Melting, ablation, and vapor phase condensation during atmospheric passage of the Bjurbole Meteorite

A detailed study of the Bjurbole fusion crust using scanning electron microscopy (SEM) and energy dispersive analysis (EDS) shows that filamentary crystals and ablation spheres may form on the meteoroid surface. Filamentary crystals, hollow spheres, and porous regions of the surface point to a period of intense vapor phase activity during atmospheric passage. Filamentary crystals can be divided into three categories on the basis of bulk composition and morphology. Two types of filamentary crystals are vapor phase condensation products formed during atmospheric entry of the meteoroid. The other type forms by the interaction of seawater with the fusion surface. The density and composition of ablation spheres varies with the flight orientation of the meteorite. The size range and composition of iron-nickel spheres on the surface of Bjurbole are similar to spheres collected in the stratosphere. A comparison of stratospheric dust collections with meteorite surfaces may provide further insight into the mechanisms of meteoroid entry into planetary atmospheres.

Infrared spectra of Mg-SiO smokes : comparison with analytical electron microscopy studies

An important component of current models for interstellar and circumstellar evolution is the infrared (IR)spectral data collected from stellar outflows around oxygen-rich stars and from the general interstellar medium [1]. IR spectra from these celestial bodies are usually interpreted as showing the general properties of sub-micron sized silicate grains [2]. Two major features at 10 and 20 microns are reasonably attributed to amorphous olivine or pyroxene (e.g. Mg2Si04 or MgSi03) on the basis of comparisons with natural standards and vapor condensed silicates [3-6]. In an attempt to define crystallisation rates for spectrally amorphous condensates, Nuth and Donn [5] annealed experimentally produced amorphous magnesium silicate smokes at 1000K. On analysing these smokes at various annealing times, Nuth and Donn [5] showed that changes in crystallinity measured by bulk X-ray diffraction occured at longer annealing times (days) than changes measured by IR spectra (a few hours). To better define the onset of crystallinity in these magnesium silicates, we have examined each annealed product using a JEOL 1OOCX analytical electron microscope (AEM). In addition, the development of chemical diversity with annealing has been monitored using energy dispersive spectroscopy of individual grains from areas <20nm in diameter. Furthermore, the crystallisation kinetics of these smokes under ambient, room temperature conditions have been examined using bulk and fourier transform infrared (FTIR)spectra.

Electron petrography of fine-grained matrix in the Karoonda C4 carbonaceous chondrite

The study of matrices of rare Type 4 carbonaceous chondrites can reveal important information on parent body rnetamorp~ic processes and provide a comparison with processes on parent bodies of ordinary chc-idrites. Reflectance spectra (Tholen, 1984) from the two largest asteroids in the asteroid belt, Ceres and Pallas, suggest that they may be metamorphosed carbonaceous chondrites. These two asteroids constitute - onethird of the mass in the asteroid belt implying that type 4-6 carbonaceous chondrites are poorly represented in the meteorite collection and may be of considerable importance. The matrix of the C4 chondrite Karoonda has been investigated using a JEOL 2000FX analytical electron microscope (AEM) with an attached Tracor-Northem TN5500 energy dispersive spectrometer (EDS). In previous studies (Scott and Taylor, 1985; Fitzgerald, 1979; Van Schmus, 1969), the petrography of the Karoonda matrix has been described as consisting largely of coarse-grained (50-200 urn in size) olivine and plagioclase (20-100 um in size), associated with micrometer sized magnetite and rare sulphides. AEM observations on matrix show that in addition to these large grains, there is a significant fraction (10 vol%) of interstitial fine grained phases « 5 urn). The mineralogy of these fine-grained phases differs in some respects from that of the coarser-grained matrix identified by optical and SEM techniques (Scott and Taylor, 1985; Fitzgerald, 1979; Van Schmus, 1969). I~ particular crystals of two compositionally distinct pyroxenes « 2 urn in size) have been identified which have not been previously observed in Karoonda by other analytical techniques. Thin film microanalyses (Mackinnon et al., 1986) of these two pyroxenes indicate compositions consistent with augite and low-Ca pyroxene (- Fs27). Fine-grained anhedral olivine « 2 urn size) is the most abundant phase with composition -Fa29' This composition is essentially indistinguishable from that determined for coarser-grained matrix olivines using an electron microprobe (Scott and Taylor, 1985; Fitzgerald, 1979; Van Schmus, 1969). All olivines are associated with subhedral magnetites « 1 urn size) which contain significant Cr (- 2%) and Al (- 1%) as was also noted for larger sized Karoonda magnetites by Delaney et al. (1985). It has recently been suggested (Burgess et al., 1987) on the basis of sulphur release profiles for S-isotope analyses of Karoonda that CaS04 (anhydrite) may be present. However, no sulphate phase has, as yet, been identified in the matrix of Karoonda. Low magnification contrast images suggest that Karoonda may have a significant porosity within the fine-grained matrix fraction. Most crystals are anhedral and do not show evidence for significant compaction. Individual grains often show single point contact with other grains which result in abundant intergranular voids. These voids frequently contain epoxy which was used as part of the specimen preparation procedure due to the friable nature of the bulk sample.

Interstellar titanium-oxides in interplanetary dust

Interstellar gas abundances (Clayton et al., 1986) suggest that titanium may be bound up in dust and indeed, excess titanium in carbonaceous chondrites is attributed to mixing of interstellar and Solar System materials (Morton, 1974). Fine-grained chondritic interplanetary dust particles (lOPs) of cometary origin are relatively pristine early Solar System materials (Mackinnon and Rietmeijer, 1987; Rietmeijer, 1987) and show chemical and mineralogical signatures related to a pre-solar or nebular origin. For example, large OtH ratios suggest a presolar or interstellar dust component in some chondritic lOPs(Mackinnon and Rietmeijer, 1987). Ti/Si ratios (normalized to bulk CI) in lOPs and carbonaceous chondrite matrices exceed solar abundances but are similar to dust from comet Halley (Jessberger et al., 1987). The Ti-distribution in chondritic lOPs shows major, small-scale « 0.1 urn) variations (Flynn et al., 1978) consistent with heterogeneously distributed Ti-bearingphases. Analytical electron microscope (AEM) studies, in fact, have identified platey grains of Ti-metal, Ti407 and Ti s09 in two different lOPs (Mackinnon and Rietmeijer, 1987). The occurrence of Ti407 was related in situ low-temperature aqueous alteration and therefore implied the presence of BaTi03 (Rietmeijer and Mackinnon, 1984). Yet, the presence ofTis09 in an lOp which shows no evidence of aqueous alteration (Rietmeijer.and McKay, 1986) requires a different interpretation. The distribution of Ti-oxides in chondritic lOPs were investigated with ultra-microtomed thin sections of fluffy chondri tic lOP U2011*B (lSC allocation U2011C2) using a lEOL 2000FX AEM operating at an accelerating voltage of 200kV and with an attached Tracor Northern TN5500 energy dispersive spectrometer.

Microstructural characterization of quenched melt-textured YBa2Cu3O7-δ materials

The microstructure of YBa2Cu3O7-δ (YBCO) materials, melt-textured in air and quenched from the temperature range 900-990°C, has been characterized using a combination of x-ray diffractometry, optical microscopy, scanning electron microscopy, transmission electron microscopy, and energy dispersive x-ray spectrometry. BaCu2O2 and BaCuO2 were found to coexist in samples quenched from the temperature range 920-960°C. The formation of BaCu2O2 preceded the formation of YBCO. Once the YBCO had formed, BaCu2O2 was present at the solidification front filling the space between nearly parallel platelets of YBCO. Large Y2BaCuO5 particles at the solidification front appeared divided into smaller ones as a result of their dissolution in the liquid that quenched as BaCu2O2.

Reaction products between Bi-Sr-Ca-Cu-oxide thick films and alumina substrates

The structure and composition of reaction products between Bi-Sr-Ca-Cu-oxide (BSCCO) thick films and alumina substrates have been characterized using a combination of electron diffraction, scanning electron microscopy and energy dispersive X-ray spectrometry (EDX). Sr and Ca are found to be the most reactive cations with alumina. Sr4Al6O12SO4 is formed between the alumina substrates and BSCCO thick films prepared from paste with composition close to Bi-2212 (and Bi-2212 + 10 wt.% Ag). For paste with composition close to Bi(Pb)-2223 + 20 wt.% Ag, a new phase with f.c.c. structure, lattice parameter about a = 24.5 A and approximate composition Al3Sr2CaBi2CuOx has been identified in the interface region. Understanding and control of these reactions is essential for growth of high quality BSCCO thick films on alumina. (C) 1997 Elsevier Science S.A.

Microstructural investigation of Bi-Sr-Ca-Cu-oxide thick films on alumina substrates

The microstructure of Bi-Sr-Ca-Cu-oxide (BSCCO) thick films on alumina substrates has been characterized using a combination of X-ray diffractometry, scanning electron microscopy, transmission electron microscopy of sections across the film/substrate interface and energy-dispersive X-ray spectrometry. A reaction layer formed between the BSCCO films and the alumina substrates. This chemical interaction is largely responsible for off-stoichiometry of the films and is more significant after partial melting of the films. A new phase with fee structure, lattice parameter a = 2.45 nm and approximate composition Al3Sr2CaBi2CuOx has been identified as reaction product between BSCCO and Al2O3.

Calcite precipitation induced by clay-bleach cation exchange in andesitic reservoir rocks

Experiments were carried out on the sodium hypochlorite bleach sensitivity of a deep subsurface andesitic reservoir in order to predict possible deleterious mineral transformations during a downhole clean-up job. Experiments involved examination of core samples from the reservoir using an Environmental Scanning Electron Microscope (ESEM) with an attached Energy Dispersive Spectrometer (EDS) before and after the samples were immersed in bleach. Bleach immersion of whole-rock samples resulted in rapid (less than 1 min) precipitation of abundant 3.0-10.0-μm-wide calcite rhombs within clay-associated micropores and on clay and feldspar grain surfaces. Abundant microporefilling calcite rhombs also formed in pure separates of constituent chlorite/corrensite, whereas no calcite formed in a pure separate of constituent zeolite. These experiments indicate that corrensite is the likely calcium source in this experimental fluid-rock system. Formation of calcite occurs via a cation exchange reaction in which calcium in the smectitic interlayers of corrensite exchanges for sodium in the bleach. Serious formation damage due to calcite precipitation would have occurred in the andesite reservoir had it been exposed to bleach. This finding gives credence to earlier suggestions that cation exchange reactions have the potential to cause calcite precipitation in some sandstone reservoirs when exposed to drilling, completion or stimulation fluids. © 1993.

Microanalysis of clays at low temperature

Accurate thin-film energy dispersive spectroscopic (EDS) analyses of clays with low-atomic-number (low Z) elements (e.g. Na, Al, Si), presents a challenge to the microscopist not only because of the spatial resolution required, but also because of their susceptibility to electron beam-induced radiation damange and very low X-ray count rates. Most common clays, such as kaolinite, smectite and illite occur as submicrometer crystallites with varying degrees of structural disorder in at least two directions and may have dimensions as small as one or two unit cells along the basal direction. Thus, even clays with relatively large a-b dimenstions (e.g., 100 x 100 nm) may be <5nm in the c-axis direction. For typical conditions in an analytical electron microscope (AEM), this sample thickness gives rise to very poor count rates (<200cps) and necessitates long counting times (>300s) in order to obtain satisfactory statistical precision. Unfortunately, beam damage rates for the common clays are very rapid (<10s in imaging mode) between 100kV and 200kV. With a focussed probe for elemental analyses, the damage rate is exacerbated by a high current density and may result in loss of low-Z elements during data collection and consequent loss of analytical accuracy.

Catalytic cracking of tars derived from rice hull gasification over goethite and palygorskite

Palygorskite (P), goethite (G), and hydrothermally synthesized goethite (HG) were used as supports for Fe and Ni. The catalytic activity of these materials was investigated involving in P, G and HG (supported Fe and Ni) for catalytic decomposition of biomass tar derived from rice hull gasification. The materials were characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), and transmission electron microscopy (TEM) with an energy dispersive X-ray (EDS). The catalytic activity of P for removal of tar was significantly better than that of G and HG. However, the activity of G with 6 mass% Ni labeled as Ni6/G (tar conversion 94.6%), which was equal to Fe6Ni6/P (94.4%), was better than Ni6/P (64.4%) and Ni6/HG (46.7%). When the loading of Ni (mass%) was 6 mass% on G, tar conversion had the best value (94.6%) and yield of gaseous products reached 486.9, 167.8 and 22.2 mL/(g·tar) for H2, CO, CH4, respectively. The catalytic activity of goethite supported Ni was better in improving tar conversion and improving increased yield of H2, CO, CH4, which was attributed to the existence of Al/Fe substitution of goethite

Electron microscopy of stratospheric particles

A recent NASA program to collect stratospheric dust particles using high-flying WB57 aircraft has made available many more potential candidates for the study of extraterrestrial materials. This preliminary report provides an interpretation of the types of particles returned from one flag (W7017) collected in August, 1981 using a subset of 81 allocated particles. This particular collection period is after the Mt. St. Helen's eruptions. Therefore, the flag may contain significant quantities of volcanic debris in addition to the expected terrestrial contaminants [1]. All particles were mounted on nucleopore filters and have been examined using a modified JEOL100CX analytical electron microscope. For most of the particles, X-ray energy dispersive spectra and images were obtained at 40kV on samples which have not received any conductive coating. However, in order to improve resolution (to ~30A) some images are recorded at 100kV. In addition, 16 samples have been coated with a thin layer (<50A) of Au/Pd.

Composition and morphology of particle emissions from in-use aircraft during takeoff and landing

In order to provide realistic data for air pollution inventories and source apportionment at airports, the morphology and composition of ultrafine particles (UFP) in aircraft engine exhaust were measured and characterized. For this purpose, two independent measurement techniques were employed to collect emissions during normal takeoff and landing operations at Brisbane Airport, Australia. PM1 emissions in the airfield were collected on filters and analyzed using the particle-induced X-ray emission (PIXE) technique. Morphological and compositional analyses of individual ultrafine particles in aircraft plumes were performed on silicon nitride membrane grids using transmission electron microscopy (TEM) combined with energy-dispersive X-ray microanalysis (EDX). TEM results showed that the deposited particles were in the range of 5 to 100 nm in diameter, had semisolid spherical shapes and were dominant in the nucleation mode (18 – 20 nm). The EDX analysis showed the main elements in the nucleation particles were C, O, S and Cl. The PIXE analysis of the airfield samples was generally in agreement with the EDX in detecting S, Cl, K, Fe and Si in the particles. The results of this study provide important scientific information on the toxicity of aircraft exhaust and their impact on local air quality.

Electrical property and characterization of nano-SnO2/wollastonite composite materials

Nano-tin oxide was deposited on the surface of wollastonite using the mixed solution including stannic chloride pentahydrate precursor and wollastonite by a hydrolysis precipitation process. The antistatic properties of the wollastonite materials under different calcined conditions and composite materials (nano-SnO2/wollastonite, SW) were measured by rubber sheeter and four-point probe (FPP) sheet resistance measurement. Effects of hydrolysis temperature and time, calcination temperature and time, pH value and nano-SnO2 coating amount on the resistivity of SW powders were studied, and the optimum experimental conditions were obtained. The microstructure and surface properties of wollastonite, precipitate and SW were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDS), specific surface area analyzer (BET), thermogravimetry (TG), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and Fourier translation infrared spectroscopy (FTIR) respectively. The results showed that the nano-SnO2/wollastonite composite materials under optimum preparation conditions showed better antistatic properties, the resistivity of which was reduced from 1.068 × 104 Ω cm to 2.533 × 103 Ω cm. From TG and XRD analysis, the possible mechanism for coating of SnO2 nanoparticles on the surface of wollastonite was proposed. The infrared spectrum indicated that there were a large number of the hydroxyl groups on the surface of wollastonite. This is beneficial to the heterogeneous nucleation reaction. Through morphology, EDS and XPS analysis, the surface of wollastonite fiber was coated with a layer of 10–15 nm thickness of tin oxide grains the distribution of which was uniform.

Removal of phosphorus using NZVI derived from reducing natural goethite

Nano zero valent iron (NZVI) prepared by reducing natural goethite in hydrogen at 550 °C was used to remove phosphate. The effect of particle size, reaction time, NZVI dose, pH, initial phosphorus concentration, and oxygen amount in reaction system on phosphorus removal was investigated. The characterization of X-ray fluorescence (XRF), X-ray diffraction (XRD), N2 adsorption and desorption (BET analysis), transmission electron microscope (TEM), field emission scanning electron microscope with a energy dispersive X-ray detector (FESEM/EDS) and X-ray photoelectron spectroscopy (XPS) indicated that nanoscale of iron (around 80–150 nm length and 5–30 nm width) was prepared successfully with high dispersion and relative large surface area around 22 m2/g. The results of batch experiments and XPS analysis suggested that this kind of NZVI had a good performance on removal of phosphate (over 99%) despite in slightly acidic media as the initial concentration of P was 5 mg/L. The reason was ascribed to the effective corrosion of this NZVI under the function of proton and dissolved oxygen in spite of the existence of thin passive films.