Hypervelocity capture of meteoritic particles in nonsilica aerogels

Abstract– The Stardust mission captured particles from the comet 81P/Wild 2 in gradient density silica aerogel and returned the collected samples to earth in 2006. The analyses of these particles have revealed several new insights into the formation of our solar system. However, since the aerogel used as the capture material was silica, the elemental analyses of the silica‐rich particles were made more complicated in certain ways due to the mixing of the silicon of the particles and that of the aerogel. By using a nonsilica aerogel, future elemental analyses of silica–rich particles captured in aerogel could be made more straightforward. Resorcinol/formaldehyde (RF), alumina, and zirconia aerogels were impact tested with meteoritic fragments and the captured fragments were mapped with synchrotron‐based X‐ray microprobe (XRM) and the particles were analyzed with X‐ray fluorescence (XRF). The resorcinol/formaldehyde aerogel proved to be the best capture material, in that it could be keystoned and XRF could be used to locate and analyze particles that were less than 10 μm.     

Capture of particles in hypervelocity impacts in aerogel

Abstract— The capture in aerogel of 106 μm diameter glass beads is investigated for impact speeds of 1 to 7.5 km s^?1. Three different aerogel densities were used, 60,96 and 180 kg m^?3. It was found that the length of the penetration track in the aerogel increases with speed until a maximum is reached. Above the maximum speed the track length decreases. This behaviour is similar to that which has previously been observed for particles impacting polystyrene foams and porous alumina. Whilst track length was not found to be an unambiguous indicator of impact speed, the excavated track volume was found to be a suitable indictor of speed. Further, it was possible to estimate the original particle size by measurements of the track volume and entrance hole size. In addition sub‐100 μm diameter particles composed of various minerals were fired into aerogel and the characterisation of the particles in situ by use of a Raman spectrometer was evaluated. This was found to work well, giving vibrational spectra essentially similar to those of the bulk minerals, thus providing a mineralogical rather than an elemental signature for the captured particles.     

Extent of thermal ablation suffered by model organic microparticles during aerogel capture at hypervelocities

Abstract— New model organic microparticles are used to assess the thermal ablation that occurs during aerogel capture at speeds from 1 to 6 km s^?1. Commercial polystyrene particles (20 μm diameter) were coated with an ultrathin 20 nm overlayer of an organic conducting polymer, polypyrrole. This overlayer comprises only 0.8% by mass of the projectile but has a very strong Raman signature, hence its survival or destruction is a sensitive measure of the extent of chemical degradation suffered. After aerogel capture, microparticles were located via optical microscopy and their composition was analyzed in situ using Raman microscopy. The ultrathin polypyrrole overlayer survived essentially intact for impacts at ～1 km s^?1, but significant surface carbonization was found at 2 km s^?1, and major particle mass loss at ≥3 km s^?1. Particles impacting at ～6.1 km s^?1 (the speed at which cometary dust was collected in the NASA Stardust mission) were reduced to approximately half their original diameter during aerogel capture (i.e., a mass loss of 84%). Thus significant thermal ablation occurs at speeds above a few km s^?1. This suggests that during the Stardust mission the thermal history of the terminal dust grains during capture in aerogel may be sufficient to cause significant processing or loss of organic materials. Further, while Raman D and G bands of carbon can be obtained from captured grains, they may well reflect the thermal processing during capture rather than the pre‐impact particle's thermal history.     

Raman spectroscopic investigation of two grains from comet 81P/Wild 2: Information that can be obtained beyond the presence of sp2‐bonded carbon

Abstract– Raman analyses were performed of individual micrometer‐sized fragments of material returned to Earth by the NASA Stardust mission to comet 81P/Wild 2. The studied fragments originated from grains (C2054,0,35,91,0 and C2092,6,80,51,0) of two different penetration tracks that occurred in two different silica aerogel collector cells. All fragments of both particles have Raman spectra characteristic of amorphous sp²‐bonded carbon that are in general agreement with the results published in previous Stardust particle studies. The present study, however, does not focus on the discussion of specific details of the D and G band parameters, but rather reports on additional information that can be obtained from returned Stardust samples via Raman spectroscopy. Most notably, the Raman spectra show that all analyzed fragments of the particles were contaminated with the capture medium (i.e., aerogel). The silica aerogel is laced with organic aliphatic and aromatic hydrocarbon impurities that resulted in strong bands in the ～ 2900 Δcm^?1 spectral range (C‐H stretching modes). Aerogel bands are also found in the 1000–1600 Δcm^?1 spectral range, where they overlap with the bands of the amorphous sp²‐bonded carbon. The peaks associated with the aerogel contamination differ between the two grains that originated from two different aerogel cells. In addition to the bands due to aerogel contamination and the always present sp²‐bonded carbon bands, fragments of particle C2092,6,80,51,0 also show Raman peaks for pyrrhotite and Fa₃₀Fo₇₀ olivine. Complete (up to 4000 Δcm^?1) raw and baseline‐corrected Raman spectra of the Stardust particles are shown and discussed in detail.     

Capture effects in carbonaceous material: A Stardust analogue study

Abstract— It is reasonable to expect that cometary samples returned to Earth by the Stardust space probe have been altered to some degree during capture in aerogel at 6.1 km/s. In order to help interpret the measured structure of these particles with respect to their original cometary nature, a series of coal samples of known structure and chemical composition was fired into aerogel at Stardust capture velocity. This portion of the study analyzed the surfaces of aerogel‐embedded particles using Raman spectroscopy. Results show that particle surfaces are largely homogenized during capture regardless of metamorphic grade or chemical composition, apparently to include a devolatilization step during capture processing. This provides a possible mechanism for alteration of some aliphatic compound‐rich phases through devolatilization of cometary carbonaceous material followed by re‐condensation within the particle. Results also show that the possibility of alteration must be considered for any particular Stardust grain, as examples of both graphitization and amorphization are found in the coal samples. It is evident that Raman G band (～1580 cm^?1) parameters provide a means of characterizing Stardust carbonaceous material to include identifying those grains which have been subjected to significant capture alteration.     

Two refractory Wild 2 terminal particles from a carrot‐shaped track characterized combining MIR/FIR/Raman microspectroscopy and FE‐SEM/EDS analyses

We present the analyses results of two bulk Terminal Particles, C2112,7,171,0,0 and C2112,9,171,0,0, derived from the Jupiter‐family comet 81P/Wild 2 returned by the Stardust mission. Each particle embedded in a slab of silica aerogel was pressed in a diamond cell. This preparation, as expected, made it difficult to identify the minerals and organic materials present in these particles. This problem was overcome using a combination of three different analytical techniques, viz. FE‐SEM/EDS, IR, and Raman microspectroscopy that allowed identifying the minerals and small amounts of amorphous carbon present in both particles. TP2 and TP3 were dominated by Ca‐free and low‐Ca, Mg‐rich, Mg,Fe‐olivine. The presence of melilite in both particles is supported by IR microspectroscopy, but is not confirmed by Raman microspectroscopy, possibly because the amounts are too small to be detected. TP2 and TP3 show similar silicate mineral compositions, but Ni‐free and low‐Ni, subsulfur (Fe,Ni)S grains are present in TP2 only. TP2 contains indigenous amorphous carbon hot spots; no indigenous carbon was identified in TP3. These nonchondritic particles probably originated in a differentiated body. This work found an unanticipated carbon contamination following the FE‐SEM/EDS analyses. It is suggested that organic materials in the embedding silica aerogel are irradiated during FE‐SEM/EDS analyses creating a carbon gas that develops a strong fluorescence continuum. The combination of the selected analytical techniques can be used to characterize bulk Wild 2 particles without the need of extraction and removal of the encapsulating aerogel. This approach offers a relatively fast sample preparation procedure, but compressing the samples can cause spurious artifacts, viz. silica contamination. Because of the combination of techniques, we account for these artifacts.     

Three‐dimensional textural and compositional analysis of particle tracks and fragmentation history in aerogel

Abstract— We report analyses of aerogel tracks using (1) synchrotron X‐ray computed microtomography (XRCMT), (2) laser confocal scanning microscopy (LCSM), and (3) synchrotron radiation X‐ray fluorescence (SRXRF) of particles and their paths resulting from simulated hypervelocity impacts (1–2), and a single ～1 mm aerogel track from the Stardust cometary sample collector (1–3). Large aerogel pieces can be imaged sequentially, resulting in high spatial resolution images spanning many tomographic fields of view (‘lambda‐tomography’). We report calculations of energy deposited, and tests on aromatic hydrocarbons showing no alteration in tomography experiments. Imaging at resolutions from ～17 to ～1 micron/pixel edge (XRCMT) and to <100 nm/pixel edge (LCSM) illustrates track geometry and interaction of particles with aerogel, including rifling, particle fragmentation, and final particle location. We present a 3‐D deconvolution method using an estimated point‐spread function for aerogel, allowing basic corrections of LCSM data for axial distortion. LCSM allows rapid, comprehensive, non‐destructive, high information return analysis of tracks in aerogel keystones, prior to destructive grain extraction. SRXRF with LCSM allows spatial correlation of grain size, chemical, and mineralogical data. If optical methods are precluded in future aerogel capture missions, XRCMT is a viable 3D imaging technique. Combinations of these methods allow for complete, nondestructive, quantitative 3‐D analysis of captured materials at high spatial resolution. This data is fundamental to understanding the hypervelocity particle‐aerogel interaction histories of Stardust grains.     

Correlated microanalysis of cometary organic grains returned by Stardust

Abstract– Carbonaceous matter in Stardust samples returned from comet 81P/Wild 2 is observed to contain a wide variety of organic functional chemistry. However, some of this chemical variety may be due to contamination or alteration during particle capture in aerogel. We investigated six carbonaceous Stardust samples that had been previously analyzed and six new samples from Stardust Track 80 using correlated transmission electron microscopy (TEM), X‐ray absorption near‐edge structure spectroscopy (XANES), and secondary ion mass spectroscopy (SIMS). TEM revealed that samples from Track 35 containing abundant aliphatic XANES signatures were predominantly composed of cometary organic matter infilling densified silica aerogel. Aliphatic organic matter from Track 16 was also observed to be soluble in the epoxy embedding medium. The nitrogen‐rich samples in this study (from Track 22 and Track 80) both contained metal oxide nanoparticles, and are likely contaminants. Only two types of cometary organic matter appear to be relatively unaltered during particle capture. These are (1) polyaromatic carbonyl‐containing organic matter, similar to that observed in insoluble organic matter (IOM) from primitive meteorites, interplanetary dust particles (IDPs), and in other carbonaceous Stardust samples, and (2) highly aromatic refractory organic matter, which primarily constitutes nanoglobule‐like features. Anomalous isotopic compositions in some of these samples also confirm their cometary heritage. There also appears to be a significant labile aliphatic component of Wild 2 organic matter, but this material could not be clearly distinguished from carbonaceous contaminants known to be present in the Stardust aerogel collector.     

Magnetite in Comet Wild 2: Evidence for parent body aqueous alteration

The mineralogy of comet 81P/Wild 2 particles, collected in aerogel by the Stardust mission, has been determined using synchrotron Fe‐K X‐ray absorption spectroscopy with in situ transmission XRD and X‐ray fluorescence, plus complementary microRaman analyses. Our investigation focuses on the terminal grains of eight Stardust tracks: C2112,4,170,0,0; C2045,2,176,0,0; C2045,3,177,0,0; C2045,4,178,0,0; C2065,4,187,0,0; C2098,4,188,0,0; C2119,4,189,0,0; and C2119,5,190,0,0. Three terminal grains have been identified as near pure magnetite Fe₃O₄. The presence of magnetite shows affinities between the Wild 2 mineral assemblage and carbonaceous chondrites, and probably resulted from hydrothermal alteration of the coexisting FeNi and ferromagnesian silicates in the cometary parent body. In order to further explore this hypothesis, powdered material from a CR2 meteorite (NWA 10256) was shot into the aerogel at 6.1 km s^?1, using a light‐gas gun, and keystones were then prepared in the same way as the Stardust keystones. Using similar analysis techniques to the eight Stardust tracks, a CR2 magnetite terminal grain establishes the likelihood of preserving magnetite during capture in silica aerogel.     

Macroscopic subdivision of silica aerogel collectors for sample return missions

Abstract— Silica aerogel collector tiles have been employed for the collection of particles in low Earth orbit and, more recently, for the capture of cometary particles by NASA's Stardust mission. Reliable, reproducible methods for cutting these and future collector tiles from sample return missions are necessary to maximize the science output from the extremely valuable embedded particles. We present a means of macroscopic subdivision of collector tiles by generating large‐scale cuts over several centimeters in silica aerogel with almost no material loss. The cut surfaces are smooth and optically clear allowing visual location of particles for analysis and extraction. This capability is complementary to the smaller‐scale cutting capabilities previously described (Westphal 2004; Ishii 2005a, 2005b) for removing individual impacts and particulate debris in tiny aerogel extractions. Macroscopic cuts enable division and storage or distribution of portions of aerogel tiles for immediate analysis of samples by certain techniques in situ or further extraction of samples suited for other methods of analysis. The capability has been implemented in the Stardust Laboratory at NASA's Johnson Space Center as one of a suite of aerogel cutting methods to be used in Stardust sample curation.     

Microstructure modifications of silicates induced by the collection in aerogel: Experimental approach and comparison with Stardust results

Abstract– Particles from comet 81P/Wild 2 were captured with silica aerogel during the flyby Stardust mission. A significant part of the collection was damaged during the impact at hypervelocity in the aerogel. In this study, we conducted impact experiments into aerogel of olivine and pyroxene powder using a light‐gas gun in similar conditions as that of the comet Wild 2 particles collection. The shot samples were investigated using transmission electron microscopy to characterize their microstructure. Both olivine and pyroxene samples show evidence of thermal alteration due to friction with the aerogel. All the grains have rounded edges after collection, whereas their shape was angular in the initial shot powder set. This is probably associated with mass loss of particles. The rims of the grains are clearly melted and mixed with aerogel. The core of olivine grains is fairly well preserved, but some grains contain dislocations in glide configuration. We interpret these dislocations as generated by the thermal stresses that have emerged due to the high temperature gradients between the core and the rim of the grains. Most of the pyroxene grains have been fully melted. Their high silica concentration reflects a strong impregnation with melted aerogel. The preferential melting of pyroxene compared with olivine is due to a difference in melting temperatures of 300°. This melting point difference probably induces a bias in the measurements of the ratio olivine/pyroxene in the Wild 2 comet. The proportion of pyroxene was probably higher on Wild 2 than expected from the samples collected into aerogel.     

Rapid extraction of dust impact tracks from silica aerogel by ultrasonic microblades

Abstract— In January 2006, NASA's Stardust mission will return with its valuable cargo of the first cometary dust particles captured at hypervelocity speeds in silica aerogel collectors and brought back to Earth. Aerogel, a proven capture medium, is also a candidate for future sample return missions and low‐Earth orbit (LEO) deployments. Critical to the science return of Stardust as well as future missions that will use aerogel is the ability to efficiently extract impacted particles from collector tiles. Researchers will be eager to obtain Stardust samples as quickly as possible; tools for the rapid extraction of particle impact tracks that require little construction, training, or investment would be an attractive asset. To this end, we have experimented with diamond and steel microblades. Applying ultrasonic frequency oscillations to these microblades via a piezo‐driven holder produces rapid, clean cuts in the aerogel with minimal damage to the surrounding collector tile. With this approach, intact impact tracks and associated particles in aerogel fragments with low‐roughness cut surfaces have been extracted from aerogel tiles flown on NASA's Orbital Debris Collector (ODC) experiment. The smooth surfaces produced during cutting reduce imaging artifacts during analysis by scanning electron microscopy (SEM). Some tracks have been dissected to expose the main cavity for eventual isolation of individual impact debris particles and further analysis using techniques such as transmission electron microscopy (TEM) and nano‐secondary ion mass spectrometry (nanoSIMS).     

Properties of original impactors estimated from three‐dimensional analysis of whole Stardust tracks

Abstract– The Stardust mission captured comet Wild 2 particles in aerogel at 6.1 km s^?1. We performed high‐resolution three‐dimensional imaging and X‐ray fluorescence mapping of whole cometary tracks in aerogel. We present the results of a survey of track structures using laser scanning confocal microscopy, including measurements of track volumes, entry hole size, and cross‐sectional profiles. We compare various methods for measuring track parameters. We demonstrate a methodology for discerning hypervelocity particle ablation rates using synchrotron‐based X‐ray fluorescence, combined with mass and volume estimates of original impactors derived from measured track properties. Finally, we present a rough framework for reconstruction of original impactor size, and volume of volatilized material, using our measured parameters. The bulk of this work is in direct support of nondestructive analysis and identification of cometary grains in whole tracks, and its eventual application to the reconstruction of the size, shape, porosity, and chemical composition of whole Stardust impactors.     

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).     

Thermal alteration of hydrated minerals during hypervelocity capture to silica aerogel at the flyby speed of Stardust

Abstract— Outside the Earth's atmosphere, silica aerogel is one of the best materials to capture finegrained extraterrestrial particles in impacts at hypervelocities. Because silica aerogel is a superior insulator, captured grains are inevitably influenced by frictional heat. Therefore, we performed laboratory simulations of hypervelocity capture by using light‐gas guns to impact into aerogels finegrained powders of serpentine, cronstedtite, and Murchison CM2 meteorite. The samples were shot at >6 km s^?1 similar to the flyby speed at comet P/Wild‐2 in the Stardust mission. We investigated mineralogical changes of each captured particle by using synchrotron radiation X‐ray diffraction (SR‐XRD), transmission electron microscope (TEM), and field emission scanning electron microscope (FE‐SEM). SR‐XRD of each grain showed that the majority of the bulk grains keep their original mineralogy. In particular, SR‐XRD and TEM investigations clearly exemplified the presence of tochilinite whose decomposition temperature is about 300 °C in the interior of the captured Murchison powder. However, TEM study of these grains also revealed that all the samples experienced melting and vesiculation on the surface. The cronstedtite and the Murchison meteorite powder show remarkable fracturing, disaggregation, melting, and vesiculation. Steep thermal gradients, about 2500 °C/μm were estimated near the surface of the grains (<2 μm thick) by TEM observation. Our data suggests that the interior of >4 μm across residual grains containing abundant materials that inhibit temperature rise would have not experienced >300 °C at the center.     

Fine‐grained material of 81P/Wild 2 in interaction with the Stardust aerogel

Abstract– The deceleration tracks in the Stardust aerogel display a wide range of morphologies, which reveal a large diversity of incoming particles from comet 81P/Wild 2. If the large and dense mineral grains survived the extreme conditions of hypervelocity capture, this was not the case for the fine‐grained material that is found strongly damaged within the aerogel. Due to their low mechanical strength, these assemblages were disaggregated, dispersed, and flash melted in the aerogel in walls of bulbous deceleration tracks. Their petrologic and mineralogical properties are found significantly modified by the flash heating of the capture. Originating from a quenched melt mixture of comet material and aerogel, the representative microstructure consists of silica‐rich glassy clumps containing Fe‐Ni‐S inclusions, vesicles and “dust‐rich” patches, the latter being remnants of individual silicate components of the impacting aggregate. The average composition of these melted particle fragments is close to the chondritic CI composition. They might originate from ultrafine‐grained primitive components comparable to those found in chondritic porous IDPs. Capture effects in aerogel and associated sample biases are discussed in terms of size, chemical and mineralogical properties of the grains. These properties are essential for the grain survival in the extremely hot environment of hypervelocity impact capture in aerogel, and thus for inferring the correct properties of Wild 2 material.     

Small hypervelocity particles captured in aerogel collectors: Location,extraction, handling and storage

Abstract— It has now been about a decade since the first demonstrations that hypervelocity particles could be captured, partially intact, in aerogel collectors. But the initial promise of a bonanza of partially‐intact extraterrestrial particles, collected in space, has yet to materialize. One of the difficulties that investigators have encountered is that the location, extraction, handling and analysis of very small (10 μm and less) grains, which constitute the vast majority of the captured particles, is challenging and burdensome. Furthermore, current extraction techniques tend to be destructive over large areas of the collectors. Here we describe our efforts to alleviate some of these difficulties. We have learned how to rapidly and efficiently locate captured particles in aerogel collectors, using an automated microscopic scanning system originally developed for experimental nuclear astrophysics. We have learned how to precisely excavate small access tunnels and trenches using an automated micromanipulator and glass microneedles as tools. These excavations are only destructive to the collector in a very small area—this feature may be particularly important for excavations in the precious Stardust collectors. Using actuatable silicon microtweezers, we have learned how to extract and store “naked” particles—essentially free of aerogel—as small as 3 μm in size. We have also developed a technique for extracting particles, along with their terminal tracks, still embedded in small cubical aerogel blocks. We have developed a novel method for storing very small particles in etched nuclear tracks. We have applied these techniques to the extraction and storage of grains captured in aerogel collectors (Particle Impact Experiment, Orbital Debris Collector Experiment, Comet‐99) in low Earth orbit.     

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.     

A cometary aggregate interplanetary dust particle as an analog for comet Wild 2 grain chemistry preserved in silica‐rich Stardust glass

Abstract— Many of the nanometer‐scale grains from comet 81P/Wild 2 did not survive hypervelocity capture. Instead, they melted and interacted with silica melt derived from the aerogel used by the Stardust mission. Their petrological properties were completely modified, but their bulk chemistry was preserved in the chemical signatures of mostly vesicular Si‐rich glass with its typical Fe‐Ni‐S compound inclusions. Chondritic aggregate IDP L2011A9 that experienced atmospheric pre‐entry thermal modification was selected as an analog to investigate these Wild 2 chemical signatures. The chemical, petrologic, and mineralogical properties of the individual constituents in this aggregate IDP are presented and used to match the chemical signatures of these Wild 2 grains. Mixing of comet material and pure silica, which is used in a diagram that recognizes this mixing behavior, is used to constrain the probable petrologic and minerals that caused the Wild 2 signatures. The Wild 2 nanometer‐scale grain signatures in Si‐rich glass allocations from three different deceleration tracks resembled mixtures of ultrafine‐grained principal components and dense agglomerate‐like material, Mg‐rich silicates (<500 nm) and Fe,Ni‐sulfides (<100 nm), and Si‐rich amorphous material. Dust resembling the mixed matrix of common chondritic aggregate IDPs was present in Jupiter‐family comet Wild 2.     

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.