Preparation of fine particles of astrophysical interest by gas evaporation techniques

Fine particles of various chemical substances—carbon, iron, iron oxide and silica—which are expected to exist in interstellar space are prepared in argon gas. The size, shape, and crystal structure of the powder particles are studied by electron microscopy and electron diffraction, and may have some bearing on models of comets and of the solar nebula.The largest size we have obtained is about 0.1 μm and the smallest about 40Å. Generally the size becomes smaller for lower temperature and also for lower pressure. This tendency is discussed in connection with nucleation theories. Except for iron and iron oxide the powder particles have no crystal structure.     

Low‐temperature phase decomposition in iron‐nickel metal of the Portales Valley meteorite

Abstract— The Portales Valley meteorite provides an opportunity to investigate and compare the microstructure in Fe‐Ni metal of the metallic particles in the chondritic portion and in the metal veins. The low‐temperature phase decomposition of Fe‐Ni metal was investigated using scanning electron microscopy, transmission electron microscopy, and atomic force microscopy. The microstructure is formed as the Portales Valley meteorite cooled from high temperatures and includes the outer taenite rim, the cloudy zone, clear taenite, and martensite. Martensite in turn decomposes into a fine admixture of fcc rods in a bcc matrix. The width of the island phase of the cloudy zone in the metal particles of the chondritic portion and the metal veins can be used to estimate a low‐temperature cooling rate. The microstructural evidence indicates that the chondritic portions and the metal veins in the Portales Valley meteorite cooled together as a mixture with a cooling rate of roughly 6.5 K/Ma.     

Properties of filamentary sublimation residues from dispersions of clay in ice

During vacuum sublimation experiments on simulated Martian polar deposits and cometary dirty ices, a fluffy filamentary sublimate residue material with unique physical properties was produced. The silica-to-silica bonds that we believe join the particles together are the result of conditions that may exist in some Martian polar deposits and on some cometary surfaces. Submicron particles of montmorillonite clay thinly dispersed (1: 1000 clay/water) and not contacting one another in water ice can form very-low-density structures (density as low as 10⁻³ g cm⁻³) during sublimation of the ice. The lightweight constructs, when viewed in scanning electron microscopy micrographs, are composed of long network chains of the clay particles. The material is sufficiently electrically conductive to drain away the scanning electron microscopy charge. It is also resistant (no change in electronic properties are apparent) to scanning electron microscopy electron-beam heating for hours in vacuo. Infrared spectra and X-ray diffraction patterns of the sublimate residues show little difference from spectra and patterns of the original minerals. Heating in an oven, in air, to 370°C produces little change in the structure of the sublimate residual material. The particle bonding forces are strong and produce a resilient, elastic lightweight material. The particle bonding will allow vapors to diffuse through it, and its thermal conductivity is very low. These properties produce a high-performance vacuum insulation. This material may have applications for insulating ice bodies (solid cryogens) in space. The incoming heat is partially carried away by the out-flowing water vapor.     

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).     

A TEM study of four particles extracted from the Stardust track 80

Abstract— Four particles extracted from track 80 at different penetration depths have been studied by analytical transmission electron microscopy (ATEM). Regardless of their positions within the track, the samples present a comparable microstructure made of a silica rich glassy matrix embedding a large number of small Fe‐Ni‐S inclusions and vesicles. This microstructure is typical of strongly thermally modified particles that were heated and melted during the hypervelocity impact into the aerogel. X‐ray intensity maps show that the particles were made of Mg‐rich silicates (typically 200 nm in diameter) cemented by a fine‐grained matrix enriched in iron sulfide. Bulk compositions of the four particles suggest that the captured dust particle was an aggregate of grains with various iron sulfide fraction and that no extending chemical mixing in the bulb occurred during the deceleration. The bulk S/Fe ratios of the four samples are close to CI and far from the chondritic meteorites from the asteroidal belt, suggesting that the studied particles are compatible with chondritic‐porous interplanetary dust particles or with material coming from a large heliocentric distance for escaping the S depletion.     

ON INVESTIGATING THE SHOCK HISTORY OF ATAXITES

It is suggested that transmission electron microscopy studies of ataxites and shock-loaded artificial nickel-iron alloys could develop criteria whereby the shock history of this class of meteorites might be established.     

Surface analysis of stratospheric dust particles

Abstract— A controversially discussed and yet central question in interplanetary dust particle (IDP) research is the degree of alteration of these particles during their residence in the stratosphere. Especially, the typical enrichment of Br in chondritic IDPs (on the average ～21 × CI) has been inferred to be a result of contamination processes, probably invoking aerosol droplets. With time-of-flight secondary ion mass spectrometry (TOF-SIMS), we examined the surfaces of 13 stratospheric particles from the dust collector U2071. Six particles had severe, surface-bound, silicone oil residues preventing a proper analysis of their surfaces. Six other particles—-according to our scanning electron microscopy, energy dispersive x-ray spectrometer (SEM-EDS) studies preclassified as one (Fe,Ni)S-rich IDP, one Ca-rich particle, and four aluminum-oxide spheres—-carry the halogens F, Cl, and Br on the surface. At least for the aluminum-oxide spheres, we provide unequivocal evidence for a surface correlation of halogens. This evidence, taken together with that from previous studies, proves a general stratospheric contamination process which has to be considered in IDP research.     

CLASSIFICATION OF A SECOND GROUP OF ORDINARY CHONDRITES FROM TEXAS

Based on optical microscopy and electron microprobe analyses of mafic minerals, six previously undescribed or poorly known ordinary chondrites from Texas were classified into compositional groups, petrologic types, and shock facies. These meteorites are Junction, L5d; Anton, H4b; Venus, H4d; Dalhart, H5a; Rosebud, H5c; and Cranfills Gap, H6c.     

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.     

Scanning electron microscopical and cross sectional analysis of extraterrestrial carbonaceous nanoglobules

Abstract— Carbonaceous nanoglobules are ubiquitous in carbonaceous chondrite (CC) meteorites. The Tagish Lake (C2) meteorite is particularly intriguing in containing an abundance of nanoglobules, with a wider range of forms and sizes than encountered in other CC meteorites. Previous studies by transmission electron microscopy (TEM) have provided a wealth of information on chemistry and structure. In this study low voltage scanning electron microscopy (SEM) was used to characterize the globule forms and external structures. The internal structure of the globules was investigated after sectioning by focused ion beam (FIB) milling. The FIB‐SEM analysis shows that the globules range from solid to hollow. Some hollow globules show a central open core, with adjoining smaller cores. The FIB with an SEM is a valuable tool for the analysis of extraterrestrial materials, even of sub‐micron‐sized “soft” carbonaceous particles. The rapid site‐specific cross‐sectioning capabilities of the FIB allow the preservation of the internal morphology of the nanoglobules, with minimal damage or alteration of the unsectioned areas.     

Laboratory annealing experiments of refractory silicate grain analogs using differential scanning calorimetry

Abstract– Exothermic reactions during the annealing of laboratory synthesized amorphous magnesium‐bearing silicate particles used as grain analogs of cosmic dust were detected by differential scanning calorimetry (DSC) in air. With infrared spectroscopy and transmission electron microscopy, we show that cosmic dust could possibly undergo fusion to larger particles, with oxidation of magnesium silicide and crystallization of forsterite as exothermic reactions in the early solar system. The reactions begin at approximately 425, approximately 625, and approximately 1000 K, respectively, and the reaction energies (enthalpies) are at least 727, 4151, and 160.22 J g⁻¹, respectively. During the crystallization of forsterite particles, the spectral evolution of the 10 μm feature from amorphous to crystalline was observed to begin at lower temperature than the crystallization temperature of 1003 K. During spectral evolution at lower temperature, nucleation and/or the formation of nanocrystallites of forsterite at the surface of the grain analogs was observed.     

MORPHOLOGIES OF IRON CRYSTALS FROM THE HAVERÖ METEORITE

Studies of unpolished chips of the Haverö meteorite using the scanning electron microscope (SEM) and the electron microprobe (EMP), show two types of metallic iron particles: A, discrete convex globules of 5 to 50 microns made up of lamellae and interlocked grains, evenly interspersed among the matrix; B, flattened contorted crystals, less than one micron, lining the iron globules and cavities in the silicates or forming rounded spiny bodies. This second type of iron is interpreted, according to the current theory, as resulting from the in situ reduction of iron-magnesium silicates     

Pyroxenes microstructure in comet 81P/Wild 2 terminal Stardust particles

Abstract— We report the examination by transmission electron microscopy (TEM) of four Stardust terminal particles extracted from two neighboring tracks (32 an 69). The particles are made of well‐preserved crystalline grains dominated by low‐Ca pyroxene ranging from nearly pure enstatite to pigeonite. Some olivine grains are also found, in chemical equilibrium with the surrounding pyroxenes. Various microstructures are observed, as a function of the composition of the grains. They include (100)‐twinned pigeonite, clino/ortho domains in enstatite and exsolution in a Ca‐rich grain. The microstructures are mostly consistent with a formation by cooling from high‐temperature phases, which could be associated to igneous processes. Some dislocations in glide configuration are also present, probably attesting for small intensity shocks. Possible effects of the rapid heating/cooling stage and thermal shock associated to the collect are discussed. It appears that most of the microstructural features reported here are plausibly pristine.     

Diverse forms of primordial organic matter identified in interplanetary dust particles

Abstract– Coordinated in situ transmission electron microscopy and isotopic measurements of carbonaceous phases in interplanetary dust particles were performed to determine their origins. Five different types of carbonaceous materials were identified based on their morphology and texture, observed by transmission electron microscopy: globular, vesicular, dirty, spongy, and smooth. Flash heating experiments were performed to explore whether some of these morphologies are the result of atmospheric entry processes. Each of these morphologies was found to have isotopically anomalous H and N. Rare C isotopic anomalies were also observed. The isotopic and morphological properties of several of these phases, particularly the organic globules, are remarkably similar to those observed in other extraterrestrial materials including carbonaceous chondrites, comet 81P/Wild 2 particles collected by the Stardust spacecraft, and Antarctic micrometeorites, indicating that they were widespread in the early solar system. The ubiquitous nature and the isotopic anomalies of the nanoglobules and some other morphologies strongly suggest that these are very primitive phases. Given that some of the isotopic anomalies (D and ¹⁵N excesses) are indicative of mass fractionation chemical reactions in a very cold environment, and some others (¹³C and ¹⁵N depletions) have other origins, these carbonaceous phases come from different reservoirs. Whatever their origins, these materials probably reflect the first stages of the evolution of solar system organic matter, having originated in the outermost regions of the protosolar disk and/or interstellar cold molecular clouds.     

Evidence from scanning electron microscopy ofexperimental influences on the morphology of Triton andTitan tholins

To simulate experimentally the production of aerosols in the atmospheres of Titan andTriton, we have studied organic material (tholins) obtained by inductively coupled plasma fromCH₄ : N₂ gas mixtures, with ratios 10 : 90 for Titan simulations and 0.1 : 99.9 for Tritonsimulations. Observation of tholins by high performance scanning electron microscopy showsthat tholin morphology varies with the chemical composition of the initial gas mixture. Althoughthe role of the experimental design (especially the diameter of the discharge chamber) and theflux of matter were not fully investigated, it appears that they have a significant effect not on theoverall morphology of the tholins but on the size distribution of the particles.     

Microscopic search for the carrier phase Q of the trapped planetary noble gases in Allende,Leoville and Vigarano

Abstract— High‐resolution transmission electron microscopy micrographs of acid‐resistant residues of the Allende, Leoville, and Vigarano meteorites show a great variety of carbon structures: curved and frequently twisted and intertwined graphene sheets, abundant carbon black‐like particles, and hollow “sacs”. It is suggested that perhaps all of these are carriers for the planetary Q‐noble gases in these meteorites. Most of these materials are pyrocarbons that probably formed by the pyrolysis of hydrocarbons either in a gas phase, or on hot surfaces of minerals. An attempt was made to analyze for argon with particle‐induced x‐ray emission in 143 spots of grains of floating and suspended matter from freeze‐dry cycles of an Allende bulk sample in water, and floating “black balls” from sonication in water of samples from the Allende meteorite. The chemical compositions of these particles were obtained, but x‐ray signals at the wavelength of argon were obtained on only a few spots.     

CLASSIFICATION OF EIGHT ORDINARY CHONDRITES FROM TEXAS

Based on optical microscopy and electron microprobe analyses, eight previously undescribed or poorly known chondrites were classified into compositional groups, petrologic types, and degree of shock alteration. These chondrites are: Leander, L4b; Nazareth(a), L6d; La Villa, H4b; Mereta, H4c; Gail, H4d; Shafter Lake, H5a; Uvalde, H5d; and Howe, H5d.     

Acrylic embedding of Stardust particles encased in aerogel

Abstract— Ultramicrotomy of samples embedded in epoxy resin is a standard method for preparing ultra‐thin sections for electron microscopy. In this report we describe a new embedding technique that uses acrylic resin instead of epoxy. This method offers several important advantages for sectioning small extraterrestrial samples. One is that the acrylic resin is soluble and can be removed after ultramicrotomy to leave a sample that is free of the mounting media. This is important for studying carbon and insoluble organic components. A second major advantage of acrylic is that, when combined with pre‐embedding compression, it provides a very effective method of mounting samples collected in silica aerogel. Acrylic embedding is currently being used to mount comet particles collected by NASA's Stardust mission. Combined with a flattening process, the acrylic embedding and sectioning preserves all pieces of collected samples in their collection matrix. In addition to Stardust, acrylic may be applied to other samples collected in aerogel such as those from the Russian Mir space station (Hörz et al. 2000) and future missions such as Sample Collection for Investigation of Mars (SCIM) (Leshin 2003), a proposed mission to collect atmospheric dust particles from Mars.     

Nanophase iron carbides in fine‐grained rims in CM2 carbonaceous chondrites: Formation of organic material by Fischer–Tropsch catalysis in the solar nebula

Transmission electron microscope studies of fine‐grained rims in three CM2 carbonaceous chondrites, Y‐791198, Murchison, and ALH 81002, have revealed the presence of widespread nanoparticles with a distinctive core–shell structure, invariably associated with carbonaceous material. These nanoparticles vary in size from ~20 nm up to 50 nm in diameter and consist of a core of Fe,Ni carbide surrounded by a continuous layer of polycrystalline magnetite. These magnetite shells are 5–7 nm in thickness irrespective of the diameter of the core Fe,Ni carbide grains. A narrow layer of amorphous carbon a few nanometers in thickness is present separating the carbide core from the magnetite shell in all the nanoparticles observed. The Fe,Ni carbide phases that constitute the core are consistent with both haxonite and cohenite, based on electron diffraction data, energy dispersive X‐ray analysis, and electron energy loss spectroscopy. Z‐contrast scanning transmission electron microscopy shows that these core–shell magnetite‐carbide nanoparticles can occur as individual isolated grains, but more commonly occur in clusters of multiple particles. In addition, energy‐filtered transmission electron microscopy (EFTEM) images show that in all cases, the nanoparticles are embedded within regions of carbonaceous material or are coated with carbonaceous material. The observed nanostructures of the carbides and their association with carbonaceous material can be interpreted as being indicative of Fischer–Tropsch‐type (FTT) reactions catalyzed by nanophase Fe,Ni metal grains that were carburized during the catalysis reaction. The most likely environment for these FTT reactions appears to be the solar nebula consistent with the high thermal stability of haxonite and cohenite, compared with other carbides and the evidence of localized catalytic graphitization of the carbonaceous material. However, the possibility that such reactions occurred within the CM parent body cannot be excluded, although this scenario seems unlikely, because the kinetics of the reaction would be extremely slow at the temperatures inferred for CM asteroidal parent bodies. In addition, carbides are unlikely to be stable under the oxidizing conditions of alteration experienced by CM chondrites. Instead, it is most probable that the magnetite rims on all the carbide particles are the product of parent body oxidation of Fe,Ni carbides, but this oxidation was incomplete, because of the buildup of an impermeable layer of amorphous carbon at the interface between the magnetite and the carbide phase that arrested the reaction before it went to completion. These observations suggest that although FTT catalysis reactions may not have been the major mechanism of organic material formation within the solar nebula, they nevertheless contributed to the inventory of complex insoluble organic matter that is present in carbonaceous chondrites.     

Kinetic Alfven waves in plasma sheet boundary layer—particle aspect analysis

The particle aspect approach is adopted to investigate the trajectories of charged particles in the electromagnetic field of kinetic Alfven wave. Expressions are found for the dispersion relation, damping rate and associated currents in homogenous plasma. Kinetic effects of electrons and ions are included to study kinetic Alfven wave because both are important in the transition region. It is found that the ratio β of electron thermal energy density to magnetic field energy density and the ratio of ion to electron thermal temperature (T_i/T_e) affect the dispersion relation, damping-rate and associated currents in both cases (warm and cold electron limits). The treatment of kinetic Alfven wave instability is based on the assumption that the plasma consists of resonant and non-resonant particles. The resonant particles participate in an energy exchange process, whereas the non-resonant particles support the oscillatory motion of the wave.