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At least 253 records · Page 14

Removal of histological sections from glass for electron microscopy - Use of Quetol 651 resin and heat

A number of approaches have been used to separate stained conventional histological sections from glass slides in preparation for a study with the electron microscope. However, in each reported case some problems were encountered with respect to the separation process. The present investigation is concerned with the use of the epoxy resin Quetol 651 as an embedding medium for this procedure, taking into account the simple application of heat (62-64 C) for performing the separation step. After the tissue has been removed from the glass by the considered technique, it is thin sectioned, and stained with uranyl acetate-lead citrate.

Kraft, L. M.↗

Selected-zone dark-field electron microscopy.

Description of a new method which makes it possible to reduce drastically the resolution-limiting influence of chromatic aberration, and thus to obtain high-quality images, by selecting the image-forming electrons that have passed through a small annular zone of an objective lens. In addition, the manufacture of special objective-lens aperture diaphragms that are needed for this method is also described.

Heinemann, K.↗

Oxidation of metals and alloys in controlled atmospheres using in situ transmission electron microscopy and Auger spectrography

Single-crystalline thin films of copper were oxidized at an isothermal temperature of 425 C and at an oxygen partial pressure of .005 Torr in situ in a high-resolution electron microscope. The specimens were prepared by epitaxial vapor deposition onto polished 100 and 110 faces of rocksalt and mounted in a hot stage inside an ultra-high-vacuum specimen chamber of the microscope. Large amounts of sulfur, carbon, and oxygen were detected by Auger electron spectroscopy on the surface of the as-received films and were removed in situ by ion-sputter etching immediately prior to the oxidation. The nucleation and growth characteristics of Cu2O on Cu were studied. Results show that neither stacking faults nor dislocations are associated with the Cu2O nucleation sites. The growth of Cu2O nuclei is linear with time. The experimental findings, including results from oxygen dissolution experiments and from repetitive oxidation-reduction-oxidation sequences, fit well into the framework of an oxidation process involving (a) the formation of a surface-charge layer, (b) oxygen saturation in the metal and (c) nucleation, followed by surface diffusion of oxygen and bulk diffusion of copper for lateral and vertical oxide growth, respectively.

Rao, D. B.↗

Low voltage scanning electron microscopy of interplanetary dust particles

The resolution of available low-voltage SEM (LVSEM) models used in the characterization of interplanetary dust particles (IDPs) is limited by a number of factors including energy spread in the electron source, beam brightness, scanning electron detector geometry, and various lens aberrations. This paper describes an improved model of LVSEM which offers an increased resolution at low voltage. The improvements include a cold cathode FE source which has an extremely low inherent energy spread and high brightness, a second condenser lens to converge the beam and maintain an optimum aperture half-angle, and a detector optimized for low-voltage scanning-electron collection. To reduce lens aberrations, the specimen is immersed in the objective lens field. The features of several IDP samples observed using the images obtained with this LVSEM model are described.

Blake, D. F.↗

Electron microscopy of some experimentally shocked counterparts of lunar minerals.

Particulate samples of experimentally shocked olivine, enstatite, and apatite and their unshocked equivalents were thinned by ion bombardment and examined by transmission methods in a conventional (100 kV) electron microscope. Enstatite shock-loaded at a peak pressure of 250 kb was partly transformed to relatively dense inverse defect spinel. Magnesian olivine shocked at a peak pressure of 200 kb shows intense lattice deformation. Magnesian olivine shock-loaded at a peak pressure of 400 kb was recrystallized to very fine polycrystalline aggregates. Apatite shock-loaded at a peak pressure of 250 kb shows planar deformation elements and shock-induced imperfections.

Sclar, C. B.↗

Electron microscopy study of the iron meteorite Santa Catharina

A characterization of the microstructural features of Santa Catharina (SC) from the millimeter to submicron scale is presented. The same specimen was examined using an optical microscope, a scanning electron microscope, an electron probe microanalyzer, and an analytical electron microscope. Findings include the fact that SC metal nodules may have different bulk Ni values, leading to different microstructures upon cooling; that SC USNM 6293 is the less corroded sample, as tetrataenite exists as less than 10 nm ordered domains throughout the entire fcc matrix (it is noted that this structure is the same as that of the Twin City meteorite and identical to clear taenite II in the retained taenite regions of the octahedrites); that SC USNM 3043 has a more complicated microstructure due to corrosion; and that the low Ni phase of the cloudy zone was selectively corroded in some areas and formed the dark regions, indicating that the SC meteorite corrosion process was electrochemical in nature and may involve Cl-containing akaganeite.

Zhang, J.↗

Electron Microscopy and Image Analysis for Selected Materials

This particular project was completed in collaboration with the metallurgical diagnostics facility. The objective of this research had four major components. First, we required training in the operation of the environmental scanning electron microscope (ESEM) for imaging of selected materials including biological specimens. The types of materials range from cyanobacteria and diatoms to cloth, metals, sand, composites and other materials. Second, to obtain training in surface elemental analysis technology using energy dispersive x-ray (EDX) analysis, and in the preparation of x-ray maps of these same materials. Third, to provide training for the staff of the metallurgical diagnostics and failure analysis team in the area of image processing and image analysis technology using NIH Image software. Finally, we were to assist in the sample preparation, observing, imaging, and elemental analysis for Mr. Richard Hoover, one of NASA MSFC's solar physicists and Marshall's principal scientist for the agency-wide virtual Astrobiology Institute. These materials have been collected from various places around the world including the Fox Tunnel in Alaska, Siberia, Antarctica, ice core samples from near Lake Vostoc, thermal vents in the ocean floor, hot springs and many others. We were successful in our efforts to obtain high quality, high resolution images of various materials including selected biological ones. Surface analyses (EDX) and x-ray maps were easily prepared with this technology. We also discovered and used some applications for NIH Image software in the metallurgical diagnostics facility.

Williams, George↗

Techniques for the correction of topographical effects in scanning Auger electron microscopy

A number of ratioing methods for correcting Auger images and linescans for topographical contrast are tested using anisotropically etched silicon substrates covered with Au or Ag. Thirteen well-defined angles of incidence are present on each polyhedron produced on the Si by this etching. If N1 electrons are counted at the energy of an Auger peak and N2 are counted in the background above the peak, then N1, N1 - N2, (N1 - N2)/(N1 + N2) are measured and compared as methods of eliminating topographical contrast. The latter method gives the best compensation but can be further improved by using a measurement of the sample absorption current. Various other improvements are discussed.

Prutton, M.↗

Transmission electron microscopy of an interplanetary dust particle with links to CI chondrites

The majority of hydrated interplanetary dust particles (IDPs) have compositions that resemble CI and CM chondrites, however, their mineralogies are most similar to the fine grained material in certain altered type-3 carbonaceous and ordinary chondrites. During the transmission electron microscope studies of hydrated IDPs, a unique particle was discovered whose mineralogy is very similar to that reported from CI chondrites. W7013F5 is the first IDP whose mineralogy and chemistry approximates that of CI chondrites. The similarity in mineralogy and mineral chemistry suggests that W7013F5 was altered under conditions similar to those that existed on the CI parent bodies.

Keller, Lindsay P.↗

Experimental Investigation of Space Radiation Processing in Lunar Soil Ilmenite: Combining Perspectives from Surface Science and Transmission Electron Microscopy

Energetic ions mostly from the solar wind play a major role in lunar space weathering because they contribute structural and chemical changes to the space-exposed surfaces of lunar regolith grains. In mature mare soils, ilmenite (FeTiO3) grains in the finest size fraction have been shown in transmission electron microscope (TEM) studies to exhibit key differences in their response to space radiation processing relative to silicates [1,2,3]. In ilmenite, solar ion radiation alters host grain outer margins to produce 10-100 nm thick layers that are microstructurally complex, but dominantly crystalline compared to the amorphous radiation-processed rims on silicates [1,2,3]. Spatially well-resolved analytical TEM measurements also show nm-scale compositional and chemical state changes in these layers [1,3]. These include shifts in Fe/Ti ratio from strong surface Fe-enrichment (Fe/Ti >> 1), to Fe depletion (Fe/Ti < 1) at 40-50 nm below the grain surface [1,3]. These compositional changes are not observed in the radiation-processed rims on silicates [4]. Several mechanism(s) to explain the overall relations in the ilmenite grain rims by radiation processing and/or additional space weathering processes were proposed by [1], and remain under current consideration [3]. A key issue has concerned the ability of ion radiation processing alone to produce some of the deeper- penetrating compositional changes. In order to provide some experimental constraints on these questions, we have performed a combined X-ray photoelectron spectroscopy (XPS) and field-emission scanning transmission electron (FE-STEM) study of experimentally ion-irradiated ilmenite. A key feature of this work is the combination of analytical techniques sensitive to changes in the irradiated samples at depth scales going from the immediate surface (approx.5 nm; XPS), to deeper in the grain interior (5-100 nm; FE-STEM).

Christoffersen, R.↗

Below Band-Gap Laser Ablation of Diamond for Transmission Electron Microscopy

A 248-nm excimer laser was used to thin naturally occurring type 1a diamond substrates at normal and glancing (22 deg) incidence. Perforation of a 250 micron thick substrate was achieved in about 15 minutes at normal incidence. Whilst the substrate thinned at glancing incidence was found to have large electron-transparent areas, that thinned at normal incidence required additional argon milling to achieve electron transparency. X-ray photoelectron spectroscopy of the back surface of the diamond failed to detect any graphite or glassy carbon, confirming that damage due to laser ablation occurs only at the incident surface. Samples prepared using this technique imaged in the transmission electron microscope were observed to have retained the nitrogen platelets

Posthill, J. B.↗

Active Learning Surrogates for Integrating Electron Microscopy and Computational Insights from Simulations in Autonomous Experiments

Artificial Intelligence (AI) combined with simulations and experiments has great potential to accelerate scientific discovery across technology and pharmaceuticals. However, the gap between simulations and experiments is challenging due to disparities in time and scale, making it difficult to estimate properties like energy and electronic states from experiments, and to provide feedback based on theoretical insights.Our research addresses the challenge by developing unique deep kernel based surrogate models that learns from microscopic images, mapping structural features to energy differences from defect formation. We start with full-training using simulated images to determine optimal settings, establishing a baseline for active learning. Using these settings from the baseline, active learning is trained, and predicts structures along simulation trajectories based on uncertainty and energetic stability, thus reducing data requirements, simulation time and computational costs. The results demonstrate that the model achieves a low average error margin of approximately 0.03 meV, indicating good performance. To enhance feature extraction and reconstruction capabilities, we developed an autoencoder-decoder as additional surrogate to create latent space to capture essential features, enabling precise comparisons between simulations and experiments. The results from this model achieved a reconstruction loss of around 0.2 and accurately reconstructed molecular structures.Overall, this work advances the steering of experiments through computational simulations by employing a surrogate models that actively predicts the trajectories of structural evolution, achieving time-to-solution comparable to experimental measurements.

Saranathan, Gayathri [Hewlett-Packard]↗

Below band-gap laser ablation of diamond for transmission electron microscopy

A 248 nm excimer laser was used to thin naturally occurring type 1a diamond substrates at normal and glancing (22 deg) incidence. Perforation of a 250-micron-thick substrate was achieved in about 15 min at normal incidence. While the substrate thinned at glancing incidence was found to have large electron-transparent areas, that thinned at normal incidence required additional argon-ion milling to achieve electron transparency. X-ray photoelectron spectroscopy of the back surface of the diamond failed to detect any graphite or glassy carbon, confirming that damage due to laser ablation occurs only at the incident surface. Samples prepared using this technique imaged in the transmission electron microscope were observed to have retained the nitrogen platelets characteristic of such type 1a diamonds.

George, T.↗

Transmission electron microscopy of composites

Since interphase-interfaces are often both the structurally weakest and chemically least stable regions of a composite material, they are critical determinants of such macrostructural characteristics as tensile strength and fracture toughness. Attention is presently given to the use of TEM for the study of interfaces between dissimilar materials; electron-diffraction, analytical, and high-resolution forms of TEM are employed, for the cases of both structural and semiconductor composites. The materials studied are SiC/Si, GaP/Si, and SiC fiber- and whisker-reinforced Si3N4.

Pirouz, P.↗

Effects of radiation upon the light-sensing elements of the retina as characterized by scanning electron microscopy

A model system using Necturus maculosus, the common mudpuppy, was established for evaluating effects of radiation upon the light-sensing elements of the retina. Accelerated heavy ions of helium and neon from the Berkeley Bevalac were used. A number of criteria were chosen to characterize radiation damage by observing morphological changes with the scanning electron microscope. The studies indicated retina sensitivity to high-LET (neon) particles at radiation levels below 10 rads (7 particles per visual element) whereas no significant effects were seen from fast helium ions below 50 rads.

Malachowski, M. J.↗

Electron Microscopy of Microbial Biomass

As humans move to long term stays in space their microbes move with them. This poses problems as the microbes can colonize various life support systems, creating biofilms that can grow and spread, which in turn causes obstructions and ultimately degrades function of these systems. MSFC currently has no protocol in place for the Scanning Electron Microscope (SEM) imaging of microbes.

Samantha Marcella↗

Phase transformations in 40-60-GPa shocked gneisses from the Haughton Crater (Canada): An Analytical Transmission Electron Microscopy (ATEM) study

In order to better understand phase transformations, chemical migration, and isotopic disequilibrium in highly shocked rocks, we have performed a microprobe and an ATEM study on gneisses shocked up to 60 GPa from the Haughton Crater. This study reveals the following chemical and structural characteristics: (1) SiO2 dominant areas are formed by a mixture of pure SiO2 polycrystalline quartz identified by electron diffraction pattern and chemical analysis and a silica-rich amorphous phase containing minor amounts of aluminium, potassium, and iron; (2) Areas with biotitelike composition are formed by less than 200-nm grains of iron-rich spinels embedded in a silica-rich amorphous phase that is very similar to the one described above; (3) Layers with feldsparlike composition are constituted by 100-200-nm-sized alumina-rich grains (the indexation of the crystalline structure is under progress) and the silica-rich amorphous phase; (4) Zones characterized by the unusual Al/Si ratio close to 1 are formed by spinel grains (200-nm-sized) embedded in the same silica-rich amorphous phase; and (5) The fracturated sillimanites contain domains with a lamellar structure, defined by the intercalation of 100-nm-wide lamellae of mullite crystals and of a silica-rich amorphous phase. These mullite crystals preserved the crystallographical orientation of the preshock sillimanite. All compositional domains, identified at the microprobe scale, can thus be explained by a mixture in different proportion between the following phases: (1) a silica-rich amorphous phase, with minor Al and K; (2) quartz crystals; (3) spinel crystals and alumina-rich crystals; (4) sillimanite; and (5) mullite. Such mixtures of amorphous phases and crystals in different proportions explain disturbed isotope systems in these rocks and chemical heterogeneities observed on the microprobe.

Martinez, I.↗

Transmission Electron Microscopy of Magnetite Plaquettes in Orgueil

Magnetite sometimes takes the form of a plaquette - barrel-shaped stack of magnetite disks - in carbonaceous chondrites (CC) that show evidence of aqueous alteration. The asymmetric nature of the plaquettes caused Pizzarello and Groy to propose magnetite plaquettes as a naturally asymmetric mineral that can indroduce symmetry-breaking in organic molecules. Our previous synchrotron X-ray computed microtomography (SXRCT) and electron backscatter diffraction (EBSD) analyses of the magnetite plaquettes in fifteen CCs indicate that magnetite plaquettes are composed of nearly parallel discs, and the crystallographic orientations of the discs change around a rotational axis normal to the discs surfaces. In order to further investigate the nanostructures of magnetite plaquettes, we made two focused ion beam (FIB) sections of nine magnetite plaquettes from a thin section of CI Orgueil for transmission electron microscope (TEM) analysis. The X-ray spectrum imaging shows that the magnetite discs are purely iron oxide Fe3O4 (42.9 at% Fe and 57.1 at% O), which suggest that the plaquettes are of aqueous origin as it is difficult to form pure magnetite as a nebular condensate. The selected area electron diffraction (SAED) patterns acquired across the plaquettes show that the magnetite discs are single crystals. SEM and EBSD analyses suggest that the planar surfaces of the magnetite discs belong to the {100} planes of the cubic inverse spinel structure, which are supported by our TEM observations. Kerridge et al. suggested that the epitaxial relationship between magnetite plaquette and carbonate determines the magnetite face. However, according to our TEM observation, the association of magnetite with porous networks of phyllosilicate indicates that the epitaxial relationship with carbonate is not essential to the formation of magnetite plaquettes. It was difficult to determine the preferred rotational orientation of the plaquettes due to the symmetry of the cubic structure, however, we are able to observe small but consistent rotational orientation across several discs within a plaquette.

Chan, Q. H. S.↗