.7–3.2, if the glycine tracks were analyzed using the soda‐lime glass calibration and density. This implies that a single calibration for impacting particle size based on track properties, as previously used by Stardust to obtain cometary dust particle size, is inappropriate.     

FIB‐TEM analysis of cometary material in 10 Stardust foil craters

Aluminum foils from the Stardust cometary dust collector contain impact craters formed during the spacecraft's encounter with comet 81P/Wild 2 and retain residues that are among the few unambiguously cometary samples available for laboratory study. Our study investigates four micron‐scale (1.8–5.2 μm) and six submicron (220–380 nm) diameter craters to better characterize the fine (<1 μm) component of comet Wild 2. We perform initial crater identification with scanning electron microscopy, prepare the samples for further analysis with a focused ion beam, and analyze the cross sections of the impact craters with transmission electron microscopy (TEM). All of the craters are dominated by combinations of silicate and iron sulfide residues. Two micron‐scale craters had subregions that are consistent with spinel and taenite impactors, indicating that the micron‐scale craters have a refractory component. Four submicron craters contained amorphous residue layers composed of silicate and sulfide impactors. The lack of refractory materials in the submicron craters suggests that refractory material abundances may differentiate Wild 2 dust on the scale of several hundred nanometers from larger particles on the scale of a micron. The submicron craters are enriched in moderately volatile elements (S, Zn) when normalized to Si and CI chondrite abundances, suggesting that, if these craters are representative of the Wild 2 fine component, the Wild 2 fines were not formed by high‐temperature condensation. This distinguishes the comet's fine component from the large terminal particles in Stardust aerogel tracks which mostly formed in high‐temperature events.     

In situ analysis of residues resulting from laboratory impacts into aluminum 1100 foil: Implications for Stardust crater analyses

Abstract— The encounter between the Stardust spacecraft and particles from comet 81P/Wild 2 gave impacts at a relative velocity of 6.1 km s^?1 and near perpendicular incidence to the collector surface. Such conditions are well within the performance limits of light gas gun laboratory simulations. For this study, two series of shots were conducted at the University of Kent, firing magnesium silicates (Mg end‐member forsterite, enstatite, diopside and lizardite), followed by a suite of increasingly Ferich olivines (through to Fe end‐member fayalite) into Stardust flight‐spare foils. Preserved residues were analysed using scanning electron microscopy combined with energy dispersive X‐ray analyses (SEM/EDX). X‐ray count integrals show that mineral compositions remain distinct from one another after impact, although they do show increased scatter. However, there is a small but systematic increase in Mg relative to Si for all residues when compared to projectile compositions. While some changes in Mg: Si may be due to complex analytical geometries in craters, there appears to be some preferential loss of Si. In practice, EDX analyses in craters on Stardust Al 1100 foil inevitably include contributions from Fe‐ and Si‐rich alloy inclusions, leading to further scattering of element ratios. Such inclusions have complicated Mg: Fe data interpretation. Compositional heterogeneity in the synthetic olivine projectiles also introduces data spread. Nevertheless, even with the preceding caveats, we find that the main groups of mafic silicates can be easily and reliably distinguished in EDX analyses performed in rapid surveys of foil craters, enabling access to a valuable additional collection of cometary materials.     

Experimental investigation of impacts by solar cell secondary ejecta on silica aerogel and aluminum foil: Implications for the Stardust Interstellar Dust Collector

Abstract– We have shown in laboratory experiment that hypervelocity impacts on a solar cell produce ejecta that can be captured on aluminum (Al 1100) foil or in low density (33 kg m^?3) aerogel. The origin of the secondary impacts can be determined by either analysis of the residue in the craters in the foils (which preserve an elemental signature of the solar cell components) or by their pointing direction for tracks in the aerogel (which we show align with the impact direction to ± 0.4°). This experimental evidence explains the observations of the NASA Stardust mission which has reported that the majority of tracks in the aerogel collector used to collect interstellar dust actually point at the spacecraft’s solar panels. From our results, we suggest that it should also be possible to recognize secondary ejecta craters in the Stardust mission aluminum foils, also used as dust sampling devices during the mission.     

Preparation of large Stardust aluminum foil craters for analysis

Over the last decade, silica aerogel tracks and aluminum foil craters on the Stardust collector have been studied extensively to determine the nature of captured cometary dust grains. Analysis of particles captured in aerogel has been developed to a fine art, aided by sophisticated preparation techniques, and yielding revolutionary knowledge of comet dust mineralogy. The Stardust foil craters can be interpreted in terms of impacting particle size and structure, but almost all studies of composition for their contents have relied on in situ analysis techniques or relatively destructive extraction of materials. This has limited their examination and interpretation. However, numerous experimental hypervelocity impact studies under Stardust-Wild 2 encounter conditions have shown that abundant dust components are preserved in foil craters of all sizes. Using some of these analogue materials, we have previously shown that modern, nondestructive scanning electron microscope imaging and X-ray microanalysis techniques can document distribution of dust remnants both quickly and thoroughly within foil craters prior to any preparation. Here we present findings from our efforts to quantify the amount of residue and demonstrate a simple method of crater shape modification which can bring material into positions where it is much more accessible for in situ analysis, or safe removal of small subsamples. We report that approximately 50% of silicate-dominated impactors were retained as impact crater residue; however, <3% of organic impactors remained in the craters after impact.     

Energy loss and impact cratering in aerogels: theory and experiment

Aerogel collectors have been deployed in low-Earth orbit to collect orbital debris and micrometeorites. An array of silica aerogel collectors is currently en-route back to Earth following an encounter with the Comet Wild-2 on board the Stardust spacecraft. Stardust is returning, for laboratory analysis, cometary and interstellar dust grains which impacted into the aerogel collectors at hypervelocities. While the morphology of impact craters in aerogels has been studied empirically, a theoretical understanding of the physical mechanisms responsible for the formation of impact craters in these solids is lacking. Here we propose and test a model of compaction driven impact cratering in aerogels. Our model derives impact crater dimensions directly from energy and momentum deposition.     

SIMS studies of Allende projectiles fired into Stardust‐type aluminum foils at 6 km/sec

Abstract— We have explored the feasibility of C, N, and O isotopic measurements by NanoSIMS and of elemental abundance determinations by time‐of‐flight secondary ion mass spectrometry (TOF‐SIMS) on residues of Allende projectiles that impacted Stardust‐type aluminum foils in the laboratory at 6 km/sec. These investigations are part of a consortium study aimed at providing the foundation for the characterization of matter associated with microcraters that were produced during the encounter of the Stardust space probe with comet 81P/Wild‐2. Eleven experimental impact craters were studied by NanoSIMS and eighteen by TOF‐SIMS. Crater sizes were between 3 and 190 μm. The NanoSIMS measurements have shown that the crater morphology has only a minor effect on spatial resolution and on instrumental mass fractionation. The achievable spatial resolution is always better than 200 nm, and C and O isotopic ratios can be measured with a precision of several percent at a scale of several 100 nm, which is the typical size of presolar grains. This clearly demonstrates that presolar matter, provided it survives the impact into the aluminum foil partly intact, is recognizable even if embedded in material of solar system origin. TOF‐SIMS studies are restricted to materials from the crater rim. The element ratios of the major rock‐forming elements in the Allende projectiles are well‐characterized by the TOF‐SIMS measurements, indicating that fractionation of those elements during impact can be expected to be negligible. This permits chemical information on the type of impactor material to be obtained. For any more detailed assignments to specific chondrite groups, however, information on the abundances of the light elements, especially C, is crucial. This information could not be obtained in the present study due to unavoidable contamination during impact experiments.     

Organic compound alteration during hypervelocity collection of carbonaceous materials in aerogel

Abstract— The NASA Stardust mission brought to Earth micron‐size particles from the coma of comet 81P/Wild 2 using aerogel, a porous silica material, as the capture medium. A major challenge in understanding the organic inventory of the returned comet dust is identifying, unambiguously, which organic molecules are indigenous to the cometary particles, which are produced from carbon contamination in the Stardust aerogel, and which are cometary organics that have been modified by heating during the particle capture process. Here it is shown that 1) alteration of cometary organic molecules along impact tracks in aerogel is highly dependent on the original particle morphology, and 2) organic molecules on test‐shot terminal particles are mostly preserved. These conclusions are based on two‐step laser mass spectrometry (L²MS) examinations of test shots with organic‐laden particles (both tracks in aerogel and the terminal particles themselves).     

Exposure and analysis of microparticles embedded in silica aerogel keystones using NF3‐mediated electron beam–induced etching and energy‐dispersive X‐ray spectroscopy

In 2006, NASA's Stardust spacecraft delivered to Earth dust particles collected from the coma of comet 81P/Wild 2, with the goal of furthering the understanding of solar system formation. Stardust cometary samples were collected in a low‐density, nanoporous silica aerogel making their study technically challenging. This article demonstrates the identification, exposure, and elemental composition analysis of particles analogous to those collected by NASA's Stardust mission using in‐situ SEM techniques. Backscattered electron imaging is shown by experimental observation and Monte Carlo simulation to be suitable for locating particles of a range of sizes relevant to Stardust (down to submicron diameters) embedded within silica aerogel. Selective removal of the silica aerogel encapsulating an embedded particle is performed by cryogenic NF₃‐mediated electron beam–induced etching. The porous, low‐density nature of the aerogel results in an enhanced etch rate compared with solid material, making it an effective, nonmechanical method for the exposure of particles. After exposure, elemental composition of the particle was analyzed by energy‐dispersive X‐ray spectroscopy using a high spectral resolution microcalorimeter. Signals from fluorine contamination are shown to correspond to nonremoved silica aerogel and only in residual concentrations.     

Interpretation of Wild 2 dust fine structure: Comparison of Stardust aluminum foil craters to the three‐dimensional shape of experimental impacts by artificial aggregate particles and meteorite powders

Abstract— New experimental results show that Stardust crater morphology is consistent with interpretation of many larger Wild 2 dust grains being aggregates, albeit most of low porosity and therefore relatively high density. The majority of large Stardust grains (i.e. those carrying most of the cometary dust mass) probably had density of 2.4 g cm^?3 (similar to soda‐lime glass used in earlier calibration experiments) or greater, and porosity of 25% or less, akin to consolidated carbonaceous chondrite meteorites, and much lower than the 80% suggested for fractal dust aggregates. Although better size calibration is required for interpretation of the very smallest impacting grains, we suggest that aggregates could have dense components dominated by μm‐scale and smaller sub‐grains. If porosity of the Wild 2 nucleus is high, with similar bulk density to other comets, much of the pore space may be at a scale of tens of micrometers, between coarser, denser grains. Successful demonstration of aggregate projectile impacts in the laboratory now opens the possibility of experiments to further constrain the conditions for creation of bulbous (Type C) tracks in aerogel, which we have observed in recent shots. We are also using mixed mineral aggregates to document differential survival of pristine composition and crystalline structure in diverse finegrained components of aggregate cometary dust analogues, impacted onto both foil and aerogel under Stardust encounter conditions.     

Morphology of craters generated by hypervelocity impacts of micron‐sized polypyrrole‐coated olivine particles

To understand the process of cosmic dust particle impacts and translate crater morphology on smoothed metallic surfaces to dust properties, correct calibration of the experimental impact data is needed. This article presents the results of studies of crater morphology generated by impacts using micron‐sized polypyrrole (PPy)‐coated olivine particles. The particles were accelerated by an electrostatic dust accelerator to high speeds before they impacted onto polished aluminum targets. The projectile diameter and velocity ranges were 0.3–1.2 μm and 3–7 km s^?1. After impact, stereopair images of the craters were taken using scanning electron microscope and 3‐D reconstructions made to provide diameter and depth measurements. In this study, not just the dimensions of crater diameters and depths, but also the shape and dimensions of crater lips were analyzed. The craters created by the coated olivine projectiles are shown to have complicated shapes believed to be due to the nonspherical shape of the projectiles.     

Automated searching of Stardust interstellar foils

Abstract– The Al foils lining the aerogel tiles of the Stardust interstellar tray represent approximately 13% of the total collecting area, about 15,300 mm². Although the flux is poorly constrained, fewer than 100 impacts are expected in all the Al foils on the collector, and most of these are likely to be less than 1 μm in diameter. Secondary electron (SE) images of the foils at a resolution of approximately 50 nm per pixel are being collected during the Stardust Interstellar Preliminary Examination, resulting in more than two million images that will eventually need to be searched for impact craters. The unknown and complicated nature of 3‐dimensional interstellar tracks in aerogel necessitated the use of a massively distributed human search to locate only a few interstellar tracks. The 2‐dimensional nature of the SE images makes the problem of searching for craters tractable for algorithmic approaches. Using templates of craters from cometary impacts into Stardust foils, we present a computer algorithm for the identification of impact craters in the Stardust interstellar foils using normalized cross‐correlation and template matching. We address the speed, sensitivity, and false‐positive rate of the algorithm. The search algorithm can be adapted for use in other applications. The program is freely available for download at http://jake.ssl.berkeley.edu:8000/groups/westphalgroup/wiki/14e52/ISPE_SEM_Crater_Search.html .     

Infrared spectroscopy of Wild 2 particle hypervelocity tracks in Stardust aerogel: Evidence for the presence of volatile organics in cometary dust

Abstract— Infrared spectroscopy maps of some tracks made by cometary dust from 81P/Wild 2 impacting Stardust aerogel reveal an interesting distribution of organic material. Out of six examined tracks, three show presence of volatile organic components possibly injected into the aerogel during particle impacts. When particle tracks contained volatile organic material, they were found to be ‐CH₂‐rich, while the aerogel is dominated by the ‐CH₃‐rich contaminant. It is clear that the population of cometary particles impacting the Stardust aerogel collectors also includes grains that contained little or none of this organic component. This observation is consistent with the highly heterogeneous nature of collected grains, as seen by a multitude of other analytical techniques.     

TOF‐SIMS analysis of Allende projectiles shot into silica aerogel

Abstract— Powdered Allende projectiles were fired into silica aerogel at 6.1 km/sec in order to evaluate particle retrieval and analysis techniques for samples from the Stardust mission. Since particles may disintegrate and ablate along the penetration paths in a high‐porosity aerogel, TOF‐SIMS analysis may be a suitable method to determine the distribution of such materials along the tracks as well as potential compositional modifications. Therefore, two ?350 μm‐sized tracks, residing at the surface of a keystone specimen that was flattened between two silicon chips, were analyzed. TOF‐SIMS allows for a detailed study of the chemical composition of particles that survived the impact mostly intact and of fine‐grained material from disintegrated projectiles. In the investigated keystone, material from light gas gun debris dominated. Besides the two tracks, a continuous, 40‐μm‐thick surface layer of implanted material—probably gun residue—was found. One of the two analyzed tracks is compositionally distinct from this surface layer and is likely to contain residual material of an Allende projectile. The analyses clearly demonstrate that tracks, resulting from impactors in the 5–10 μm size range, can be successfully analyzed with TOF‐SIMS.     

Fine‐grained material associated with a large sulfide returned from Comet 81P/Wild 2

In a consortium analysis of a large particle captured from the coma of comet 81P/Wild 2 by the Stardust spacecraft, we report the discovery of a field of fine‐grained material (FGM) in contact with a large sulfide particle. The FGM was partially located in an embayment in the sulfide. As a consequence, some of the FGM appears to have been protected from damage during hypervelocity capture in aerogel. Some of the FGM particles are indistinguishable in their characteristics from common components of chondritic‐porous interplanetary dust particles, including glass with embedded metals and sulfides and equilibrated aggregates. The sulfide exhibits surprising Ni‐rich lamellae, which may indicate that this particle experienced a long‐duration heating event after its formation but before incorporation into Wild 2.     

Physical, Chemical, and Mineralogical Properties of Comet 81P/Wild 2 Particles Collected by Stardust

NASA’s Stardust spacecraft collected dust from the coma of Comet 81P/Wild 2 by impact into aerogel capture cells or into Al-foils. The first direct, laboratory measurement of the physical, chemical, and mineralogical properties of cometary dust grains ranging from <10⁻¹⁵ to ∼10⁻⁴ g were made on this dust. Deposition of material along the entry tracks in aerogel and the presence of compound craters in the Al-foils both indicate that many of the Wild 2 particles in the size range sampled by Stardust are weakly bound aggregates of a diverse range of minerals. Mineralogical characterization of fragments extracted from tracks indicates that most tracks were dominated by olivine, low-Ca pyroxene, or Fe-sulfides, although one track was dominated by refractory minerals similar to Ca–Al inclusions in primitive meteorites. Minor mineral phases, including Cu–Fe-sulfide, Fe–Zn-sulfide, carbonate and metal oxides, were found along some tracks. The high degree of variability of the element/Fe ratios for S, Ca, Ti, Cr, Mn, Ni, Cu, Zn, and Ga among the 23 tracks from aerogel capture cells analyzed during Stardust Preliminary Examination is consistent with the mineralogical variability. This indicates Wild 2 particles have widely varying compositions at the largest size analyzed (>10 μm). Because Stardust collected particles from several jets, sampling material from different regions of the interior of Wild 2, these particles are expected to be representative of the non-volatile component of the comet over the size range sampled. Thus, the stream of particles associated with Comet Wild 2 contains individual grains of diverse elemental and mineralogical compositions, some rich in Fe and S, some in Mg, and others in Ca and Al. The mean refractory element abundance pattern in the Wild 2 particles that were examined is consistent with the CI meteorite pattern for Mg, Si, Cr, Fe, and Ni to 35%, and for Ca, Ti and Mn to 60%, but S/Si and Fe/Si both show a statistically significant depletion from the CI values and the moderately volatile elements Cu, Zn, Ga are enriched relative to CI. This elemental abundance pattern is similar to that in anhydrous, porous interplanetary dust particles (IDPs), suggesting that, if Wild 2 dust preserves the original composition of the Solar Nebula, the anhydrous, porous IDPs, not the CI meteorites, may best reflect the Solar Nebula abundances. This might be tested by elemental composition measurements on cometary meteors.