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Sample records for microscopy tem study

  1. High-resolution TEM microscopy study of the creep behaviour of carbon-based cathode materials

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Wei, E-mail: wwlyzwkj@126.com [College of Materials Science and Engineering, Henan University of Science and Technology, Luoyang 471023 (China); Collaborative Innovation Center of Nonferrous Metals Henan Province, Luoyang 471023 (China); Chen, Weijie [College of Materials Science and Engineering, Henan University of Science and Technology, Luoyang 471023 (China); Collaborative Innovation Center of Nonferrous Metals Henan Province, Luoyang 471023 (China); Gu, Wanduo [Collaborative Innovation Center of Nonferrous Metals Henan Province, Luoyang 471023 (China)

    2017-02-27

    Creep is in close relationship with the materials deterioration and deformation of the cathodes in aluminum reduction cells. The purpose of this work is to obtain the creep mechanism of the carbon cathode for aluminum electrolysis. A modified Rapoport equipment was used for measuring the creep strain of the semi-graphitic cathodes during aluminum electrolysis with CR=2.5 and at temperature of 945 ℃. The arrangement of carbon atom has been studied after hexagonal graphite converting into rhombohedral graphite during aluminum electrolysis by XRD and high-resolution transmission electron microscopy (HRTEM). The creep deformation of the carbon cathode has a close relationship with the mobile dislocation walls. These results will be helpful in controlling the cathode quality and its performance in aluminum reduction cells.

  2. The principle of electron microscopy; SEM and TEM

    International Nuclear Information System (INIS)

    Fauzi, S.H.

    1992-01-01

    The article reviews the principle of electron microscopy which is used in scanning electron microscope (SEM) and transmission electron microscope (TEM). These instruments are important for the examination and analysis of the microstructural properties of solid objects. Relevance physical concept lies behind the devices are given. The main components of each device are also discussed

  3. In-situ TEM Studies : Heat-treatment and Corrosion

    NARCIS (Netherlands)

    Malladi, S.R.K.

    2014-01-01

    Transmission electron microscopy (TEM) has been well known as a powerful characterisation tool to understand the structure and composition of various materials down to the atomic level. Over the years, several TEM studies have been carried out to understand the compositional, structural and

  4. An efficient and reproducible process for transmission electron microscopy (TEM) of rare cell populations

    Science.gov (United States)

    Kumar, Sachin; Ciraolo, Georgianne; Hinge, Ashwini; Filippi, Marie-Dominique

    2014-01-01

    Transmission electron microscopy (TEM) provides ultra-structural details of cells at the sub-organelle level. However, details of the cellular ultrastructure, and the cellular organization and content of various organelles in rare populations, particularly in the suspension, like hematopoietic stem cells (HSCs) remained elusive. This is mainly due to the requirement of millions of cells for TEM studies. Thus, there is a vital requirement of a method that will allow TEM studies with low cell numbers of such rare populations. We describe an alternative and novel approach for TEM studies for rare cell populations. Here we performed TEM study from 10,000 HSC cells with quite ease. In particular, tiny cell pellets were identified by Evans blue staining after PFA-GA fixation. The cell pellet was pre-embedded in agarose in a small microcentrifuge tube and processed for dehydration, infiltration and embedding. Semi-thin and ultra-thin sections identified clusters of numerous cells per sections with well preserved morphology and ultrastructural details of golgi complex and mitochondria. Together, this method provides an efficient, easy and reproducible process to perform qualitative and quantitative TEM analysis from limited biological samples including cells in suspension. PMID:24291346

  5. TEM studies of P+ implanted and subsequently laser annealed Si

    International Nuclear Information System (INIS)

    Sadana, D.K.; Wilson, M.C.; Booker, G.R.; Washburn, J.

    1979-05-01

    The present investigation is concerned with laser annealing of P + implanted Si. The aim of the work was to study the crystallization behavior of damage structure occurring due to high dose rate implantation using transmission electron microscopy (TEM) as the method of examination

  6. A TEM Study on the Ti-Alloyed Grey Iron

    DEFF Research Database (Denmark)

    Moumeni, Elham; Tiedje, Niels Skat; Grumsen, Flemming Bjerg

    2014-01-01

    The microstructure of graphite flakes in titanium alloyed cast iron is studied using electron microscopy techniques. Dual beam SEM/FIB has been used for TEM sample preparation. A TEM study has been carried out on graphite flakes in grey cast iron using selected area electron diffraction. Based...... and that there is a high proportion of twins in the fine grained graphite. It appears that twinning and stacking faults are involved in the fine grained structure of the graphite. It is discussed how Ti addition affect crystal growth and may lead to formation of superfine graphite....

  7. eV-TEM: Transmission electron microscopy in a low energy cathode lens instrument

    Energy Technology Data Exchange (ETDEWEB)

    Geelen, Daniël, E-mail: geelen@physics.leidenuniv.nl [Huygens-Kamerlingh Onnes Laboratory, Leiden Institute of Physics, Leiden University, P.O. Box 9504, 2300 RA Leiden (Netherlands); Thete, Aniket [Huygens-Kamerlingh Onnes Laboratory, Leiden Institute of Physics, Leiden University, P.O. Box 9504, 2300 RA Leiden (Netherlands); Schaff, Oliver; Kaiser, Alexander [SPECS GmbH, Voltastrasse 5, D-13355 Berlin (Germany); Molen, Sense Jan van der [Huygens-Kamerlingh Onnes Laboratory, Leiden Institute of Physics, Leiden University, P.O. Box 9504, 2300 RA Leiden (Netherlands); Tromp, Rudolf [IBM T.J. Watson Research Center, 1101 Kitchawan Road, P.O. Box 218, Yorktown Heights, NY 10598 (United States)

    2015-12-15

    We are developing a transmission electron microscope that operates at extremely low electron energies, 0–40 eV. We call this technique eV-TEM. Its feasibility is based on the fact that at very low electron energies the number of energy loss pathways decreases. Hence, the electron inelastic mean free path increases dramatically. eV-TEM will enable us to study elastic and inelastic interactions of electrons with thin samples. With the recent development of aberration correction in cathode lens instruments, a spatial resolution of a few nm appears within range, even for these very low electron energies. Such resolution will be highly relevant to study biological samples such as proteins and cell membranes. The low electron energies minimize adverse effects due to radiation damage. - Highlights: • We present a new way of performing low energy transmission electron microscopy in an aberration corrected LEEM/PEEM instrument. • We show a proof of principle where we measure transmitted electrons through a suspended graphene monolayer with a preliminary setup. • We present an improved setup design that provides better control of the incident electron beam.

  8. TEM Study of SAFARI-2000 Aerosols

    Science.gov (United States)

    Buseck, Peter R.

    2004-01-01

    The aim of our research was to obtain data on the chemical and physical properties of individual aerosol particles from biomass smoke plume s in southern Africa and from air masses in the region that are affec ted by the smoke. We used analytical transmission electron microscopy (ATEM), including energy-dispersive X-ray spectrometry (EDS) and ele ctron energy-loss spectroscopy (EELS), and field-emission electron microscopy (FESEM) to study aerosol particles from several smoke and haz e samples and from a set of cloud samples.

  9. Atom-counting in High Resolution Electron Microscopy:TEM or STEM - That's the question.

    Science.gov (United States)

    Gonnissen, J; De Backer, A; den Dekker, A J; Sijbers, J; Van Aert, S

    2017-03-01

    In this work, a recently developed quantitative approach based on the principles of detection theory is used in order to determine the possibilities and limitations of High Resolution Scanning Transmission Electron Microscopy (HR STEM) and HR TEM for atom-counting. So far, HR STEM has been shown to be an appropriate imaging mode to count the number of atoms in a projected atomic column. Recently, it has been demonstrated that HR TEM, when using negative spherical aberration imaging, is suitable for atom-counting as well. The capabilities of both imaging techniques are investigated and compared using the probability of error as a criterion. It is shown that for the same incoming electron dose, HR STEM outperforms HR TEM under common practice standards, i.e. when the decision is based on the probability function of the peak intensities in HR TEM and of the scattering cross-sections in HR STEM. If the atom-counting decision is based on the joint probability function of the image pixel values, the dependence of all image pixel intensities as a function of thickness should be known accurately. Under this assumption, the probability of error may decrease significantly for atom-counting in HR TEM and may, in theory, become lower as compared to HR STEM under the predicted optimal experimental settings. However, the commonly used standard for atom-counting in HR STEM leads to a high performance and has been shown to work in practice. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Analysis of Premature Wear-Out of Aircraft Gun Barrel by Applying a Transmission Electron Microscopy (TEM

    Directory of Open Access Journals (Sweden)

    Łęczycki Krzysztof

    2017-08-01

    Full Text Available Firing from gun armament generates a wide range of physico-chemical phenomena contributing to the degradation of barrel material, e.g. pressure, high temperature, chemically aggressive character of post-detonation gases and friction of a driving band. In this work the technique of thin foils was used in Transmission Electron Microscopy (TEM to study the influence of physicochemical phenomena on the material microstructure of aircraft gun barrel. A mechanism and reason of premature wear-out of the barrel under consideration was also outlined by utilising light microscopy and hardness measurements.

  11. Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

    Science.gov (United States)

    Kim, Hyun Jung; Choi, Sang H.; Bae, Hyung-Bin; Lee, Tae Woo

    2012-01-01

    The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

  12. Experimental study on propagation properties of large size TEM antennas

    International Nuclear Information System (INIS)

    Zhang Guowei; Wang Haiyang; Chen Weiqing; Wang Wei; Zhu Xiangqin; Xie Linshen

    2014-01-01

    The propagation properties of large size TEM antennas were studied by experiment. The size of the TEM antennas is 60 m × 20 m × 10 m and the character Impedance is 120 Ω. A kind of dielectric foil switch is designed compactly with TEM antennas which can generate double exponential waveform with altitude of 10 kV and rise time of l.2 ns. The radiated field distribution was measured. The relationship between rise time/altitude and distance were provided, and the propagation properties of large size TEM antennas were summarized. (authors)

  13. Direct Observations of Oxygen-induced Platinum Nanoparticle Ripening Studied by In Situ TEM

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose; Chorkendorff, Ib; Dahl, Søren

    2010-01-01

    This study addresses the sintering mechanism of Pt nanoparticles dispersed on a planar, amorphous Al2O3 support as a model system for a catalyst for automotive exhaust abatement. By means of in situ transmission electron microscopy (TEM), the model catalyst was monitored during the exposure to 10...

  14. Atomic-resolution environmental TEM for quantitative in-situ microscopy in materials science.

    Science.gov (United States)

    Takeda, Seiji; Yoshida, Hideto

    2013-02-01

    We have compiled our recent in-situ quantitative environmental transmission electron microscopy (ETEM) studies on typical gold nanoparticulate catalysts for the low-temperature oxidation of CO to describe the issues surrounding the application of ETEM, with a special regard to catalyst chemistry. Thanks to the recent development of high-resolution environmental transmission electron microscopes that can work robustly to accumulate observation data in controlled environments, we can deal with the electron irradiation effects and heterogeneity of real catalysts. We established a structural evolution diagram that summarizes the structure of catalysts under electron irradiation as a function of the electron current density ϕ and the electron dose, D. By extrapolating to ϕ = 0, D = 0, we could deduce the intrinsic catalysis structure (without electron irradiation) in various environments, including reaction environments. By numerically and statistically analyzing a substantial number of ETEM images of gold nanoparticles, we established a morphology phase diagram that summarizes how the majority of gold nanoparticles change their morphology systematically as a function of the partial pressures of CO and O(2). Similar diagrams will be helpful in elucidating the phenomena that directly correlate with the catalytic activity determined from ETEM observations. Using these quantitative analyses, we could analyze Cs-corrected ETEM images of the catalysts. The surfaces of gold nanoparticles were structurally reconstructed under reaction conditions, via interactions with CO molecules. CO molecules were observed on the surfaces of catalysts under reaction conditions using high-resolution ETEM. Finally, we discuss the potential of environmental transmission electron microscopy for quantitative in-situ microscopy at the atomic scale.

  15. SOFC anode reduction studied by in situ TEM

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose; Wagner, Jakob Birkedal; Hansen, Thomas Willum

    The Solid Oxide Fuel Cell (SOFC) is a promising part of future energy approaches due to a relatively high energy conversion efficiency and low environmental pollution. SOFCs are typically composed of ceramic materials which are highly complex at the nanoscale. TEM is routinely applied ex situ...... for studying these nanoscale structures, but only few SOFC studies have applied in situ TEM to observe the ceramic nanostructures in a reactive gas environment at elevated temperatures. The present contribution focuses on the reduction of an SOFC anode which is a necessary process to form the catalytically...... active Ni surface before operating the fuel cells. The reduction process was followed in the TEM while exposing a NiO/YSZ (YSZ = Y2O3-stabilized ZrO2) model anode to H2 at T = 250-1000⁰C. Pure NiO was used in reference experiments. Previous studies have shown that the reduction of pure Ni...

  16. SIMS and TEM study on oxide characteristics of Zircaloy

    International Nuclear Information System (INIS)

    Jung, Y. H.; Baek, J. H.; Kim, S. J.; Kim, K. H.; Choi, B. K.; Jung, Y. H.

    1998-01-01

    Long-term corrosion test, SIMS analysis, and TEM study were carried out to investigate the corrosion characteristics and corrosion mechanism of Zircaloy-4 in LiOH solution. The corrosion tests were performed in alkali solutions at 350 deg C for 500days. SIMS analysis was performed for the specimens prepared to have an equal oxide thickness to measure the cation content. TEM studies on the samples formed in various alkali solutions were also conducted. Based on the corrosion test, SIMS analysis, and TEM study, the cation is considered to control the corrosion in LiOH solution and its effect is dependent on the concentration of alkali and the oxide thickness. The slight acceleration of corrosion rate at a low concentration is thought to be caused by the cation incorporation into oxide while the significant acceleration at a high concentration is due to the transformation of oxide microstructure that would be induced by the cation incorporation

  17. TEM and Moessbauer Study of Nano Sized Fe2MnAl Flakes

    International Nuclear Information System (INIS)

    Vinesh, A.; Sudheesh, V. D.; Lakshmi, N.; Venugopalan, K.

    2011-01-01

    Magnetic and structural properties of L21 ordered Fe 2 MnAl Heusler alloy have been studied by X-ray diffraction, Transmission electron microscopy (TEM), Moessbauer spectroscopy and DC magnetization. Structural texturing induced by ball milling is destroyed on heating while Moessbauer and DC magnetization studies show magnetic texturing persists after thermal treatment. TEM shows large distribution in particle size with an average size of 27 nm. Thermal annealing of ball milled sample results L2 1 ordering and the needle shaped particle contributes spin texturing.

  18. SANS and TEM studies of carbide precipitation and creep damage in type 304 stainless steel

    International Nuclear Information System (INIS)

    Yoo, M.H.; Ogle, J.C.; Schneibel, J.H.; Swindeman, R.W.

    1984-01-01

    Small-angle neutron scattering (SANS) and transmission electron microscopy (TEM) studies were performed to characterize the carbide (M 23 C 6 ) precipitation and creep damage induced in type 304 stainless steel in the primary creep stage. The size distribution of matrix carbides evaluated from SANS analyses was consistent with TEM data, and the expected accelerated kinetics of precipitation under applied stress was confirmed. Additional SANS measurements after the postcreep solution annealing were made in order to differentiate cavities from the carbides. Potential advantages and difficulties associated with characterization of creep-induced cavitation by the SANS techniques are discussed

  19. Towards 3D crystal orientation reconstruction using automated crystal orientation mapping transmission electron microscopy (ACOM-TEM).

    Science.gov (United States)

    Kobler, Aaron; Kübel, Christian

    2018-01-01

    To relate the internal structure of a volume (crystallite and phase boundaries) to properties (electrical, magnetic, mechanical, thermal), a full 3D reconstruction in combination with in situ testing is desirable. In situ testing allows the crystallographic changes in a material to be followed by tracking and comparing the individual crystals and phases. Standard transmission electron microscopy (TEM) delivers a projection image through the 3D volume of an electron-transparent TEM sample lamella. Only with the help of a dedicated TEM tomography sample holder is an accurate 3D reconstruction of the TEM lamella currently possible. 2D crystal orientation mapping has become a standard method for crystal orientation and phase determination while 3D crystal orientation mapping have been reported only a few times. The combination of in situ testing with 3D crystal orientation mapping remains a challenge in terms of stability and accuracy. Here, we outline a method to 3D reconstruct the crystal orientation from a superimposed diffraction pattern of overlapping crystals without sample tilt. Avoiding the typically required tilt series for 3D reconstruction enables not only faster in situ tests but also opens the possibility for more stable and more accurate in situ mechanical testing. The approach laid out here should serve as an inspiration for further research and does not make a claim to be complete.

  20. Coarsening of Pd nanoparticles in an oxidizing atmosphere studied by in situ TEM

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose; Chorkendorff, Ib; Dahl, Søren

    2016-01-01

    The coarsening of supported palladium nanoparticles in an oxidizing atmosphere was studied in situ by means of transmission electron microscopy (TEM). Specifically, the Pd nanoparticles were dispersed on a planar and amorphous Al2O3 support and were observed during the exposure to 10 mbar technical...... for the Ostwald ripening process indicates that the observed change in the particle size distribution can be accounted for by wetting of the Al2O3 support by the larger Pd nanoparticles....

  1. TEM studies of plasma nitrided austenitic stainless steel.

    Science.gov (United States)

    Stróz, D; Psoda, M

    2010-03-01

    Cross-sectional transmission electron microscopy and X-ray phase analysis were used to study the structure of a layer formed during nitriding the AISI 316L stainless steel at temperature 440 degrees C. It was found that the applied treatment led to the formation of 6-microm-thick layer of the S-phase. There is no evidence of CrN precipitation. The X-ray diffraction experiments proved that the occurred austenite lattice expansion - due to nitrogen atoms - depended on the crystallographic direction. The cross-sectional transmission electron microscopy studies showed that the layer consisted of a single cubic phase that contained a lot of defects such as dislocations, stacking faults, slip bands and twins. The high-resolution electron microscopy observations were applied to study the defect formation due to the nitriding process. It was shown that the presence of great number of stacking faults leads to formation of nanotwins. Weak, forbidden {100} reflections were still another characteristic feature of the S-phase. These were not detected in the X-ray spectra of the phase. Basing on the high-resolution electron microscopy studies it can be suggested that the short-range ordering of the nitrogen atoms in the octahedral sites inside the f.c.c. matrix lattice takes place and gives rise to appearance of these spots. It is suggested that the cubic lattice undergoes not only expansion but also slight rombohedral distortion that explains differences in the lattice expansion for different crystallographic directions.

  2. A TEM Study on the Microstructure of Fine Flaky Graphite

    DEFF Research Database (Denmark)

    Moumeni, Elham; Tiedje, Niels Skat; Horsewell, Andy

    In this investigation the microstructure of the graphite flakes in titanium alloyed cast iron is studied using electron microscopy techniques. Based on this information, growth models for the platelets in the fine graphite flakes in cast iron are considered. Detailed crystallographic analysis...... of the defects observed such as multiple twin boundaries and possible spiral growth configurations are required...

  3. Use of atomic force microscopy and transmission electron microscopy for correlative studies of bacterial capsules.

    Science.gov (United States)

    Stukalov, Oleg; Korenevsky, Anton; Beveridge, Terry J; Dutcher, John R

    2008-09-01

    Bacteria can possess an outermost assembly of polysaccharide molecules, a capsule, which is attached to their cell wall. We have used two complementary, high-resolution microscopy techniques, atomic force microscopy (AFM) and transmission electron microscopy (TEM), to study bacterial capsules of four different gram-negative bacterial strains: Escherichia coli K30, Pseudomonas aeruginosa FRD1, Shewanella oneidensis MR-4, and Geobacter sulfurreducens PCA. TEM analysis of bacterial cells using different preparative techniques (whole-cell mounts, conventional embeddings, and freeze-substitution) revealed capsules for some but not all of the strains. In contrast, the use of AFM allowed the unambiguous identification of the presence of capsules on all strains used in the present study, including those that were shown by TEM to be not encapsulated. In addition, the use of AFM phase imaging allowed the visualization of the bacterial cell within the capsule, with a depth sensitivity that decreased with increasing tapping frequency.

  4. TEM study of the ion beam induced damage during 14 kev P+ implantation in silicon

    International Nuclear Information System (INIS)

    Rubanov, S.; Tamanyan, G.; Hudson, F.; Jamieson, D.N.; McCallum, J.C.; Prawer, S.

    2005-01-01

    The proposed silicon-based quantum computer architecture comprises an array of phosphorus donor atoms (qubits) positioned with nanometre accuracy beneath the surface of a semiconductor host, using a single ion implantation technique. The average depth of the implanted ions (the projected range R p ), lateral range R p 1, and the distribution of ions about that depth can be approximated as two-dimensional Gaussian with standard deviation ΔR p and ΔR p 1 (lateral straggle). Using transmission electron microscopy (TEM) we studied ion beam induced damage after 14 keV P + implantation in Si. The TEM images allowed us to compare the depth of the amorphous cluster formation to R p , R p 1, ΔR p 1 calculated from SRIM and hence determine evidence for the limitation on the accuracy of the position of the implanted ions imposed by straggling. (author). 4 refs., 3 figs

  5. Coordinated Isotopic and TEM Studies of Presolar Graphites from Murchison

    Science.gov (United States)

    Croat, T. K.; Stadermann, F. J.; Zinner, E.; Bernatowicz, T. J.

    2004-03-01

    TEM and NanoSIMS investigations of the same presolar Murchison KFC graphites revealed high Zr, Mo, and Ru content in refractory carbides within the graphites. Along with isotopically light carbon, these suggest a low-metallicity AGB source.

  6. In vitro safety assessment of papain on human skin: A qualitative Light and Transmission Electron Microscopy (TEM study Avaliação in vitro da segurança de uso da papaína em pele humana: Estudo qualitativo por microscopia de luz e eletrônica de transmissão (MET

    Directory of Open Access Journals (Sweden)

    Patrícia Santos Lopes

    2008-03-01

    Full Text Available Papain is a thiol proteolytic enzyme widely used in dermatology that found applications in wound treatment. Recently, papain was also used as absorption enhancer which can modify the peptide/protein material in the bilayer domain. We investigated papain safety using human skin that was exposed to papain in vitro at different times: 4, 24 and 48 hours. The samples were examined using Light and Transmission Electron Microscopy (TEM to study of the mechanisms involved in enhancer-skin interaction. After 24 hours, changes occurred in corneosomes. However, samples of 48 hours did not show major changes in agreement with the control. These findings indicated that papain could be used safely onto the skin.Papaína é uma enzima proteolítica amplamente utilizada na dermatologia para o tratamento de feridas. Atualmente, a papaína também tem sido empregada como promotor de absorção cutânea passível de modificar os domínios protéicos da epiderme. Nesta pesquisa investigou-se in vitro a segurança da papaína, utilizando pele humana exposta a enzima em diferentes períodos de tempo de contato: 4, 24 e 48 horas. As amostras foram avaliadas por Microscopia de Luz e Eletrônica de Transmissão (MET, técnicas que podem ser utilizadas no estudo dos mecanismos envolvidos na interação de promotores de absorção cutânea e a pele. Após 24 horas de contato entre a pele a solução de papaína, mudanças ocorreram nos corneossomos, no entanto, as amostras em contato por 24 horas não evidenciaram alterações relevantes comparadas com o controle. Os resultados indicaram que a papaína poderia ser seguramente aplicada sobre a pele.

  7. TEM study of impurity segregations in beryllium pebbles

    Energy Technology Data Exchange (ETDEWEB)

    Klimenkov, M., E-mail: michael.klimenkov@kit.edu [Institute for Applied Materials – Applied Materials Physics, Karlsruhe Institute of Technology, Hermann-von-Helmholz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Chakin, V.; Moeslang, A. [Institute for Applied Materials – Applied Materials Physics, Karlsruhe Institute of Technology, Hermann-von-Helmholz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Rolli, R. [Institute for Applied Materials – Materials and Biomechanics, Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany)

    2014-12-15

    Beryllium is planned to be used as a neutron multiplier in the Helium-cooled Pebble Bed European concept of a breeding blanket of demonstration power reactor DEMO. In order to evaluate the irradiation performance, individual pebbles and constrained pebble beds were neutron-irradiated at temperatures typical of fusion blankets. Beryllium pebbles 1 mm in diameter produced by the rotating electrode method were subjected to a TEM study before and after irradiation at High Flux Reactor, Petten, Netherlands at 861 K. The grain size varied in a wide range from sub-micron size up to several tens of micrometers, which indicated formation bimodal grain size distribution. Based on the application of combined electron energy loss spectroscopy and energy dispersive X-ray spectroscopy methods, we suggest that impurity precipitates play an important role in controlling the mechanical properties of beryllium. The impurity elements were present in beryllium at a sub-percent concentration form beryllide particles of a complex (Fe/Al/Mn/Cr)B composition. These particles are often ordered along dislocations lines, forming several micron-long chains. It can be suggested that fracture surfaces often extended along these chains in irradiated material.

  8. Synthesis, XRD, TEM, EPR, and Optical Absorption Spectral Studies of CuZnO2 Nanocompound

    Directory of Open Access Journals (Sweden)

    T. Ravindra Reddy

    2014-01-01

    Full Text Available Synthesis of nano CuZnO2 compound is carried out by thermal decomposition method. The crystalline phase of the material is characterized by XRD. The calculated unit cell constants are a=3.1 Å and c=3.4786 Å and are of tetragonal structure. The unit cell constants are different from wurtzite (hexagonal which indicate that a nanocompound is formed. Further TEM images reveal that the metal ion is in tetragonal structure with oxygen ligands. The prepared CuZnO2 is then characterized for crystallite size analysis by employing transmission electron microscopy (TEM. The size is found to be 100 nm. Uniform bright rings are noticed in the TEM picture suggesting that the nanocrystals have preferential instead of random orientations. The selected-area electron diffraction (SAED pattern clearly indicates the formation of CuO-ZnO nanocompound. The nature of bonding is studied by electron paramagnetic resonance (EPR. The covalency character is about 0.74 and thus the compound is electrically less conductive. Optical absorption spectral studies suggest that Cu(II is placed in tetragonal elongation crystal field. The spin-orbit coupling constant, λ, is calculated using the EPR and optical absorption spectral results suggest some covalent bond between metal and ligand. Near infrared (NIR spectra are due to hydroxyl and water fundamentals.

  9. Studying the interface between cyanobacteria and biotite mineral surfaces using FIB and TEM

    International Nuclear Information System (INIS)

    Ward, M B; Brown, A P

    2014-01-01

    Recent analysis of the bioweathering of minerals has highlighted the challenges for investigating the interface between fungi or bacteria and the surface of the mineral that they live on. Transmission electron microscopy (TEM) with its ability to gather imaging information and collect elemental data at high spatial resolution is the ideal technique to analyse such interfaces. Further to this, a dual beam scanning electron and focused ion beam (FIB) microscope is an ideal instrument to prepare specimens for TEM because of its ability to simultaneously cut through hard and soft materials from specific sites of interest. There are however precautions that must be taken when analysing such mineral systems. The electron beam sensitive nature of most sheet silicate minerals means that consideration has to be made as to whether the structure and/or chemistry of the material is being altered during (S)TEM analysis. Here, results from a study of cyanobacteria grown on the surface of biotite are discussed. Particular reference is given to the methods used to determine an electron beam intensity threshold, below which STEM-EDX analysis could be performed without detrimental alteration to the mineral

  10. TEM studies of the crystal growth of indanthrone pigments

    International Nuclear Information System (INIS)

    McHendry, P.

    1998-01-01

    The aim of this work was to study the crystal growth of indanthrone during the pigmentation process. The colouring properties of a pigment are dependant on the chemical and crystallographic structure of the pigment. However, other factors are known to affect these properties including particle size, particle size distribution and level of dispersion in the chosen application medium. The parameters which affect the growth of the pigment particles were investigated with the emphasis placed on the mechanism by which growth took place. The final form of the crystals after growth was also investigated in some detail. Various electron microscopy techniques were employed in the investigations in this thesis. High and low magnification imaging and diffraction were studied on the CTEM (conventional transmission electron microscope) whilst PEELS (parallel electron energy loss spectroscopy) and DPC (differential phase contrast) studies took place on the VG HB5 STEM (scanning transmission electron microscope). In addition to these studies, x-ray diffraction and surface area analysis techniques were employed. The low magnification CTEM work gave good information on the size, shape and size distribution of the pigment particles and enabled detailed analysis of the level of growth attained under varied reaction conditions. (author)

  11. Low-pressure Environmental TEM (ETEM) studies of Au assisted MgO nanorod growth

    DEFF Research Database (Denmark)

    Duchstein, Linus Daniel Leonhard; Damsgaard, Christian Danvad; Hansen, Thomas Willum

    2012-01-01

    where they become inactive for CO oxidation. Here, we present an environmental transmission electron microscopy (ETEM) study of shape changes of Au nanoparticles supported on MgO in a controlled gas atmosphere, in order to elucidate the mobility of surface species and the configuration of the Au...... and interface structure of supported nanoparticles in a controlled environment [7]. This allows for a deeper understanding of the dynamic response of the surface and interface to changes in gas composition, pressure and temperature. Additionally, an Ultra High Vacuum (UHV) TEM has been used in order to have...... a higher degree of control of the initial state and probe the low-pressure regime. This combination is a powerful toolbox for charactering the behavior of the mobility of atomic species at the MgO surface leading to the formation of nanorods. Figure 1 shows Au particles on MgO cubes being irradiated...

  12. TEM study of radiation induced defects in baffle-former-barrel assembly from decommissioned NPP Greifswald

    International Nuclear Information System (INIS)

    Srba, O.; Michalicka, J.; Keilova, E.; Kocik, K.

    2013-06-01

    A complex transmission electron microscopy (TEM) study of reactor vessel internal (RVI) materials from the baffle-former-barrel assembly from NPP Greifswald (VVER 440), Unit 1 decommissioned after 15 service cycles has been undertaken. All parts of the baffle-former-barrel assembly are made from Ti-stabilized austenitic stainless steel 08Ch18N10T. The materials were exposed to different dose of neutron radiation (2.4 - 11.4 dpa) at temperatures 267 - 398 deg. C depending on position in the core. Three types of radiation induced defects were identified and quantified, namely: dislocations, cavities (voids) and fine-scaled precipitated particles of Ni-Si rich phases. Black-dot type defects were observed too. Operation conditions are around ≅ 300 deg. C that is why we have observed defect typical for both low and high regions of irradiation temperatures. (authors)

  13. TEM and XANES study of MOVPE grown InAIN layers with different indium content

    International Nuclear Information System (INIS)

    Kret, S; Wolska, A; Klepka, M T; Letrouit, A; Ivaldi, F; Szczepańska, A; Carlin, J-F; Kaufmann, N A K; Grandjean, N

    2011-01-01

    We present structure and spatially resolved composition studies by TEM (Transmission Electron Microscopy) and XANES (X-ray Absorption Near Edge Structure) of InAIN MOVPE (Metal-Organic Vapor Phase Epitaxy) epilayers containing 16-27 at% of indium. Investigations of the In L 3 edge by synchrotron radiation absorption show a significant change of the post-edge structure depending on the indium content. We attribute this to the solubility limit and phase separation in this system. Our measurements suggest that the critical composition is 18% for our growth conditions. HRTEM cross-sectional and EDX investigations confirm such phase separation as well as the changing of the structure from 2D growth to columnar like growth for the sample with the highest indium content.

  14. Visualising reacting single atoms under controlled conditions: Advances in atomic resolution in situ Environmental (Scanning) Transmission Electron Microscopy (E(S)TEM)

    Science.gov (United States)

    Boyes, Edward D.; Gai, Pratibha L.

    2014-02-01

    Advances in atomic resolution Environmental (Scanning) Transmission Electron Microscopy (E(S)TEM) for probing gas-solid catalyst reactions in situ at the atomic level under controlled reaction conditions of gas environment and temperature are described. The recent development of the ESTEM extends the capability of the ETEM by providing the direct visualisation of single atoms and the atomic structure of selected solid state heterogeneous catalysts in their working states in real-time. Atomic resolution E(S)TEM provides a deeper understanding of the dynamic atomic processes at the surface of solids and their mechanisms of operation. The benefits of atomic resolution-E(S)TEM to science and technology include new knowledge leading to improved technological processes with substantial economic benefits, improved healthcare, reductions in energy needs and the management of environmental waste generation. xml:lang="fr"

  15. Study of InGaN/GaN quantum dot systems by TEM techniques and photoluminescence spectroscopy

    International Nuclear Information System (INIS)

    Kashtiban, R J; Bangert, U; Harvey, A J; Sherliker, B; Halsall, M P

    2010-01-01

    InGaN/GaN multilayer quantum dot structures produced by MOCVD techniques on c-plane sapphire were studied by transmission electron microscopy (TEM) and photoluminescence (PL) techniques. Indium fluctuations ranging from 1-4 nm were observed with both energy filtered TEM (EFTEM) and high angle annular dark field (HAADF) scanning TEM. The existence of V-shaped defects with nucleation centres at the termination of threading dislocation were observed in HAADF images. There was also evidence of the formation of large quantum dots at low densities from lattice HRTEM images. This was further confirmed by PL measurements through the observation of a single sharp line at low power with the typical saturation behaviour at higher power excitation.

  16. TEM Study of High-Temperature Precipitation of Delta Phase in Inconel 718 Alloy

    Directory of Open Access Journals (Sweden)

    Moukrane Dehmas

    2011-01-01

    Full Text Available Inconel 718 is widely used because of its ability to retain strength at up to 650∘C for long periods of time through coherent metastable  Ni3Nb precipitation associated with a smaller volume fraction of  Ni3Al precipitates. At very long ageing times at service temperature,  decomposes to the stable Ni3Nb phase. This latter phase is also present above the  solvus and is used for grain control during forging of alloy 718. While most works available on precipitation have been performed at temperatures below the  solvus, it appeared of interest to also investigate the case where phase precipitates directly from the fcc matrix free of  precipitates. This was studied by X-ray diffraction and transmission electron microscopy (TEM. TEM observations confirmed the presence of rotation-ordered domains in plates, and some unexpected contrast could be explained by double diffraction due to overlapping phases.

  17. FIB and TEM studies of damage mechanisms in DLC coatings sliding against aluminum

    International Nuclear Information System (INIS)

    Meng-Burany, X.; Alpas, A.T.

    2007-01-01

    Material transfer and adhesion phenomena during sliding contact of non-hydrogenated diamond like carbon (DLC) coatings against an aluminum-silicon (319 Al) counterface tested in vacuum were studied using TEM investigations of the cross-sectional microstructures of the wear tracks. Site-specific focused ion beam (FIB) lift-out method was used to prepare the sections at the precise locations where aluminum pieces were adhered to the DLC surface. The dense amorphous structure of DLC coatings with nanocrystalline graphite platelets is confirmed by the high-resolution transmission electron microscopy. The focused ion channeling contrast images obtained from the cross-sections of the wear track indicated that in some sections of DLC coatings considerable wear was inflicted by aluminum, reducing the coating thickness. The aluminum that was transferred on the DLC coatings' contact surfaces consisted of nanocrystalline grains of less than 100 nm. TEM examination of the contact surface of the 319 Al pin has revealed that the initial aluminum grain size was also reduced to the nanocrystalline scale and this was accompanied with a hardness increase. These observations revealed that local severe plastic deformation accompanied the aluminum adhesion process to DLC coating surfaces

  18. Present status and future prospects of spherical aberration corrected TEM/STEM for study of nanomaterials

    International Nuclear Information System (INIS)

    Tanaka, Nobuo

    2008-01-01

    The present status of Cs-corrected TEM/STEM is described from the viewpoint of the observation of nanomaterials. Characteristic features in TEM and STEM are explained using the experimental data obtained by our group and other research groups. Cs correction up to the 3rd-order aberration of an objective lens has already been established and research interest is focused on correcting the 5th-order spherical aberration and the chromatic aberration in combination with the development of a monochromator below an electron gun for smaller point-to-point resolution in optics. Another fundamental area of interest is the limitation of TEM and STEM resolution from the viewpoint of the scattering of electrons in crystals. The minimum size of the exit-wave function below samples undergoing TEM imaging is determined from the calculation of scattering around related atomic columns in the crystals. STEM does not have this limitation because the resolution is, in principle, determined by the probe size. One of the future prospects of Cs-corrected TEM/STEM is the possibility of extending the space around the sample holder by correcting the chromatic and spherical aberrations. This wider space will contribute to the ease of performing in situ experiments and various combinations of TEM and other analysis methods. High-resolution, in situ dynamic and 3D observations/analysis are the most important keywords in the next decade of high-resolution electron microscopy. (topical review)

  19. TEM study of amorphous alloys produced by ion implantation

    International Nuclear Information System (INIS)

    Johnson, E.; Grant, W.A.; Wohlenberg, P.; Hansen, P.; Chadderton, L.T.

    1978-01-01

    Ion implantation is a technique for introducing foreign elements into surface layers of solids. Ions, as a suitably accelerated beam, penetrate the surface, slow down by collisions with target atoms to produce a doped layer. This non-equilibrium technique can provide a wide range of alloys without the restrictions imposed by equilibrium phase diagrams. This paper reports on the production of some amorphous transition metal-metalloid alloys by implantation. Thinned foils of Ni, Fe and stainless steel were implanted at room temperature with Dy + and P + ions at doses between 10 13 - 10 17 ions/cm 2 at energies of 20 and 40 keV respectively. Transmission electron microscopy and selected area diffraction analysis were used to investigate the implanted specimens. Radial diffracted intensity measurements confirmed the presence of an amorphous implanted layer. The peak positions of the maxima are in good agreement with data for similar alloys produced by conventional techniques. Only certain ion/target combinations produce these amorphous layers. Implantations at doses lower than those needed for amorphization often result in formation of new crystalline phases such as an h.c.p. phase in nickel and a b.c.c. phase in stainless steel. (Auth.)

  20. Native oxide formation on pentagonal copper nanowires: A TEM study

    Science.gov (United States)

    Hajimammadov, Rashad; Mohl, Melinda; Kordas, Krisztian

    2018-06-01

    Hydrothermally synthesized copper nanowires were allowed to oxidize in air at room temperature and 30% constant humidity for the period of 22 days. The growth of native oxide layer was followed up by high-resolution transmission electron microscopy and diffraction to reveal and understand the kinetics of the oxidation process. Copper oxides appear in the form of differently oriented crystalline phases around the metallic core as a shell-like layer (Cu2O) and as nanoscopic islands (CuO) on the top of that. Time dependent oxide thickness data suggests that oxidation follows the field-assisted growth model at the beginning of the process, as practically immediately an oxide layer of ∼2.8 nm thickness develops on the surface. However, after this initial rapid growth, the local field attenuates and the classical parabolic diffusion limited growth plays the main role in the oxidation. Because of the single crystal facets on the side surface of penta-twinned Cu nanowires, the oxidation rate in the diffusion limited regime is lower than in polycrystalline films.

  1. Early studies of placental ultrastructure by electron microscopy

    DEFF Research Database (Denmark)

    Carter, A M; Enders, A C

    2016-01-01

    many other scientists to Washington University in St. Louis. Work on human placental ultrastructure was initiated at Cambridge and Kyoto whilst domestic animals were initially studied by Björkman in Stockholm and electron micrographs of bat placenta were published by Wimsatt of Cornell University......BACKGROUND: Transmission electron microscopy (TEM) was first applied to study placental ultrastructure in the 1950's. We review those early studies and mention the scientists that employed or encouraged the use of TEM. FINDINGS: Among the pioneers Edward W. Dempsey was a key figure who attracted...

  2. Strain study of gold nanomaterials as HR-TEM calibration standard.

    Science.gov (United States)

    Peng, X Y; Zhou, L Q; Li, X; Tao, X F; Ren, L L; Cao, W H; Xu, G F

    2015-12-01

    This work presents the use of high resolution electron microscopy (HREM) and geometric phase analysis (GPA) to measure the interplanar spacing and strain distribution of three gold nanomaterials, respectively. The results showed that the {111} strain was smaller than the {002} strain for any kind of gold materials at the condition of same measuring method. The 0.65% of {111} strain in gold film measured by HREM (0.26% measured by GPA) was smaller than the {111} strains in two gold particles. The presence of lattice strain was interpreted according to the growth mechanism of metallic thin film. It is deduced that the {111} interplanar spacing of the gold thin film is suitable for high magnification calibration of transmission electron microscopy (TEM) and the gold film is potential to be a new calibration standard of TEM. Copyright © 2015 Elsevier Ltd. All rights reserved.

  3. Characterization of duplex stainless steels by TEM [transmission electron microscopy], SANS [small-angle neutron scattering], and APFIM [atom-probe field ion microscopy] techniques

    International Nuclear Information System (INIS)

    Chung, H.M.; Chopra, O.K.

    1987-06-01

    Results are presented of complementary characterization of aged duplex stainless steels by advanced metallographic techniques, including transmission and high-voltage electron microscopies; small-angle neutron scattering; and atom-probe field ion microscopy. On the basis of the characterization, the mechanisms of aging embrittlement have been shown to be associated with the precipitation of Ni- and Si-rich G phase and Cr-rich α' in the ferrite, and M 23 C 6 carbides on the austenite-ferrite phase boundaries. 19 refs., 19 figs., 1 tab

  4. U-Zr alloy: XPS and TEM study of surface passivation

    Science.gov (United States)

    Paukov, M.; Tkach, I.; Huber, F.; Gouder, T.; Cieslar, M.; Drozdenko, D.; Minarik, P.; Havela, L.

    2018-05-01

    Surface reactivity of Uranium metal is an important factor limiting its practical applications. Bcc alloys of U with various transition metals are much less reactive than pure Uranium. So as to specify the mechanism of surface protection, we have been studying the U-20 at.% Zr alloy by photoelectron spectroscopy and transmission electron microscopy. The surface was studied in as-obtained state, in various stages of surface cleaning, and during an isochronal annealing cycle. The analysis based on U-4f, Zr-3p, and O-1 s spectra shows that a Zr-rich phase segregates at the surface at temperatures exceeding 550 K, which provides a self-assembled coating. The comparison of oxygen exposure of the stoichiometric and coated surfaces shows that the coating is efficiently preventing the oxidation of uranium even at elevated temperatures. The coating can be associated with the UZr2+x phase. TEM study indicated that the coating is about 20 nm thick. For the clean state, the U-4f core-level lines of the bcc alloy are practically identical to those of α-U, revealing similar delocalization of the 5f electronic states.

  5. TEM studies of domain formation mechanisms in MnV{sub 2}O{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Murakami, Y., E-mail: murakami@tagen.tohoku.ac.jp [Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, Sendai 980-8577 (Japan); Advanced Science Institute, RIKEN, Wako 351-0198 (Japan); Nii, Y.; Arima, T. [Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, Sendai 980-8577 (Japan); Shindo, D. [Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, Sendai 980-8577 (Japan); Advanced Science Institute, RIKEN, Wako 351-0198 (Japan); Yanagisawa, K. [Advanced Science Institute, RIKEN, Wako 351-0198 (Japan); Okinawa Institute of Science and Technology, Onna-son, Okinawa 904-0412 (Japan); Tonomura, A. [Advanced Science Institute, RIKEN, Wako 351-0198 (Japan); Central Research Laboratory, Hitachi Ltd., Hatoyama 350-0395 (Japan); Okinawa Institute of Science and Technology, Onna-son, Okinawa 904-0412 (Japan)

    2013-11-15

    Highlights: ► Irregular shape of the phase boundary, due to the small transformation strain. ► TEM studies demonstrate the essential reduction of net magnetization by cooling. ► Twining morphology provides a key to understating of the anomalous magnetic domains. -- Abstract: Crystallographic and magnetic domains produced in a spinel-type compound MnV{sub 2}O{sub 4}, which exhibits a type of giant magnetostriction attributed to twin boundary motion, have been studied using transmission electron microscopy techniques. Although MnV{sub 2}O{sub 4} undergoes a displacive cubic-to-tetragonal transformation upon cooling, it does not show a well-defined habit plane (i.e. the plane with a specific index that is favored for minimizing the transformation) due to the small elongation/contraction in the lattice. Electron holography demonstrates a considerable reduction in the magnetic signal by cooling the tetragonal phase to 40 K. Despite the elimination of micrometer-scale ferrimagnetic domains, weak magnetic contrast still remained, indicating small residual magnetic domains in particular portions, such as in the crosshatch of twinning pairs.

  6. First ultrastructural data on the human tapeworm Taenia asiatica eggs by scanning and transmission electron microscopy (SEM, TEM).

    Science.gov (United States)

    Galán-Puchades, M Teresa; Yang, Yichao; Marcilla, Antonio; Choe, Seongjun; Park, Hansol; Osuna, Antonio; Eom, Keeseon S

    2016-09-01

    Humans are definitive hosts of three species of the Taenia genus, namely Taenia solium, Taenia saginata and Taenia asiatica. The relative novelty of the latter explains the lack of knowledge concerning certain relevant aspects related to this parasite, such as its definite geographical distribution and whether its eggs can infect humans or not. So far, only the eggs of T. solium are known to be infective for humans, producing cysticercosis. Although eggs contain the infective stage, the oncosphere, there is a lack of research on the ultrastructure of eggs of human taeniids. We show, for the first time, the ultrastructure of eggs of T. asiatica by means of SEM and TEM analyses. We detected all the envelopes, namely the egg shell, vitelline layer, outer embryophoric membrane, embryophore, granular layer, basal membrane, oncospheral membrane and oncospheral tegument. Hooks surrounded by myofibrils and glycogen-like particles, the two types of secretory granules of the penetration glands, as well as several nuclei and mitochondria were also revealed in the oncospheres. In addition to the already known structures in eggs from other Taenia species, the presence of two types of small vesicles is described herein, possibly corresponding to exosomes and ectosomes because of their shape and size, which could participate in the host/parasite intercellular communication.

  7. TEM and ellipsometry studies of nanolaminate oxide films prepared using atomic layer deposition

    Energy Technology Data Exchange (ETDEWEB)

    Mitchell, D.R.G. [Materials and Engineering Science, ANSTO, PMB 1, Menai, NSW 2234 (Australia)]. E-mail: drm@ansto.gov.au; Attard, D.J. [Materials and Engineering Science, ANSTO, PMB 1, Menai, NSW 2234 (Australia); Finnie, K.S. [Materials and Engineering Science, ANSTO, PMB 1, Menai, NSW 2234 (Australia); Triani, G. [Materials and Engineering Science, ANSTO, PMB 1, Menai, NSW 2234 (Australia); Barbe, C.J. [Materials and Engineering Science, ANSTO, PMB 1, Menai, NSW 2234 (Australia); Depagne, C. [Materials and Engineering Science, ANSTO, PMB 1, Menai, NSW 2234 (Australia); Bartlett, J.R. [Materials and Engineering Science, ANSTO, PMB 1, Menai, NSW 2234 (Australia)

    2005-04-30

    Nanolaminate oxide layers consisting of TiO{sub 2} and Al{sub 2}O{sub 3} have been deposited on silicon using atomic layer deposition (ALD). Characterisation of these films has been achieved by use of a range of modern transmission electron microscopy (TEM)-based techniques, including plasmon loss imaging, energy filtered imaging and scanning TEM (STEM) X-ray line profiling. These have shown that the target thickness of the individual layers in the nanolaminate structures (20 nm) has been met with a high degree of accuracy, that the layers are extremely flat and parallel and that the interfaces between the layers are compositionally abrupt. Localised crystallisation within the stacks, and responses to electron beam irradiation point to the presence of a stress gradient within the layers. The performance of ellipsometry in characterising multilayer stacks has been benchmarked against the TEM measurements. Errors in determination of individual layer thicknesses were found to increase with growing stack size, as expected given the increasing number of interfaces incorporated in each model. The most sophisticated model gave maximum deviations of {+-}4 nm from the TEM determined values for the 5- and 10-layer stacks.

  8. Nanoparticle sizing: a comparative study using atomic force microscopy, transmission electron microscopy, and ferromagnetic resonance

    International Nuclear Information System (INIS)

    Lacava, L.M.; Lacava, B.M.; Azevedo, R.B.; Lacava, Z.G.M.; Buske, N.; Tronconi, A.L.; Morais, P.C.

    2001-01-01

    Atomic force microscopy (AFM), transmission electron microscopy (TEM), and ferromagnetic resonance (FMR) were used to unfold the nanoparticle size of a ferrofluid sample. Compared to TEM, the AFM method showed a nanoparticle diameter (D m ) reduction of 20% and standard deviation (σ) increase of 15%. The differences in D m and σ were associated with the AFM tip and the nanoparticle concentration on the substrate

  9. In situ TEM study of the coarsening of carbon black supported Pt nanoparticles in hydrogen

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose; Wang, Yan; Jensen, Jens Oluf

    2017-01-01

    The control of sizes and shapes of nanostructures is of tremendous importance for the catalytic activity in electrochemistry and in catalysis more generally. However, due to relatively large surface free energies, nanostructures often sinter to form coarser and more stable structures that may...... not have the intended physicochemical properties. Pt is known to be a very active catalyst in several chemical reactions and for example as carbon supported nanoparticles in fuel cells. The presentation focusses on coarsening mechanisms of Pt nanoparticles supported on carbon black during exposure...... to hydrogen. By means of in situ transmission electron microscopy (TEM), Pt nanoparticle coarsening was monitored in 6 mbar 20 % H2/Ar while ramping up the temperature to ca. 900 °C. Time-resolved TEM images directly reveal that separated ca. 3 nm sized Pt nanoparticles in the pure hydrogen environment...

  10. Recent advances in FIB-TEM specimen preparation techniques

    International Nuclear Information System (INIS)

    Li Jian; Malis, T.; Dionne, S.

    2006-01-01

    Preparing high-quality transmission electron microscopy (TEM) specimens is of paramount importance in TEM studies. The development of the focused ion beam (FIB) microscope has greatly enhanced TEM specimen preparation capabilities. In recent years, various FIB-TEM foil preparation techniques have been developed. However, the currently available techniques fail to produce TEM specimens from fragile and ultra-fine specimens such as fine fibers. In this paper, the conventional FIB-TEM specimen preparation techniques are reviewed, and their advantages and shortcomings are compared. In addition, a new technique suitable to prepare TEM samples from ultra-fine specimens is demonstrated

  11. In-situ TEM study of dislocation patterning during deformation in single crystal aluminum

    International Nuclear Information System (INIS)

    Landau, P; Shneck, R Z; Makov, G; Venkert, A

    2010-01-01

    The evolution of dislocation patterns in single crystal aluminum was examined using transmission electron microscopy (TEM). In-situ tensile tests of single crystals were carried out in a manner that activated double slip. Cross slip of dislocations, which is prominent in all stages of work hardening, plays an important role in dislocation motion and microstructural evolution. In spite of the limitations of in-situ straining to represent bulk phenomena, due to surface effects and the thickness of the samples, it is shown that experiments on prestrained samples can represent the early stages of deformation. Transition between stage I and stage II of work hardening and evolution during stage III were observed.

  12. TEM study of microstructure in explosive welded joints between Zircaloy-4 and stainless steel

    International Nuclear Information System (INIS)

    Zhou Hairong; Zhou Bangxin

    1996-10-01

    The microstructure of explosive welded joints between Zircaloy-4 and 18/8 stainless steel has been investigated by transmission electron microscopy (TEM). The metallurgical bonding was achieved by combining effect of diffusion and local melting when the explosive parameters were selected correctly. The molten region which consists of amorphous and crystalline with hexagonal crystal structure is hard and brittle. But the welded joints can be pulled, bent and cold rolled without cracks formed on the bonding layer, so as the molten regions are small and distributed as isolated islands. (6 refs., 6 figs., 1 tab.)

  13. Dynamics of electrochemical lithiation/delithiation of graphene-encapsulated silicon nanoparticles studied by in-situ TEM.

    Science.gov (United States)

    Luo, Langli; Wu, Jinsong; Luo, Jiayan; Huang, Jiaxing; Dravid, Vinayak P

    2014-01-24

    The incorporation of nanostructured carbon has been recently reported as an effective approach to improve the cycling stability when Si is used as high-capacity anodes for the next generation Li-ion battery. However, the mechanism of such notable improvement remains unclear. Herein, we report in-situ transmission electron microscopy (TEM) studies to directly observe the dynamic electrochemical lithiation/delithiation processes of crumpled graphene-encapsulated Si nanoparticles to understand their physical and chemical transformations. Unexpectedly, in the first lithiation process, crystalline Si nanoparticles undergo an isotropic to anisotropic transition, which is not observed in pure crystalline and amorphous Si nanoparticles. Such a surprising phenomenon arises from the uniformly distributed localized voltage around the Si nanoparticles due to the highly conductive graphene sheets. It is observed that the intimate contact between graphene and Si is maintained during volume expansion/contraction. Electrochemical sintering process where small Si nanoparticles react and merge together to form large agglomerates following spikes in localized electric current is another problem for batteries. In-situ TEM shows that graphene sheets help maintain the capacity even in the course of electrochemical sintering. Such in-situ TEM observations provide valuable phenomenological insights into electrochemical phenomena, which may help optimize the configuration for further improved performance.

  14. A Structural Study of Escherichia coli Cells Using an In Situ Liquid Chamber TEM Technology

    Directory of Open Access Journals (Sweden)

    Yibing Wang

    2015-01-01

    Full Text Available Studying cell microstructures and their behaviors under living conditions has been a challenging subject in microbiology. In this work, in situ liquid chamber TEM was used to study structures of Escherichia coli cells in aqueous solutions at a nanometer-scale resolution. Most of the cells remained intact under electron beam irradiation, and nanoscale structures were observed during the TEM imaging. The analysis revealed structures of pili surrounding the E. coli cells; the movements of the pili in the liquid were also observed during the in situ tests. This technology also allowed the observation of features of the nucleoid in the E. coli cells. Overall, in situ TEM can be applied as a valuable tool to study real-time microscopic structures and processes in microbial cells residing in native aqueous solutions.

  15. A preliminary study of CdS for solar cells using combined TEM and cathodoluminescence

    International Nuclear Information System (INIS)

    Mam, K.; Durose, K.; Halliday, D.P.; Szczerbakow, A.

    2005-01-01

    A study of the suitability of a combined transmission electron microscope (TEM)/cathodoluminescence (CL) imaging and spectroscopy apparatus for investigations of CdS is presented. Photoluminescence (PL) was used to evaluate the effect of the Ar + and I + ion beam thinning used in TEM specimen preparation of CdS: a minor increase in yellow emission (594 nm) resulted. However, excitation of luminescence spectra in the TEM had a quenching effect on red luminescence (734 nm), this being considered due to the high excitation density compared to that in PL. Significant electron beam damage to the CdS could be avoided by using scanning transmission electron microscope (STEM) illumination in preference to the conventional TEM mode, which generally uses higher beam current density. Dislocation images were correlated with contrast in the STEM-CL imaging mode. The potential of the apparatus to make further direct correlations of CL images with diffraction contrast TEM imaging was assessed using the Rose visibility criterion

  16. Electron microscopy methods in studies of cultural heritage sites

    Energy Technology Data Exchange (ETDEWEB)

    Vasiliev, A. L., E-mail: a.vasiliev56@gmail.com; Kovalchuk, M. V.; Yatsishina, E. B. [National Research Centre “Kurchatov Institute” (Russian Federation)

    2016-11-15

    The history of the development and application of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive X-ray microanalysis (EDXMA) in studies of cultural heritage sites is considered. In fact, investigations based on these methods began when electron microscopes became a commercial product. Currently, these methods, being developed and improved, help solve many historical enigmas. To date, electron microscopy combined with microanalysis makes it possible to investigate any object, from parchment and wooden articles to pigments, tools, and objects of art. Studies by these methods have revealed that some articles were made by ancient masters using ancient “nanotechnologies”; hence, their comprehensive analysis calls for the latest achievements in the corresponding instrumental methods and sample preparation techniques.

  17. Electron microscopy methods in studies of cultural heritage sites

    Science.gov (United States)

    Vasiliev, A. L.; Kovalchuk, M. V.; Yatsishina, E. B.

    2016-11-01

    The history of the development and application of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive X-ray microanalysis (EDXMA) in studies of cultural heritage sites is considered. In fact, investigations based on these methods began when electron microscopes became a commercial product. Currently, these methods, being developed and improved, help solve many historical enigmas. To date, electron microscopy combined with microanalysis makes it possible to investigate any object, from parchment and wooden articles to pigments, tools, and objects of art. Studies by these methods have revealed that some articles were made by ancient masters using ancient "nanotechnologies"; hence, their comprehensive analysis calls for the latest achievements in the corresponding instrumental methods and sample preparation techniques.

  18. Electron microscopy methods in studies of cultural heritage sites

    International Nuclear Information System (INIS)

    Vasiliev, A. L.; Kovalchuk, M. V.; Yatsishina, E. B.

    2016-01-01

    The history of the development and application of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive X-ray microanalysis (EDXMA) in studies of cultural heritage sites is considered. In fact, investigations based on these methods began when electron microscopes became a commercial product. Currently, these methods, being developed and improved, help solve many historical enigmas. To date, electron microscopy combined with microanalysis makes it possible to investigate any object, from parchment and wooden articles to pigments, tools, and objects of art. Studies by these methods have revealed that some articles were made by ancient masters using ancient “nanotechnologies”; hence, their comprehensive analysis calls for the latest achievements in the corresponding instrumental methods and sample preparation techniques.

  19. 2.5D Modeling of TEM Data Applied to Hidrogeological Studies in PARANÁ Basin, Brazil

    Science.gov (United States)

    Bortolozo, C. A.; Porsani, J. L.; Santos, F. M.

    2013-12-01

    The transient electromagnetic method (TEM) is used all over the world and has shown great potential in hydrological, hazardous waste site characterization, mineral exploration, general geological mapping, and geophysical reconnaissance. However, the behavior of TEM fields are very complex and is not yet fully understood. Forward modeling is one of the most common and effective methods to understand the physical behavior and significance of the electromagnetics responses of a TEM sounding. Until now, there are a limited number of solutions for the 2D forward problem for TEM. More rare are the descriptions of a three-component response of a 3D source over 2D earth, which is the so-called 2.5D. The 2.5D approach is more realistic than the conventional 2D source previous used, once normally the source cannot be realistic represented for a 2D approximation (normally source are square loops). At present the 2.5D model represents the only way of interpreting TEM data in terms of a complex earth, due to the prohibitive amount of computer time and storage required for a full 3D model. In this work we developed a TEM modeling program for understanding the different responses and how the magnetic and electric fields, produced by loop sources at air-earth interface, behave in different geoelectrical distributions. The models used in the examples are proposed focusing hydrogeological studies, once the main objective of this work is for detecting different kinds of aquifers in Paraná sedimentary basin, in São Paulo State - Brazil. The program was developed in MATLAB, a widespread language very common in the scientific community.

  20. 'In situ' and 'Post-mortem' TEM study of the super-elastic effect in Cu-Al-Ni shape memory alloys

    International Nuclear Information System (INIS)

    Ibarra, A.; San Juan, J.; Bocanegra, E.H.; Caillard, D.; No, M.L.

    2006-01-01

    An analysis of the microstructure evolution during super-elastic cycling has been performed by transmission electron microscopy (TEM) in order to understand the physical mechanism responsible for the thermo-mechanical properties evolution, as well as the martensitic transformation ageing. Particularly, in this work we have studied the super-elastic effect in Cu-Al-Ni shape memory alloys by 'in situ' TEM experiments. The bright field images and diffraction patterns have allowed us to determine, during the transformation, the kind of nucleated martensite variants and their relative orientations. Finally, we have analysed the super-elastic effect on the dislocation microstructure and on the transformation temperatures

  1. Quantitative TEM study of the precipitation microstructure in aluminium alloy Al(MgSiCu) 6056 T6

    International Nuclear Information System (INIS)

    Delmas, F.; Casanove, M.J.; Lours, P.; Couret, A.; Coujou, A.

    2004-01-01

    The precipitate microstructure in the last-generation aluminium alloy 6056 T6 [AlMgSiCu] is investigated using three complementary techniques of transmission electron microscopy (TEM) with a special focus on the density and volume fraction of strengthening particles. High-resolution TEM allows the identification of the precipitates and the measurement of the precipitate sizes to be performed. Conventional TEM is used to evaluate the number of precipitates in the investigated area as well as their distribution in the matrix. In situ TEM straining, via the analysis of the dislocation slip traces, permits to determine precisely the thickness and the volume of the foil in the region where the precipitates are analysed. Taking into account the shape and the dimensions of precipitates with respect to the foil thickness, a novel methodology for measuring the volume density and the volume fraction of precipitates is proposed

  2. TEM and EELS study of deuterated carbon: application to the fuel retention in tokamaks

    International Nuclear Information System (INIS)

    Bernier, N.

    2007-12-01

    We developed a methodology, based on the combination of TEM and EELS techniques, for a structural and chemical characterization, at a high spatial resolution, of a wide range of carbon materials. We i) optimized, in the framework of theoretical models, the sp2 fraction quantification from pure carbons by EELS ii) transferred this quantification to deuterated amorphous carbon layers iii) showed, from graphitized carbons, how the TEM-EELS combination allows to detect low concentrations of implanted D. Due to the accomplishment of these developments, we applied our approach to the study of D retention in composites C/C, which are the plasma-facing materials in TS. We showed that specific localized retention sites correspond to relatively large (∼ 3 mm.) cracks between fibres and matrix; such cracks offer a simple and direct path for deuterated amorphous carbon. The particle balance performed in TS is discussed in the light of this trapping mechanism. (author)

  3. The mandibular ridge oral mucosa model of stromal influences on the endothelial tip cells: an immunohistochemical and TEM study.

    Science.gov (United States)

    Rusu, Mugurel Constantin; Didilescu, Andreea Cristiana; Stănescu, Ruxandra; Pop, Florinel; Mănoiu, Valentina Mariana; Jianu, Adelina Maria; Vâlcu, Marek

    2013-02-01

    This study aimed to evaluate by immunohistochemistry and transmission electron microscopy (TEM) the morphological features of the oral mucosa endothelial tip cells (ETCs) and to determine the immune and ultrastructural patterns of the stromal nonimmune cells which could influence healing processes. Immune labeling was performed on bioptic samples obtained from six edentulous patients undergoing surgery for dental implants placement; three normal samples were collected from patients prior to the extraction of the third mandibular molar. The antibodies were tested for CD34, CD117(c-kit), platelet derived growth factor receptor-alpha (PDGFR-α), Mast Cell Tryptase, CD44, vimentin, CD45, CD105, alpha-smooth muscle actin, FGF2, Ki67. In light microscopy, while stromal cells (StrCs) of the reparatory and normal oral mucosa, with a fibroblastic appearance, were found positive for a CD34/CD44/CD45/CD105/PDGFR-α/vimentin immune phenotype, the CD117/c-kit labeling led to a positive stromal reaction only in the reparatory mucosa. In TEM, non-immune StrCs presenting particular ultrastructural features were identified as circulating fibrocytes (CFCs). Within the lamina propria CFCs were in close contact with ETCs. Long processes of the ETCs were moniliform, and hook-like collaterals were arising from the dilated segments, suggestive for a different stage migration. Maintenance and healing of oral mucosa are so supported by extensive processes of angiogenesis, guided by ETCs that, in turn, are influenced by the CFCs that populate the stromal compartment both in normal and reparatory states. Therefore, CFCs could be targeted by specific therapies, with pro- or anti-angiogenic purposes. Copyright © 2012 Wiley Periodicals, Inc.

  4. Tem study of thermal ageing of ferrite in cast duplex stainless steel

    International Nuclear Information System (INIS)

    Nenonen, P.; Massoud, J.P.; Timofeev, B.T.

    2002-01-01

    The changes in the microstructure and composition of ferrite in two types of cast duplex stainless steels and in an austenitic-ferritic weld metal after long term thermal ageing has been studied using analytical transmission electron microscope (FEGTEM). A cast test steel containing Mo was investigated first as a reference material in three different conditions: as solution annealed, aged at 300 C and aged at 400 C. This investigation was carried out to gain experience of how EDS (X-ray analyser) analyser and TEM (transmission electron microscope) can be used to study elemental inhomogeneity, which is usually investigated with an atom probe (APFIM). The two other materials, an austenitic-ferritic weld metal and a cast duplex Ti-stabilised stainless steel used for long time at NPP operation temperature were investigated using the experience obtained with the test steel. The results showed that analytical TEM can be used to investigate elemental inhomogeneity of ferrite, but there are several important things to be taken into account when the spectra for this purpose are collected. These things are, such as the thickness of the specimen, probe size, contamination rate, 'elemental background' of the spectrum and possible enrichment of certain alloying elements in the surface oxide layer of the TEM-specimens. If minor elements are also analysed, it may increase the scattering of the results. (authors)

  5. Bayesian resolution of TEM, CSEM and MT soundings: a comparative study

    Science.gov (United States)

    Blatter, D. B.; Ray, A.; Key, K.

    2017-12-01

    We examine the resolution of three electromagnetic exploration methods commonly used to map the electrical conductivity of the shallow crust - the magnetotelluric (MT) method, the controlled-source electromagnetic (CSEM) method and the transient electromagnetic (TEM) method. TEM and CSEM utilize an artificial source of EM energy, while MT makes use of natural variations in the Earth's electromagnetic field. For a given geological setting and acquisition parameters, each of these methods will have a different resolution due to differences in the source field polarization and the frequency range of the measurements. For example, the MT and TEM methods primarily rely on induced horizontal currents and are most sensitive to conductive layers while the CSEM method generates vertical loops of current and is more sensitive to resistive features. Our study seeks to provide a robust resolution comparison that can help inform exploration geophysicists about which technique is best suited for a particular target. While it is possible to understand and describe a difference in resolution qualitatively, it remains challenging to fully describe it quantitatively using optimization based approaches. Part of the difficulty here stems from the standard electromagnetic inversion toolkit, which makes heavy use of regularization (often in the form of smoothing) to constrain the non-uniqueness inherent in the inverse problem. This regularization makes it difficult to accurately estimate the uncertainty in estimated model parameters - and therefore obscures their true resolution. To overcome this difficulty, we compare the resolution of CSEM, airborne TEM, and MT data quantitatively using a Bayesian trans-dimensional Markov chain Monte Carlo (McMC) inversion scheme. Noisy synthetic data for this study are computed from various representative 1D test models: a conductive anomaly under a conductive/resistive overburden; and a resistive anomaly under a conductive/resistive overburden. In

  6. Microscopy

    Science.gov (United States)

    Patricia A. Moss; Les Groom

    2001-01-01

    Microscopy is the study and interpretation of images produced by a microscope. "Interpretation" is the keyword, because the microscope enables one to see structures that are too small or too close together to be resolved by the unaided eye. (The human eye cannot separate two points or lines that are closer together than 0.1 mm.) it is important to...

  7. TOPICAL REVIEW: Present status and future prospects of spherical aberration corrected TEM/STEM for study of nanomaterials

    Directory of Open Access Journals (Sweden)

    Nobuo Tanaka

    2008-01-01

    Full Text Available The present status of Cs-corrected TEM/STEM is described from the viewpoint of the observation of nanomaterials. Characteristic features in TEM and STEM are explained using the experimental data obtained by our group and other research groups. Cs correction up to the 3rd-order aberration of an objective lens has already been established and research interest is focused on correcting the 5th-order spherical aberration and the chromatic aberration in combination with the development of a monochromator below an electron gun for smaller point-to-point resolution in optics. Another fundamental area of interest is the limitation of TEM and STEM resolution from the viewpoint of the scattering of electrons in crystals. The minimum size of the exit-wave function below samples undergoing TEM imaging is determined from the calculation of scattering around related atomic columns in the crystals. STEM does not have this limitation because the resolution is, in principle, determined by the probe size. One of the future prospects of Cs-corrected TEM/STEM is the possibility of extending the space around the sample holder by correcting the chromatic and spherical aberrations. This wider space will contribute to the ease of performing in situ experiments and various combinations of TEM and other analysis methods. High-resolution, in situ dynamic and 3D observations/analysis are the most important keywords in the next decade of high-resolution electron microscopy.

  8. TEM Nanostructural Study of Al-6Si-3Cu-Mg Melt-Spun Ribbons

    Directory of Open Access Journals (Sweden)

    Ismeli Alfonso López

    2008-01-01

    Full Text Available Three quaternary Al-6Si-3Cu-xMg (x = 0.59, 3.80, and 6.78 wt.% alloys were produced by melt-spun and characterized using X-ray diffractometry (XRD, transmission electron microscopy (TEM, and microhardness techniques. Obtained second phases were Al2Cu( for the alloy with 0.59% Mg and Al5Cu2Mg8Si6 (Q for the alloys with 3.80 and 6.78% Mg. These phases are present as 30–50 nm or as 5–10 nm nanoparticles. Alloying elements content in solid solution increased, mainly for Si and Mg. The high alloying elements content in solid solution and the small -Al cell size for melt-spun alloys leads to microhardness values about 2 times higher than those of ingot counterparts. The microhardness increase for melt-spun alloys with 3.80 and 6.78% Mg depends on Mg content in solid solution.

  9. Sintering of oxide-supported Pt and Pd nanoparticles in air studied by in situ TEM

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose

    This thesis presents a fundamental study of the sintering of supported nanoparticles in relation to diesel oxidation catalysts. The sintering of supported nanoparticles is an important challenge in relation to this catalyst, as well as many other catalyst systems, and a fundamental understanding...... of Pt, Pd and bimetallic Pt-Pd nanoparticles supported on a flat and homogeneous Al2O3 or SiO2 surface. By using in situ TEM on the planar model catalysts it was possible to directly monitor the detailed dynamical changes of the individual nanoparticles during exposure to oxidizing conditions...

  10. TEM and EELS studies of microwave-irradiation synthesis of bimetallic platinum nanocatalysts

    International Nuclear Information System (INIS)

    Mathe, N R; Scriba, M R; Coville, N J; Olivier, J E

    2014-01-01

    Microwave-irradiation (MW) synthesis of nanostructured materials provides for the synthesis of metal nanoparticles, using fast and uniform heating rates. This procedure affords better control of the shape and size of the nanoparticles when compared to conventional methods. In this work, microwave-irradiation was used to produce platinum-cobalt (Pt-Co) and platinum-nickel (Pt-Ni) nanoparticles for use as electrocatalysts in the methanol oxidation reaction. High resolution TEM imaging and EELS studies revealed that these bimetallic nanoparticles form islands or hetero-structures

  11. In-situ TEM studies of microstructure evolution under ion irradiation for nuclear engineering applications

    International Nuclear Information System (INIS)

    Kaoumi, D.

    2011-01-01

    One of the difficulties of studying processes occurring under irradiation (in a reactor environment) is the lack of kinetics information since usually samples are examined ex situ (i.e. after irradiation) so that only snapshots of the process are available. Given the dynamic nature of the phenomena, direct in situ observation is invaluable for better understanding the mechanisms, kinetics and driving forces of the processes involved. This can be done using in situ ion irradiation in a TEM at the IVEM facility at Argonne National Laboratory which, in the USA, is a unique facility. To predict the in reactor behavior of alloys, it is essential to understand the basic mechanisms of radiation damage formation (loop density, defect interactions) and accumulation (loop evolution, precipitation or dissolution of second phases etc.). In-situ Ion-irradiation in a TEM has proven a very good tool for that purpose as it allows for the direct determination of the formation and evolution of irradiation-induced damage and the spatial correlation of the defect structures with the pre-existing microstructure (including lath boundaries, network dislocations and carbides) as a function of dose, dose rate, temperature and ion type. Using this technique, different aspects of microstructure evolution under irradiation were studied, such as defect cluster formation and evolution as a function of dose in advanced Ferritic/Martensitic (F/M) steels, the irradiation stability of precipitates in Oxide Dispersion Strengthened (ODS) steels, and irradiation-induced grain-growth. Such studies will be reported in this presentation

  12. Graphene oxide and reduced graphene oxide studied by the XRD, TEM and electron spectroscopy methods

    International Nuclear Information System (INIS)

    Stobinski, L.; Lesiak, B.; Malolepszy, A.; Mazurkiewicz, M.; Mierzwa, B.; Zemek, J.; Jiricek, P.; Bieloshapka, I.

    2014-01-01

    Highlights: • Graphene oxide (FL-GOc) and reduced graphene oxide (FL-RGOc): XRD, TEM, XPS, REELS. • FL-GOc: stacking nanostructure—22 × 6 nm (DxH), 0.9 nm layers separation (XRD). • FL-RGOc: stacking nanostructure—8 × 1 nm (DxH), 0.4 nm layers separation (XRD). • Reduction: oxygen group degradation, decreasing distance between graphene layers. • Number of graphene layers in stacking nanostructure: 6–7 (FL-GOc), 2–3 (FL-RGOc). - Abstract: The commercial and synthesised few-layer graphene oxide, prepared using oxidation reactions, and few-layer reduced graphene oxide samples were structurally and chemically investigated by the X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron spectroscopy methods, i.e. X-ray photoelectron spectroscopy (XPS) and reflection electron energy loss spectroscopy (REELS). The commercial graphene oxide (FL-GOc) shows a stacking nanostructure of about 22 × 6 nm average diameter by height with the distance of 0.9 nm between 6-7 graphene layers, whereas the respective reduced graphene oxide (FL-RGOc)—about 8 × 1 nm average diameter by height stacking nanostructure with the distance of 0.4 nm between 2-3 graphene layers (XRD). The REELS results are consistent with those by the XRD indicating 8 (FL-GOc) and 4 layers (FL-RGOc). In graphene oxide and reduced graphene oxide prepared from the graphite the REELS indicates 8–11 and 7–10 layers. All graphene oxide samples show the C/O ratio of 2.1–2.3, 26.5–32.1 at% of C sp 3 bonds and high content of functional oxygen groups (hydroxyl—C-OH, epoxy—C-O-C, carbonyl—C=O, carboxyl—C-OOH, water) (XPS). Reduction increases the C/O ratio to 2.8–10.3, decreases C sp 3 content to 11.4–20.3 at% and also the content of C-O-C and C=O groups, accompanied by increasing content of C-OH and C-OOH groups. Formation of additional amount of water due to functional oxygen group reduction leads to layer delamination. Removing of functional oxygen groups

  13. Is the TEM obsolescent?

    International Nuclear Information System (INIS)

    Williams, D.B.

    2002-01-01

    significantly faster and has become more indispensable than the TEM to the future of materials research in many areas. For instance, the ability of modern SEMs to characterize the crystallographic make-up of complex materials via electron backscatter pattern diffraction analysis should have been available via kikuchi pattern and CBED analysis on a computerized TEM many years ago. In the author's opinion, unless significant moves are made to redesign the TEM to become significantly more flexible, more easily operated and much cheaper, other instruments will take over the TEM market and there will be no need for mammoth tomes of several hundred pages instructing students on the intricacies of operation of this once-proud instrument. Copyright (2002) Australian Society for Electron Microscopy Inc

  14. In-Situ TEM Study of a Nanoporous Ni–Co Catalyst Used for the Dry Reforming of Methane

    Directory of Open Access Journals (Sweden)

    Takeshi Fujita

    2017-10-01

    Full Text Available We performed in-situ transmission electron microscopy (TEM on a dealloyed nanoporous NiCo catalyst used for the dry reforming of methane (DRM to investigate the origin of the catalytic activity and structural durability. The in-situ observations and local chemical analysis indicated that the DRM induced chemical demixing of Ni and Co accompanied by grain refinement, implying possible “synergic effects” in a general bimetallic NiCo catalyst when used for the DRM.

  15. The potentials and challenges of electron microscopy in the study of atomic chains

    Science.gov (United States)

    Banhart, Florian; Torre, Alessandro La; Romdhane, Ferdaous Ben; Cretu, Ovidiu

    2017-04-01

    The article is a brief review on the potential of transmission electron microscopy (TEM) in the investigation of atom chains which are the paradigm of a strictly one-dimensional material. After the progress of TEM in the study of new two-dimensional materials, microscopy of free-standing one-dimensional structures is a new challenge with its inherent potentials and difficulties. In-situ experiments in the TEM allowed, for the first time, to generate isolated atomic chains consisting of metals, carbon or boron nitride. Besides having delivered a solid proof for the existence of atomic chains, in-situ TEM studies also enabled us to measure the electrical properties of these fundamental linear structures. While ballistic quantum conductivity is observed in chains of metal atoms, electrical transport in chains of sp1-hybridized carbon is limited by resonant states and reflections at the contacts. Although substantial progress has been made in recent TEM studies of atom chains, fundamental questions have to be answered, concerning the structural stability of the chains, bonding states at the contacts, and the suitability for applications in nanotechnology. Contribution to the topical issue "The 16th European Microscopy Congress (EMC 2016)", edited by Richard Brydson and Pascale Bayle-Guillemaud

  16. TEM study of damage recovery in SiC by swift Xe ion irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Skuratov, V.A., E-mail: skuratov@jinr.ru [Joint Institute for Nuclear Research, Dubna (Russian Federation); O’Connell, J. [Centre for HRTEM, Nelson Mandela Metropolitan University, Port Elizabeth (South Africa); Sohatsky, A.S. [Joint Institute for Nuclear Research, Dubna (Russian Federation); Neethling, J. [Centre for HRTEM, Nelson Mandela Metropolitan University, Port Elizabeth (South Africa)

    2014-05-01

    The microstructure of 4H–SiC samples subsequently irradiated with low energy He (10 keV), Ti (220 keV) and high energy (167 MeV) Xe ions has been studied using cross-sectional transmission electron microscopy. It was found that xenon ions with fluences above 10{sup 13} cm{sup −2} restore crystallinity in a heavily damaged partially amorphous zone. No, or negligible damage recovery is observed in fully amorphized layers of silicon carbide.

  17. TEM study of damage recovery in SiC by swift Xe ion irradiation

    International Nuclear Information System (INIS)

    Skuratov, V.A.; O’Connell, J.; Sohatsky, A.S.; Neethling, J.

    2014-01-01

    The microstructure of 4H–SiC samples subsequently irradiated with low energy He (10 keV), Ti (220 keV) and high energy (167 MeV) Xe ions has been studied using cross-sectional transmission electron microscopy. It was found that xenon ions with fluences above 10 13 cm −2 restore crystallinity in a heavily damaged partially amorphous zone. No, or negligible damage recovery is observed in fully amorphized layers of silicon carbide

  18. TEM of nanostructured metals and alloys

    International Nuclear Information System (INIS)

    Karnthaler, H.P.; Waitz, T.; Rentenberger, C.; Mingler, B.

    2004-01-01

    Nanostructuring has been used to improve the mechanical properties of bulk metals and alloys. Transmission electron microscopy (TEM) including atomic resolution is therefore appropriate to study these nanostructures; four examples are given as follows. (1) The early stages of precipitation at RT were investigated in an Al-Mg-Si alloy. By high resolution TEM it is shown that the precipitates lie on (0 0 1) planes having an ordered structure. (2) In Co alloys the fronts of martensitic phase transformations were analysed showing that the transformation strains are very small thus causing no surface relief. (3) Re-ordering and recrystallization were studied by in situ TEM of an Ni 3 Al alloy being nanocrystalline after severe plastic deformation. (4) In NiTi severe plastic deformation is leading to the formation of amorphous shear bands. From the TEM analysis it is concluded that the amorphization is caused by plastic shear instability starting in the shear bands

  19. Electron microscopy studies of materials used for hydrogen storage

    Energy Technology Data Exchange (ETDEWEB)

    Andrei, Carmen M.

    2004-07-01

    Concerns over global warming and air pollution have stimulated the concept of the ''Hydrogen Economy'' and the potential extensive use of hydrogen as an energy carrier. Hydrogen storage in a solid matrix has become one of the promising solutions for vehicular applications. In this study, several transmission electron microscopy (TEM) techniques such as high resolution (HR), electron diffraction, energy dispersive X-ray spectroscopy (EDS), electron energy loss spectroscopy (EELS) and energy-filtered transmission electron microscopy (EFT EM) as well as scanning electron microscopy (SEM) have been used to study the microstructure of materials related to hydrogen storage applications. Some of the results are compared with powder X-ray diffraction (PXD) data. A TbNiAl compound processed by the hydrogenation-disproportionation-desorption-recombination (HDDR) route has been studied using a combination of SEM, TEM and PXD. Information about the variations in the composition and surface topography in both disproportionation and recombination stages is given by the SEM backscattered electrons and secondary electrons images. The crystallites that have undergone the recombination process were found smaller in size. The sodium alanate, NaAIH4 is one of the most promising candidate materials for hydrogen storage. Ti additives are effective at reducing the reaction temperatures and improving the efficiency of the kinetics. The microstructure of NaAlH4 with TiF3 additive has been examined after the initial ball milling and after 15 cycles, using TEM, SEM and EDS. The effect of the additive on particle morphology, grain size and distribution of the phases has been studied. The additive has uneven distribution in the sample after initial ball milling. After 15 cycles, EDS maps show some combination of Ti with the alanate phase. No significant change in grain size of the Na/Al rich particles between the ball milled and 15 cycled sample was observed. The LiAlD4

  20. Microparticle adhesion studies by atomic force microscopy

    NARCIS (Netherlands)

    Segeren, L.H.G.J.; Siebum, B.; Karssenberg, F.G.; Berg, van den J.W.A.; Vancso, G.J.

    2002-01-01

    Atomic force microscopy (AFM) is one of the most flexible and simple techniques for probing surface interactions. This article reviews AFM studies on particle adhesion. Special attention is paid to the characterization of roughness and its effect on adhesion. This is of importance when comparing the

  1. SAXS and TEM Investigation of Bentonite Structure

    International Nuclear Information System (INIS)

    Matusewicz, Michal; Liljestroem, Ville; Muurinen, Arto; Serimaa, Ritva

    2013-01-01

    A preliminary investigation of bentonite structure using Small-Angle X-ray Scattering (SAXS) and Transmission Electron Microscopy (TEM) is presented. Three types of clay were used: unchanged MX-80 bentonite and purified clays with sodium or calcium ions. Quantitative information in nano-scale - basal spacing, mean crystallite size - was obtained from SAXS, which was complemented by TEM to give qualitative information from micron to nanometre scale. SAXS seems to be a more reliable source of quantitative data than TEM. SAXS gives the averaged information about basal spacing. TEM in this study gives more qualitative information, but in a greater resolution range. The presented work is a starting point to combine more methods to obtain a better idea of bentonite structure. (authors)

  2. Inter- and intragranular plasticity mechanisms in ultrafine-grained Al thin films: An in situ TEM study

    International Nuclear Information System (INIS)

    Mompiou, F.; Legros, M.; Boé, A.; Coulombier, M.; Raskin, J.-P.; Pardoen, T.

    2013-01-01

    The nature of the elementary deformation mechanisms in small-grained metals has been the subject of numerous recent studies. In the submicron range, mechanisms other than intragranular dislocation mechanisms, such as grain boundary (GB)-based mechanisms, are active and can explain the deviations from the Hall–Petch law. Here, we report observations performed during in situ transmission electron microscopy (TEM) tensile tests on initially dislocation-free Al thin films with a mean grain size around 250 nm prepared by microfabrication techniques. Intergranular plasticity is activated at the onset of plasticity. It consists of the motion of dislocations in the GB plane irrespective of the GB character. Surface imperfections, such as GB grooves, are supposed to trigger intergranular plasticity. At larger deformations, the motion of the intergranular dislocations leads to GB sliding and eventually cavitation. In the meantime, GB stress-assisted migration and dislocation emission inside the grain from GB sources have also been observed. The observation of these different mechanisms during the deformation provides an important insight into the understanding of the mechanical properties of metallic thin films.

  3. Microstructural studies of 35 degrees C copper Ni-Ti orthodontic wire and TEM confirmation of low-temperature martensite transformation.

    Science.gov (United States)

    Brantley, William A; Guo, Wenhua; Clark, William A T; Iijima, Masahiro

    2008-02-01

    Previous temperature-modulated differential scanning calorimetry (TMDSC) study of nickel-titanium orthodontic wires revealed a large exothermic low-temperature peak that was attributed to transformation within martensitic NiTi. The purpose of this study was to use transmission electron microscopy (TEM) to verify this phase transformation in a clinically popular nickel-titanium wire, identify its mechanism and confirm other phase transformations found by TMDSC, and to provide detailed information about the microstructure of this wire. The 35 degrees C Copper nickel-titanium wire (Ormco) with cross-section dimensions of 0.016 in. x 0.022 in. used in the earlier TMDSC investigation was selected. Foils were prepared for TEM analyses by mechanical grinding, polishing, dimpling, ion milling and plasma cleaning. Standard bright-field and dark-field TEM images were obtained, along with convergent-beam electron diffraction patterns. A cryo-stage with the electron microscope (Phillips CM 200) permitted the specimen to be observed at -187, -45, and 50 degrees C, as well as at room temperature. Microstructures were also observed with an optical microscope and a scanning electron microscope. Room temperature microstructures had randomly oriented, elongated grains that were twinned. Electron diffraction patterns confirmed that phase transformations took place over temperature ranges previously found by TMDSC. TEM observations revealed a high dislocation density and fine-scale oxide particles, and that twinning is the mechanism for the low-temperature transformation in martensitic NiTi. TEM confirmed the low-temperature peak and other phase transformations observed by TMDSC, and revealed that twinning in martensite is the mechanism for the low-temperature peak. The high dislocation density and fine-scale oxide particles in the microstructure are the result of the wire manufacturing process.

  4. How TEM Projection Artifacts Distort Microstructure Measurements: A Case Study in a 9 pct Cr-Mo-V Steel

    Science.gov (United States)

    Monsegue, Niven; Reynolds, William T.; Hawk, Jeffrey A.; Murayama, Mitsuhiro

    2014-08-01

    Morphological data obtained from two-dimensional (2D) and three-dimensional (3D) transmission electron microscopy (TEM) observations were compared to assess the effects of TEM projection errors for submicron-size precipitates. The microstructure consisted of M23C6 carbides in a 9 pct Cr-Mo-V heat resistant steel before and after exposure to creep conditions. Measurements obtained from about 800 carbides demonstrate that particle size and spacing estimates made from 2D observations overestimate the more accurate values obtained from 3D reconstructions. The 3D analysis also revealed the M23C6 precipitates lengthen anisotropically along lath boundary planes, suggesting that coarsening during the early stage of creep in this alloy system is governed by grain boundary diffusion.

  5. Cryogenic transmission electron microscopy nanostructural study of shed microparticles.

    Directory of Open Access Journals (Sweden)

    Liron Issman

    Full Text Available Microparticles (MPs are sub-micron membrane vesicles (100-1000 nm shed from normal and pathologic cells due to stimulation or apoptosis. MPs can be found in the peripheral blood circulation of healthy individuals, whereas elevated concentrations are found in pregnancy and in a variety of diseases. Also, MPs participate in physiological processes, e.g., coagulation, inflammation, and angiogenesis. Since their clinical properties are important, we have developed a new methodology based on nano-imaging that provides significant new data on MPs nanostructure, their composition and function. We are among the first to characterize by direct-imaging cryogenic transmitting electron microscopy (cryo-TEM the near-to-native nanostructure of MP systems isolated from different cell types and stimulation procedures. We found that there are no major differences between the MP systems we have studied, as most particles were spherical, with diameters from 200 to 400 nm. However, each MP population is very heterogeneous, showing diverse morphologies. We investigated by cryo-TEM the effects of standard techniques used to isolate and store MPs, and found that either high-g centrifugation of MPs for isolation purposes, or slow freezing to -80 °C for storage introduce morphological artifacts, which can influence MP nanostructure, and thus affect the efficiency of these particles as future diagnostic tools.

  6. Comparative TEM study of bonded silicon/silicon interfaces fabricated by hydrophilic, hydrophobic and UHV wafer bonding

    International Nuclear Information System (INIS)

    Reznicek, A.; Scholz, R.; Senz, S.; Goesele, U.

    2003-01-01

    Wafers of Czochralski-grown silicon were bonded hydrophilically, hydrophobically and in ultrahigh vacuum (UHV) at room temperature. Wafers bonded hydrophilically adhere together by hydrogen bonds, those bonded hydrophobically by van der Waals forces and UHV-bonded ones by covalent bonds. Annealing the pre-bonded hydrophilic and hydrophobic wafer pairs in argon for 2 h at different temperatures increases the initially low bonding energy. UHV-bonded wafer pairs were also annealed to compare the results. Transmission electron microscopy (TEM) investigations show nano-voids at the interface. The void density depends on the initial bonding strength. During annealing the shape, coverage and density of the voids change significantly

  7. TEM study of soot, organic aerosol, and sea-salt particles collected during CalNex

    Science.gov (United States)

    Adachi, K.; Buseck, P. R.

    2010-12-01

    Anthropogenic aerosol particles are emitted in abundance from megacities. Those particles can have important effects on both human health and climate. In this study, aerosol particles having aerodynamic diameters between 50 and 300 nm were collected during the CalNex campaign at the Pasadena ground site from May 15 to June 15, 2010, ~15 km northeast of downtown Los Angeles. The samples were analyzed using transmission electron microscopes (TEMs) to characterize particle shapes and compositions. Most samples are dominated by soot, organic aerosol (OA), sulfate, sea salt, or combinations thereof. Sizes and amounts of OA particles increased during the afternoons, and most soot particles were internally mixed with OA and sulfate in the afternoons. The proportion of soot to other material in individual particles increased and soot particles were more compact during the nights and early mornings. Sea-salt particles were commonly internally mixed with other materials. They have high Na contents with lesser N, Mg, S, K, and Ca and almost no Cl, suggesting that the Cl was replaced by sulfate or nitrate in the atmosphere. There is less OA and more sea salt and sulfate in the CalNex samples than in the samples from Mexico City that were collected during the MILAGRO campaign. Our study indicates that compositions of internally mixed aerosol particles and shapes of soot particles change significantly within a day. These changes probably influence the estimates of their effects on human health and climate.

  8. Moessbauer and TEM study of martensitic transformations in ion implanted 17/7 stainless steel

    International Nuclear Information System (INIS)

    Johnson, E.; Johansen, A.; Sarholt-Kristensen, L.; Graabaek, L.

    1986-01-01

    It has earlier been shown that implantation of antimony into austenitic stainless steels induces martensitic phase transformations γ (fcc)→α (bcc). In the present work we have investigated which mechanisms are responsible for the transformation. Samples of 17/7 steels were implanted with noble gases (Kr, Ar) or the stainless steel constituent elements (Fe, Ni, Cr). The energies were selected to give ranges ∝40 nm. The phases present after implantation and the microstructures of the implanted samples were studied by CEMS and TEM respectively. A martensitic (α) phase was found to form after implantation both with Ni, Fe and Cr, in spite of the fact that these elements have opposite tendencies for stabilization of the austenite (γ) phase. The efficiency of martensite formation is therefore mainly related to stress relief associated with secondary radiation damage. This was substantiated from the noble gas implantations, where the highest degree of transformation was observed for fluences where bubble formation occurs. The CEMS analyses show that the transformation efficiency in such cases is nearly 100%. The hyperfine parameters of the implantation induced α phase are similar to those from conventionally induced martensites. (orig.)

  9. Changes in background aerosol composition in Finland during polluted and clean periods studied by TEM/EDX individual particle analysis

    Directory of Open Access Journals (Sweden)

    J. V. Niemi

    2006-01-01

    Full Text Available Aerosol samples were collected at a rural background site in southern Finland in May 2004 during pollution episode (PM1~16 µg m−3, backward air mass trajectories from south-east, intermediate period (PM1~5 µg m−3, backtrajectories from north-east and clean period (PM1~2 µg m−3, backtrajectories from north-west/north. The elemental composition, morphology and mixing state of individual aerosol particles in three size fractions were studied using transmission electron microscopy (TEM coupled with energy dispersive X-ray (EDX microanalyses. The TEM/EDX results were complemented with the size-segregated bulk chemical measurements of selected ions and organic and elemental carbon. Many of the particles in PM0.2–1 and PM1–3.3 size fractions were strongly internally mixed with S, C and/or N. The major particle types in PM0.2–1 samples were 1 soot and 2 (ammoniumsulphates and their mixtures with variable amounts of C, K, soot and/or other inclusions. Number proportions of those two particle groups in PM0.2–1 samples were 0–12% and 83–97%, respectively. During the pollution episode, the proportion of Ca-rich particles was very high (26–48% in the PM1–3.3 and PM3.3–11 samples, while the PM0.2–1 and PM1–3.3 samples contained elevated proportions of silicates (22–33%, metal oxides/hydroxides (1–9% and tar balls (1–4%. These aerosols originated mainly from polluted areas of Eastern Europe, and some open biomass burning smoke was also brought by long-range transport. During the clean period, when air masses arrived from the Arctic Ocean, PM1–3.3 samples contained mainly sea salt particles (67–89% with a variable rate of Cl substitution (mainly by NO3−. During the intermediate period, the PM1–3.3 sample contained porous (sponge-like Na-rich particles (35% with abundant S, K and O. They might originate from the burning of wood pulp wastes of paper industry. The proportion of biological particles and C-rich fragments

  10. Chemical and structural analysis of the bone-implant interface by TOF-SIMS, SEM, FIB and TEM: Experimental study in animal

    International Nuclear Information System (INIS)

    Palmquist, Anders; Emanuelsson, Lena; Sjövall, Peter

    2012-01-01

    Although bone-anchored implants are widely used in reconstructive medicine, the mechanism of osseointegration is still not fully understood. Novel analytical tools are needed to further understand this process, where both the chemical and structural aspects of the bone-implant interface are important. The aim of this study was to evaluate the advantages of combining time-of-flight secondary ion mass spectroscopy (TOF-SIMS) with optical (LM), scanning (SEM) and transmission electron microscopy (TEM) techniques for studying the bone-implant interface of bone-anchored implants. Laser-modified titanium implants with surrounded bone retrieved after 8 weeks healing in rabbit were dehydrated and resin embedded. Three types of sample preparation were studied to evaluate the information gained by combining TOF-SIMS, SEM, FIB and TEM. The results show that imaging TOF-SIMS can provide detailed chemical information, which in combination with structural information from microscopy methods provide a more complete characterization of anatomical structures at the bone-implant interface. By investigating various sample preparation techniques, it is shown that grinded cross section samples can be used for chemical imaging using TOF-SIMS, if careful consideration of potential preparation artifacts is taken into account. TOF-SIMS analysis of FIB-prepared bone/implant cross section samples show distinct areas corresponding to bone tissue and implant with a sharp interface, although without chemical information about the organic components.

  11. Extensive FE-SEM/EDS, HR-TEM/EDS and ToF-SIMS studies of micron- to nano-particles in anthracite fly ash

    Energy Technology Data Exchange (ETDEWEB)

    Ribeiro, Joana [Centro de Geologia, Universidade do Porto, Rua do Campo Alegre, 687, 4169-007 Porto (Portugal); DaBoit, Kátia [Institute of Environmental Research and Human Development, IPADHC, Capivari de Baixo, Santa Catarina (Brazil); Flores, Deolinda [Centro de Geologia, Universidade do Porto, Rua do Campo Alegre, 687, 4169-007 Porto (Portugal); Departamento de Geociências, Ambiente e Ordenamento do Território, Faculdade de Ciências, Universidade do Porto, Rua do Campo Alegre, 687, 4169-007 Porto (Portugal); Kronbauer, Marcio A. [Laboratory of Environmental Researches and Nanotechnology Development, Centro Universitário La Salle, Victor Barreto, 2288 Centro 92010-000, Canoas, RS (Brazil); Silva, Luis F.O., E-mail: felipeqma@hotmail.com [Laboratory of Environmental Researches and Nanotechnology Development, Centro Universitário La Salle, Victor Barreto, 2288 Centro 92010-000, Canoas, RS (Brazil); Environmental Science and Nanotechnology Department, Catarinense Institute of Environmental Research and Human Development, IPADHC, Capivari de Baixo, Santa Catarina (Brazil)

    2013-05-01

    The generation of anthropogenic carbonaceous matter and mixed crystalline/amorphous mineral ultrafine/nano-particles in the 1 to 100 nm size range by worldwide coal power plants represents serious environmental problems due to their potential hazards. Coal fly ash (CFA) that resulted from anthracite combustion in a Portuguese thermal power plant was studied in this work. The physico-chemical characterization of ultrafine/nano-particles present in the CFA samples and their interaction with environment are the aim of this study. The methodologies applied for this work were field emission scanning electron microscopy (FE-SEM) with energy dispersive X-ray spectroscopy (EDS), high-resolution transmission electron microscopy with energy dispersive X-ray spectroscopy (HR-TEM/EDS) and time of flight secondary ion mass spectrometry (ToF-SIMS). Some hazardous volatile elements, C, N, S and Hg contents were also determined in the studied samples. Generally, the CFA samples comprise carbonaceous, glassy and metallic solid spheres with some containing mixed amorphous/crystalline phases. The EDS analysis coupled with the FE-SEM and HR-TEM observations of the fly ash particles with 100 to 0.1 nm demonstrates that these materials contain a small but significant proportion of encapsulated HVEs. In addition, the presence of abundant multi-walled carbon nanotubes (MWCNTs) and amorphous carbon particles, both containing hazardous volatile elements (HVEs), was also evidenced by the FE-SEM/EDS and HR-TEM/EDS analysis. A wide range of organic and inorganic compounds was determined by chemical maps obtained in ToF-SIMS analysis. - Highlights: ► We examine changes in the level of ultrafine and nanoparticles of coal mining. ► Increasing geochemical information will increase human health information in this area. ► Electron bean and Tof-SIMS increase area information.

  12. MICROORGANISMS FOUND IN SECONDARY CATARACT MATERIAL OF ECCE PATIENTS, A STUDY WITH SEM AND TEM

    NARCIS (Netherlands)

    KALICHARAN, D; JONGEBLOED, WL; LOS, LI; WORST, JGF

    1993-01-01

    Globular secondary cataract material, removed from 24 patients with ECCE after ophthalmic cleaning of the anterior capsule, were investigated with SEM and TEM. Besides spherical, somewhat oval shaped bodies of various shape and size comparable with those found in cataractous lenses, (an)aerobic

  13. Substrate-HTcS thin film interaction studies by (S)TEM

    NARCIS (Netherlands)

    Ramaekers, P.P.J.; Klepper, D.; Kitazawa, K.; Ishiguro, T.

    1989-01-01

    This paper concerns with compatibility aspects beween HTcS thin film either their substrates. The influence of substrate-thin film interaction and thin film microstructure on the superconducting properties is discussed. In this respect, data based on (S)TEM observations are presented. It is

  14. In-situ TEM study of domain switching in GaN thin films

    Science.gov (United States)

    Wang, Baoming; Wang, Tun; Haque, Aman; Snure, Michael; Heller, Eric; Glavin, Nicholas

    2017-09-01

    Microstructural response of gallium nitride (GaN) films, grown by metal-organic chemical vapor deposition, was studied as a function of applied electrical field. In-situ transmission electron microscopy showed sudden change in the electron diffraction pattern reflecting domain switching at around 20 V bias, applied perpendicular to the polarization direction. No such switching was observed for thicker films or for the field applied along the polarization direction. This anomalous behavior is explained by the nanoscale size effects on the piezoelectric coefficients of GaN, which can be 2-3 times larger than the bulk value. As a result, a large amount of internal energy can be imparted in 100 nm thick films to induce domain switching at relatively lower voltages to induce such events at the bulk scale.

  15. Environmental TEM study of the dynamic nanoscaled morphology of NiO/YSZ during reduction

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose; Agersted, Karsten; Hansen, Karin Vels

    2015-01-01

    The reduction of a metal oxide is often a critical preparation step for activating catalytic behaviour. This study addresses the reduction process of NiO in pure form and in a composite of NiO/yttria-stabilized zirconia (YSZ) in hydrogen relevant for solid oxide electrochemical cells by comparing...... results from environmental transmission electron microscopy (ETEM) with thermogravimetric analysis (TGA). The temperature dependent reduction profiles obtained from TGA confirm an inhibitive effect from YSZ on the NiO reduction. The ETEM images show the growth of Ni in decaying NiO and reveal...... the nanoscale morphological changes such as pore formation in NiO above 280°C and densification and collapse of the pore structures above 400°C. The accelerated Ni front in NiO illustrates the auto catalysis of the reaction. A rapid temperature ramping from room temperature to 780°C in hydrogen in 1 second...

  16. Joint TEM and MT aquifer study in the Atacama Desert, North Chile

    Science.gov (United States)

    Ruthsatz, Alexander D.; Sarmiento Flores, Alvaro; Diaz, Daniel; Reinoso, Pablo Salazar; Herrera, Cristian; Brasse, Heinrich

    2018-06-01

    The Atacama Desert represents one of the driest regions on earth, and despite the absence of sustainable clean water reserves the demand has increased drastically since 1970 as a result of growing population and expanding mining activities. Magnetotelluric (MT) and Transient Electromagnetic (TEM) measurements were carried out for groundwater exploration in late 2015 in the area of the Profeta Basin at the western margin of the Chilean Precordillera. Both methods complement each other: While MT in general attains larger penetration depths, TEM allows better resolution of near surface layers; furthermore TEM is free from galvanic distortion. Data were collected along three profiles, enabling a continuous resistivity image from the surface to at least several hundred meters depth. TEM data were inverted in a 1-D manner, consistently yielding a poorly conductive near-surface layer with a thickness of approximately 30 m and below a well-conducting layer which we interpret as the aquifer with resistivities around 10 Ωm. At marginal sites of the main SW-NE-profile the resistive basement was found in 150 m. These depths are confirmed by interpretation of the MT soundings. Those were firstly inverted with a 2-D approach and then by 3-D inversion as clear indications of three-dimensionality exist. Several modeling runs were performed with different combinations of transfer functions and smoothing parameters. Generally, MT and TEM results agree reasonably well and an overall image of the resistivity structures in the Profeta Basin could be achieved. The aquifer reaches depths of more than 500 m in parts and, by applying Archie's law, resistivities of 1 Ωm can be assumed, indicating highly saline fluids from the source region of the surrounding high Andes under persisting arid conditions.

  17. Swelling induced by alpha decay in monazite and zirconolite ceramics: A XRD and TEM comparative study

    Science.gov (United States)

    Deschanels, X.; Seydoux-Guillaume, A. M.; Magnin, V.; Mesbah, A.; Tribet, M.; Moloney, M. P.; Serruys, Y.; Peuget, S.

    2014-05-01

    Zirconolite and monazite matrices are potential ceramics for the containment of actinides (Np, Cm, Am, Pu) which are produced over the reprocessing of spent nuclear fuel. Actinides decay mainly through the emission of alpha particles, which in turn causes most ceramics to undergo structural and textural changes (amorphization and/or swelling). In order to study the effects of alpha decays on the above mentioned ceramics two parallel approaches were set up. The first involved the use of an external irradiation source, Au, which allowed the deposited recoil energy to be simulated. The second was based on short-lived actinide doping with 238Pu, (i.e. an internal source), via the incorporation of plutonium oxide into both the monazite and zirconolite structures during synthesis. In both types of irradiation experiments, the zirconolite samples became amorphous at room temperature with damage close to 0.3 dpa; corresponding to a critical dose of 4 × 1018 α g-1 (i.e. ∼1.3 × 1021 keV cm-3). Both zirconolite samples also showed the same degree of macroscopic swelling at saturation (∼6%), with ballistic processes being the predominant damaging effect. In the case of the monazite however, the macroscopic swelling and amorphization were dependent on the nature of the irradiation. Externally, (Au), irradiated samples became amorphous while also demonstrating a saturation swelling of up to 8%. In contrast to this, the swelling of the 238Pu doped samples was much smaller at ∼1%. Also, unlike the externally (Au) irradiated monazite these 238Pu doped samples remained crystalline up to 7.5 × 1018 α g-1 (0.8 dpa). XRD, TEM and swelling measurements were used to fully characterize and interpret this behavior. The low swelling and the conservation of the crystalline state of 238Pu doped monazite samples indicates that alpha annealing took place within this material.

  18. Fault detection by Turam TEM survey. Numerical model studies and a case history; TEM ho Turam sokutei haichi ni yoru danso kenshutsu no kokoromi. Model keisan to jisshirei

    Energy Technology Data Exchange (ETDEWEB)

    Wada, K; Tsutsui, T [Mitsui Mineral Development Engineering Co. Ltd., Tokyo (Japan); Ito, T [Chiba Univ., Chiba (Japan). Faculty of Science; Takeuchi, A [Toyama University, Toyama (Japan). Faculty of Science; He, P [Power Reactor and Nuclear fuel Development Corp., Tokyo (Japan)

    1997-05-27

    With an objective to detect faults estimated to exist along the Shigesumi valley in the Kamioka mine, discussions were given by using electromagnetic survey, which uses the Turam measurement arrangement based on the TEM method, and three-dimensional model calculations. The Turam measurement arrangement, which installs transmission loop fixedly, is used to identify nature and distribution of electrically conductive objects upon noticing abnormal portions in magnetic fields in the measurement data. In the model calculation, the plate model calculation method and the FDTD method were used, and so was the calculation code TEM3DL. The result revealed that strong topographical influence is seen from steep V-shaped valley existing along the traverse line in the measurement data, but an abnormal resistivity band accompanying remarkable distortion in the curve was detected. According to the result of the model calculation, anomaly detection may be found difficult in locations where a low resistivity band has not grown enough locally. It was possible from these facts to assume a model in which the low resistivity band exists directly below the Shigesumi valley, suggesting existence of faults. 2 refs., 8 figs.

  19. The adhesion behavior of carbon coating studied by re-indentation during in situ TEM nanoindentation

    Energy Technology Data Exchange (ETDEWEB)

    Fan, Xue; Diao, Dongfeng, E-mail: dfdiao@szu.edu.cn

    2016-01-30

    Graphical abstract: Nanoscale adhesion induced response in terms of re-indentation was directly observed. During unloading (start from B), the re-indentation phenomenon with the displacement sudden drop and the external loading force change from tension (C) to compression (D) within 0.1 s was captured by in situ TEM nanoindentation. - Highlights: • In situ TEM nanoindentation was performed on carbon coating. • Adhesion induced nano-response of re-indentation was directly observed. • Adhesive forces were measured from the load–displacement curves. • Adhesion energies released for re-indentation were quantitatively analyzed. • Carbon coating reduced the impact of adhesion for silicon substrate. - Abstract: We report a nanoscale adhesion induced nano-response in terms of re-indentation during in situ transmission electron microscope (TEM) nanoindentation on the carbon coating with silicon substrate. The adhesive force generated with nanoindentation was measured, and re-indentation phenomenon during unloading with displacement sudden drop and external loading force change from tension to compression was found. The occurrence of re-indentation during unloading was ascribed to the adhesive force of the contact interface between the indenter and the coating surface. Adhesion energies released for re-indentation processes were quantitatively analyzed from the re-indentation load–displacement curves, and carbon coating reduced the impact of adhesion for silicon substrate. The adhesion induced nano-response of contact surfaces would affect the reliability and performance of nano devices.

  20. In Situ High-Resolution Transmission Electron Microscopy (TEM) Observation of Sn Nanoparticles on SnO2 Nanotubes Under Lithiation.

    Science.gov (United States)

    Cheong, Jun Young; Chang, Joon Ha; Kim, Sung Joo; Kim, Chanhoon; Seo, Hyeon Kook; Shin, Jae Won; Yuk, Jong Min; Lee, Jeong Yong; Kim, Il-Doo

    2017-12-01

    We trace Sn nanoparticles (NPs) produced from SnO2 nanotubes (NTs) during lithiation initialized by high energy e-beam irradiation. The growth dynamics of Sn NPs is visualized in liquid electrolytes by graphene liquid cell transmission electron microscopy. The observation reveals that Sn NPs grow on the surface of SnO2 NTs via coalescence and the final shape of agglomerated NPs is governed by surface energy of the Sn NPs and the interfacial energy between Sn NPs and SnO2 NTs. Our result will likely benefit more rational material design of the ideal interface for facile ion insertion.

  1. High resolution TEM study of Ni4Ti3 precipitates in austenitic Ni51Ti49

    International Nuclear Information System (INIS)

    Tirry, Wim; Schryvers, Dominique

    2003-01-01

    Binary NiTi with a composition of 51 at.% Ni was heat treated to form lens-shaped Ni 4 Ti 3 precipitates that are coherent or semi-coherent with the B2 matrix. High resolution transmission electron microscopy (HRTEM) was used to study the internal structure of the precipitates, precipitate-precipitate and matrix-precipitate interfaces and the deformation of the B2 matrix near a precipitate. Observations were made in the B2 and B2 zones and compared with computer simulated high resolution images. The B2 observations made it possible to study the [0 0 1] H zone orientation of Ni 4 Ti 3 (direction defined according to the hexagonal unit cell of Ni 4 Ti 3 ) which corresponds to the normal of the central plane of the discs. In these images the superperiodicity of the 4:3 ordering is clearly visible confirming the known atomic structure. Close to the precipitate the B2 matrix is deformed, as determined by measuring the interplanar spacing from the HRTEM images. The observed deformations are compared with theoretical models for the stress field

  2. Studying the Kinetics of Crystalline Silicon Nanoparticle Lithiation with In Situ Transmission Electron Microscopy

    KAUST Repository

    McDowell, Matthew T.

    2012-09-04

    In situ transmission electron microscopy (TEM) is used to study the electrochemical lithiation of high-capacity crystalline Si nanoparticles for use in Li-ion battery anodes. The lithiation reaction slows down as it progresses into the particle interior, and analysis suggests that this behavior is due not to diffusion limitation but instead to the influence of mechanical stress on the driving force for reaction. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Studying the Kinetics of Crystalline Silicon Nanoparticle Lithiation with In Situ Transmission Electron Microscopy

    KAUST Repository

    McDowell, Matthew T.; Ryu, Ill; Lee, Seok Woo; Wang, Chongmin; Nix, William D.; Cui, Yi

    2012-01-01

    In situ transmission electron microscopy (TEM) is used to study the electrochemical lithiation of high-capacity crystalline Si nanoparticles for use in Li-ion battery anodes. The lithiation reaction slows down as it progresses into the particle interior, and analysis suggests that this behavior is due not to diffusion limitation but instead to the influence of mechanical stress on the driving force for reaction. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Moessbauer effect and TEM in mineralogy

    International Nuclear Information System (INIS)

    Ferrow, E.A.

    1994-01-01

    Moessbauer effect (ME) provides useful information on oxidation state, co-ordination number, co-ordination state, site occupancies, and magnetic properties of Fe-bearing phases. The information gained by ME together with the information provided by other conventional techniques is used to extract temperature, pressure, and kinetics of rock-forming processes. Nevertheless, ME requires that the phases studied are homogeneous over an extremely large volume and that Fe is a major component of the system. Transmission electron microscopy (TEM), on the other hand, provides similar information over a very small volume for a system of any component. However, present TEM spectrometers do not provide sufficient resolution to detect the mixed oxidation state. A complete characterisation of phases in rocks requires, therefore, that conventional techniques be combined with TEM. (orig.)

  5. In situ TEM study of microplasticity and Bauschinger effect in nanocrystalline metals

    International Nuclear Information System (INIS)

    Rajagopalan, Jagannathan; Rentenberger, Christian; Peter Karnthaler, H.; Dehm, Gerhard; Saif, M. Taher A.

    2010-01-01

    In situ transmission electron microscopy straining experiments with concurrent macroscopic stress-strain measurements were performed to study the effect of microstructural heterogeneity on the deformation behavior of nanocrystalline metal films. In microstructurally heterogeneous gold films (mean grain size d m = 70 nm) comprising randomly oriented grains, dislocation activity is confined to relatively larger grains, with smaller grains deforming elastically, even at applied strains approaching 1.2%. This extended microplasticity leads to build-up of internal stresses, inducing a large Bauschinger effect during unloading. Microstructurally heterogeneous aluminum films (d m = 140 nm) also show similar behavior. In contrast, microstructurally homogeneous aluminum films comprising mainly two grain families, both favorably oriented for dislocation glide, show limited microplastic deformation and minimal Bauschinger effect despite having a comparable mean grain size (d m = 120 nm). A simple model is proposed to describe these observations. Overall, our results emphasize the need to consider both microstructural size and heterogeneity in modeling the mechanical behavior of nanocrystalline metals.

  6. In situ TEM study of microplasticity and Bauschinger effect in nanocrystalline metals

    Energy Technology Data Exchange (ETDEWEB)

    Rajagopalan, Jagannathan [Mechanical Science and Engineering Department, University of Illinois at Urbana-Champaign, 1206 W Green Street, Urbana, IL 61801 (United States); Rentenberger, Christian; Peter Karnthaler, H. [Physics of Nanostructured Materials, Faculty of Physics, University of Vienna, Boltzmanngasse 5, A-1090 Wien (Austria); Dehm, Gerhard [Erich Schmid Institute of Materials Science, Austrian Academy of Sciences, and Dept. Materials Physics, University of Leoben, Jahnstr.12, 8700 Leoben (Austria); Saif, M. Taher A., E-mail: saif@illinois.edu [Mechanical Science and Engineering Department, University of Illinois at Urbana-Champaign, 1206 W Green Street, Urbana, IL 61801 (United States)

    2010-08-15

    In situ transmission electron microscopy straining experiments with concurrent macroscopic stress-strain measurements were performed to study the effect of microstructural heterogeneity on the deformation behavior of nanocrystalline metal films. In microstructurally heterogeneous gold films (mean grain size d{sub m} = 70 nm) comprising randomly oriented grains, dislocation activity is confined to relatively larger grains, with smaller grains deforming elastically, even at applied strains approaching 1.2%. This extended microplasticity leads to build-up of internal stresses, inducing a large Bauschinger effect during unloading. Microstructurally heterogeneous aluminum films (d{sub m} = 140 nm) also show similar behavior. In contrast, microstructurally homogeneous aluminum films comprising mainly two grain families, both favorably oriented for dislocation glide, show limited microplastic deformation and minimal Bauschinger effect despite having a comparable mean grain size (d{sub m} = 120 nm). A simple model is proposed to describe these observations. Overall, our results emphasize the need to consider both microstructural size and heterogeneity in modeling the mechanical behavior of nanocrystalline metals.

  7. Microstructural study of codeposited pentacene:perfluoropentacene grown on KCl by TEM techniques

    Science.gov (United States)

    Félix, Rocío; Breuer, Tobias; Witte, Gregor; Volz, Kerstin; Gries, Katharina I.

    2017-08-01

    Transmission electron microscopy techniques have been used as a research tool to derive information on structure and orientation of organic semiconductor blends. Within this work, we have studied the structure and morphology of pentacene (PEN, C22H14) and perfluoropentacene (PFP, C22F14) blends grown with [2:1] and [1:2] mixing ratios on KCl substrates. The [2:1] mixture exhibits a uniform layer on the substrate with domains that are rotated in-plane by 90° towards each other. Electron diffraction experiments revealed that these domains are formed by a crystalline mixed phase (consisting of PEN and PFP) and a PEN phase in excess whose lattice parameters are rather similar. By contrast, in the [1:2] blend, two different arrangements were found. The majority of the sample exhibits some spicular fibers on a background layer lying on top of the KCl substrate. The microstructural characterization revealed that these fibers consist of pure PFP in excess while the background layer is formed by the mixed phase. The other arrangement, which is present to a lesser extent, consists of a PFP film that is in direct contact with the KCl substrate. Using electron diffraction experiments, the orientation of the different phases with respect to each other and in some cases relative to the KCl substrate has been determined.

  8. Studying the TEM response of a 3-D conductor at a geological contact using the FDTD method

    Energy Technology Data Exchange (ETDEWEB)

    Wang, T.; Tripp, A.C.; Hohmann, G.W. [Univ. of Utah, Salt Lake City, UT (United States). Dept. of Geology and Geophysics

    1995-07-01

    Many mineral targets are located near contact zones. Since the change of resistivity across the contact can distort or obscure the transient electromagnetic (TEM) response of the target, it is important to understand the possible effects. Previous investigators have examined similar problems using scale models. For example, Spies and Parker (1984) studied the TEM responses of fixed-loop and moving-loop configurations to geological contacts with lateral resistivity variations. More recently, Wilt (1991) systematically studied TEM soundings near a geological contact and observed that different survey systems respond to the contact in different ways. This paper will illustrate the use of the finite-difference, time-domain (FDTD) algorithm of Wang and Hohmann (1993) for calculating the TEM response of a 3-D conductive body at a geological contact. The algorithm is based on the Yee staggered grid FDTD method for solving the transient electrical nonmagnetic field responses of a 3-D model. On a suitable computer, a wide range of model responses can be readily calculated, a versatility that scale modeling does not share. This study uses a fixed transmitter loop, roving-receiver configuration. Many other configurations can be regarded as special cases of this survey. It is commonly employed, for instance, by the Newmont EMP (Body and Wiles, 1984), UTEM (West et al., 1984), and Geonics EM37 systems. The configuration also facilitates finite-difference, time-domain modeling because it does not require frequent movement of the source.

  9. In-situ irradiation of cerium precursors in TEM to study nanocrystal formation

    Science.gov (United States)

    Asghar, Muhammad Sajid Ali; Sabri, Mohammed Mohammed; Tian, Zijian; Möbus, Günter

    2017-09-01

    Three of the most commonly used precursor chemicals for wet-chemical nano-ceria synthesis are examined by means of direct dry electron irradiation in TEM. Transformation reactions of micron-size carbonate, chloride, and nitrate grains into nanocrystallites (internal or external) are recorded in situ. Progress of possible redox-changes of cerium is tracked by EELS. We find a straight local oxidation reaction for carbonates, but external nanorod formation by condensation in the case of chlorides, while nitrates show a multi-stage complex redox behaviour.

  10. In situ TEM study of deformation twinning in Ni-Mn-Ga non-modulated martensite

    Czech Academy of Sciences Publication Activity Database

    Zárubová, Niva; Ge, Y.; Heczko, Oleg; Hannula, S.-P.

    2013-01-01

    Roč. 61, č. 14 (2013), s. 5290-5299 ISSN 1359-6454 R&D Projects: GA ČR(CZ) GAP107/11/0391; GA MŠk(CZ) LM2011026; GA ČR GAP107/12/0800; GA AV ČR IAA100100920 Institutional support: RVO:68378271 Keywords : Ni-Mn-Ga * in situ TEM * magnetic shape memory * deformation twinning * twinning dislocation Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 3.940, year: 2013

  11. Neutron, x-ray scattering and TEM studies of Ni-Ti multilayers

    International Nuclear Information System (INIS)

    Keem, J.E.; Wood, J.; Grupido, N.; Hart, K.; Nutt, S.; Reichel, D.G.; Yelon, W.B.

    1988-01-01

    The authors present an analysis of Ni-Ti multilayer neutron reflectors and supermirrors undertaken to identify the causes of the lower than expected observed scattering power and critical angle enhancement of Ni-Ti supermirrors. Results of these investigations focus attention on cusp formation in the Ni-Ti bilayers as probable cause for the reduced neutron scattering power. Grazing angle x-ray and neutron scattering, wide angle neutron diffraction and analytical cross sectional TEM have been used. The multilayers were produced by magnetron sputtering and ion-beam deposition on float glass substrates and silicon wafers

  12. Sub-surface microstructure of single and polycrystalline tungsten after high flux plasma exposure studied by TEM

    Energy Technology Data Exchange (ETDEWEB)

    Dubinko, A., E-mail: adubinko@sckcen.be [Institute for Nuclear Material Sciences, SCK-CEN, 2400 Mol (Belgium); Department of Applied Physics, Ghent University, 9000 Ghent (Belgium); Terentyev, D. [Institute for Nuclear Material Sciences, SCK-CEN, 2400 Mol (Belgium); Bakaeva, A. [Institute for Nuclear Material Sciences, SCK-CEN, 2400 Mol (Belgium); Department of Applied Physics, Ghent University, 9000 Ghent (Belgium); Hernández-Mayoral, M. [Division of Materials, CIEMAT, 28040 Madrid (Spain); De Temmerman, G. [ITER Organization, Route de Vinon-sur-Verdon, CS 90 046, 13067 St Paul-lez-Durance Cedex (France); Buzi, L. [Forschungszentrum Julich, Inst. Energie & Klimaforsch Plasmaphys, D-52425 Julich (Germany); Noterdaeme, J.-M. [Department of Applied Physics, Ghent University, 9000 Ghent (Belgium); Unterberg, B. [Forschungszentrum Julich, Inst. Energie & Klimaforsch Plasmaphys, D-52425 Julich (Germany)

    2017-01-30

    Highlights: • Plasma exposure induces dislocation-dominated microstructure as indicated by TEM. • Plasma exposure increases surface dislocation density by an order of magnitude in the polycrystalline tungsten. • Intensive dislocation-grain boundary interaction observed in polycrystalline tungsten. • Dislocation loops are observed in both polycrystalline and single crystal tungsten. - Abstract: We have performed high flux plasma exposure of tungsten and subsequent microstructural characterization using transmission electron microscopy (TEM) techniques. The aim was to reveal the nanometric features in the sub-surface region as well as to compare the microstructural evolution in tungsten single crystal and ITER-relevant specification. In both types of samples, TEM examination revealed the formation of a dense dislocation network and dislocation tangles. The estimated dislocation density in the sub-surface region was of the order of 10{sup 14} m{sup −2} and it gradually decreased with a depth position of the examined sample. Besides individual dislocation lines, networks and tangles, the interstitial dislocation loops have been observed in all examined samples only after the exposure. Contrary to that, examination of the pristine single crystal W and backside of the plasma-exposed samples did not reveal the presence of dislocation loops and tangles. This clearly proves that high flux plasma exposure induces severe plastic deformation in the sub-surface region irrespective of the presence of initial dislocations and sub-grains, and the formation of dislocation tangles, networks and interstitial loops is a co-product of thermal stress and intensive plasma particles uptake.

  13. Polycrystalline oxides formation during transient oxidation of (001) Cu-Ni binary alloys studied by in situ TEM and XRD

    International Nuclear Information System (INIS)

    Yang, J.C.; Li, Z.Q.; Sun, L.; Zhou, G.W.; Eastman, J.A.; Fong, D.D.; Fuoss, P.H.; Baldo, P.M.; Rehn, L.E.; Thompson, L.J.

    2009-01-01

    The nucleation and growth of Cu 2 O and NiO islands due to oxidation of Cu x Ni 1-x (001) films were monitored, at various temperatures, by in situ ultra-high vacuum (UHV) transmission electron microscopy (TEM) and in situ synchrotron X-ray diffraction (XRD). In remarkable contrast to our previous observations of Cu and Cu-Au oxidation, irregular-shaped polycrystalline oxide islands formed with respect to the Cu-Ni alloy film, and an unusual second oxide nucleation stage was noted. In situ XRD experiments revealed that NiO formed first epitaxially, then other orientations appeared, and finally polycrystalline Cu 2 O developed as the oxidation pressure was increased. The segregation of Ni and Cu towards or away, respectively, from the alloy surface during oxidation could disrupt the surface and cause polycrystalline oxide formation.

  14. A study on the microstructure of Pt/TaN/Si films by high resolution TEM analysis

    CERN Document Server

    Cho, K N; Oh, J E; Park, C S; Lee, S I; Lee, M Y

    1998-01-01

    The microstructure change of Pt/amorphous TaN/Si films after various heat treatments has been investigated by high resolution transmission electron microscopy (HR-TEM) analysis. TaN thin films are deposited by remote plasma metalorganic chemical vapor deposition (RP-MOCVD) using pentakis-dimethyl-amino-tantalum (PDMATa) and radical sources, hydrogen and ammonia plasma. Deposited TaN thin film shows excellent barrier properties such as good resistance against oxidation after post-heat treatment at high temperature. In the case of hydrogen plasma, however, diffusion of Pt into TaN layer was observed, which was caused by the out-diffusion of carbon through the grain boundaries of Pt. In the case of ammonia plasma, the formation of thin oxide layer at the Pt/TaN interface was observed.

  15. Recombination-related properties of a-screw dislocations in GaN: A combined CL, EBIC, TEM study

    Energy Technology Data Exchange (ETDEWEB)

    Medvedev, O. S., E-mail: o.s.medvedev@spbu.ru; Mikhailovskii, V. Yu. [V.A. Fok Institute of Physics, St. Petersburg State University (Russian Federation); IRC for Nanotechnology, Research Park, St.-Petersburg State University (Russian Federation); Vyvenko, O. F.; Bondarenko, A. S.; Ubyivovk, E. V. [V.A. Fok Institute of Physics, St. Petersburg State University (Russian Federation); Peretzki, P.; Seibt, M. [IV. Physikalisches Institut Georg-August Universität Göttingen (Germany)

    2016-06-17

    Cathodoluminescence (CL), electron beam current (EBIC) and transmission electron microscopy (TEM) techniques have been applied to investigate recombination properties and structure of freshly introduced dislocations in low-ohmic GaN crystals. It was confirmed that the only a-screw dislocations exhibited an intense characteristic dislocation-related luminescence (DRL) which persisted up to room temperature and was red-shifted by about 0.3 eV with respect to the band gap energy not only in HVPE but also in MOCVD grown samples. EBIC contrast of the dislocations was found to be temperature independent indicating that the dislocation-related recombination level is situated below 200 meV with respect of conduction band minimum. With the increasing of the magnification of the dislocation TEM cross-sectional images they were found to disappear, probably, due to the recombination enhanced dislocation glide (REDG) under electron beam exposure which was immediately observed in CL investigations on a large scale. The stacking fault ribbon in the core of dissociated a-screw dislocation which form a quantum well for electrons was proposed to play an important role both in DRL spectrum formation and in REDG.

  16. From Nanoparticles to Process An Aberration Corrected TEM Study of Fischer Tropsch Catalysts at Various Steps of the Process

    International Nuclear Information System (INIS)

    Braidy, N.; Blanchard, J.; Abatzoglou, N.; Andrei, C.

    2011-01-01

    χThe nanostructure of Fischer-Tropsch (FT) Fe carbides are investigated using aberration-corrected high-resolution transmission electron microscopy (TEM). The plasma-generated Fe carbides are analyzed just after synthesis, following reduction via a H2 treatment step and once used as FT catalyst and deactivated. The as-produced nanoparticles (NPs) are seen to be abundantly covered with graphitic and amorphous carbon. Using the extended information limit from the spherical aberration-corrected TEM, the NPs could be indexed as a mixture of NPs in the θ-Fe 3 C and χ-Fe 5 C 2 phases. The reduction treatment exposed the NPs by removing most of the carbonaceous speSubscript textcies while retaining the χ-Fe 5 C 2 . Fe-carbides NPs submitted to conditions typical to FT synthesis develop a Fe3O4 shell which eventually consumes the NPs up to a point where 3-4 nm residual carbide is left at the center of the particle. Subscript textVarious mechanisms explaining the formation of such a microstructure are discussed. (author)

  17. TEM and EELS studies of microwave-irradiation synthesis of bimetallic platinum nanocatalysts

    CSIR Research Space (South Africa)

    Mathe, NR

    2014-01-01

    Full Text Available .M., Quevedo-Lopez M.A., Betancourt-Galindo R. and Buenos-Baques D. 2011 Journal of Nanomaterials 2011 [8] Langlois C., Alloyeau D., Bouar Y.L., Loiseau A., Oikawa T., Mottet C. and Ricolleau C. 2008 Faraday Discussions 138 375 - 91 Electron Microscopy...

  18. The outcome of rectal cancer after early salvage TME following TEM compared with primary TME: a case-matched study.

    Science.gov (United States)

    Levic, K; Bulut, O; Hesselfeldt, P; Bülow, S

    2013-08-01

    Transanal endoscopic microsurgery (TEM) allows locally complete resection of early rectal cancer as an alternative to conventional radical surgery. In case of unfavourable histology after TEM, or positive resection margins, salvage surgery can be performed. However, it is unclear if the results are equivalent to primary treatment with total mesorectal excision (TME). The aim of this retrospective study was to determine whether there is a difference in outcome between patients who underwent early salvage resection with TME after TEM, and those who underwent primary TME for rectal cancer. From 1997 to 2011, early salvage surgery with TME after TEM was performed in 25 patients in our institution. These patients were compared with 25 patients who underwent primary TME, matched according to gender, age (±2 years), cancer stage and operative procedure. Data were obtained from the patients' charts and reviewed retrospectively. No patients received preoperative chemotherapy. Perioperative data and oncological outcome were analysed. The Mann-Whitney U-test and Fisher's exact test were used to compare the results between the two groups. There was no significant difference between the two groups in median operating time (P = 0.39), median blood loss (P = 0.19) or intraoperative complications (P = 1.00). The 30-day mortality was 8 % (n = 2) among patients who underwent salvage TME after TEM, and no patients died in the primary TME group (P = 0.49). There was no significant difference between two groups of patients in the median number of harvested lymph nodes (P = 0.34), median circumferential resection margin (CRM) (P = 0.99) or the completeness of the mesorectal fascia plane. No local recurrences occurred among the patients with salvage TME, and there were 2 patients (8 %) with local recurrences among the patients with primary TME (P = 0.49). Distant metastasis occurred in one patient (4 %) after salvage TME and in 3 patients (12 %) with primary TME (P = 0.61). The median

  19. Bauxite and bauxite residue, characterization and electron microscopy study

    International Nuclear Information System (INIS)

    Antunes, M.L.P.; Conceicao, F.T.; Toledo, S.P.; Kiyohara, P.K.

    2012-01-01

    Through the Bayer process, bauxite is refined and alumina is produced. In this process, a highly alkaline residue, red mud is generated and its disposal represents an environmental problem. The aim of this paper is to present the characterization of Brazilian bauxite and Brazilian red mud by: X-ray diffraction, specific surface area, chemical composition analysis by ICP-MS, transmission electron microscopy (TEM) and energy dispersive X-ray spectrometry (EDS), and scanning electron microscopy (SEM) and discuss possible applications of this residue. The results identify as a constituent of both materials: Al 2 O 3 , Fe 2 O 3 , TiO 2 and SiO 2 and the presence of Na 2 O in residue. The analysis by electron microscopy of Bauxite shows particles with hexagonal shape and red mud shows small particles size. (author)

  20. Applications of advanced electron microscopy techniques to the studies of radiation effects in ceramic materials

    International Nuclear Information System (INIS)

    Wang, L.M.

    1998-01-01

    This paper summarizes some recent results from the application of several advanced transmission electron microscopy (TEM) techniques to the studies of radiation effects in insulators with the main focus on radiation-induced amorphization. These techniques include in situ TEM during ion-beam irradiation at cryogenic and elevated temperatures, cross-sectional TEM, high-resolution TEM, and image simulation on partially damaged materials, as well as digital TEM with image processing and analysis. The combination of these techniques may often provide very detailed information about the microstructure evolution during energetic particle irradiation, especially at the early stages, which is unobtainable with any other analytical methods. These techniques have been successfully applied to the analysis of a large group of ion-beam-irradiated ceramics, including quartz, silicon carbides, uranium oxide, apatite, spinel and other complex mineral phases. The advantages and limitations of each technique, as well as some important technical details for the analysis of radiation damage in ceramics are presented. (orig.)

  1. Networking strategies of the microscopy community for improved utilization of advanced instruments: (3) Two European initiatives to support TEM infrastructures and promote electron microscopy over Europe, ESTEEM (2006-2011) and ESTEEM 2 (2012-2016)

    International Nuclear Information System (INIS)

    Snoeck, E.; Van Tendeloo, G.

    2014-01-01

    The ESTEEM consortium of electron microscopy laboratories for materials science and solid-state physics has been created as an EU-supported delocalized infrastructure to bring together the major electron microscopy centres in Europe. Its main objectives were to develop networking, to offer trans-national access to these centres with specialized and complementary techniques and skills and to upgrade in close collaboration different technical and methodological aspects such as tomography, spectroscopy, holography, detectors, and specimen holders. These efforts were aimed to strengthen the position of European microscopy and to generate new technologies potentially of high relevance in many domains identified as strategic. Following the success of the first program, ESTEEM has been conducted again in 2012 for 4 more years with an enlarged set of partners. (authors)

  2. TEM sample preparation by FIB for carbon nanotube interconnects

    International Nuclear Information System (INIS)

    Ke, Xiaoxing; Bals, Sara; Romo Negreira, Ainhoa; Hantschel, Thomas; Bender, Hugo; Van Tendeloo, Gustaaf

    2009-01-01

    A powerful method to study carbon nanotubes (CNTs) grown in patterned substrates for potential interconnects applications is transmission electron microscopy (TEM). However, high-quality TEM samples are necessary for such a study. Here, TEM specimen preparation by focused ion beam (FIB) has been used to obtain lamellae of patterned samples containing CNTs grown inside contact holes. A dual-cap Pt protection layer and an extensive 5 kV cleaning procedure are applied in order to preserve the CNTs and avoid deterioration during milling. TEM results show that the inner shell structure of the carbon nanotubes has been preserved, which proves that focused ion beam is a useful technique to prepare TEM samples of CNT interconnects.

  3. TEM sample preparation by FIB for carbon nanotube interconnects

    Energy Technology Data Exchange (ETDEWEB)

    Ke, Xiaoxing, E-mail: xiaoxing.ke@ua.ac.be [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Bals, Sara [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Romo Negreira, Ainhoa [IMEC, Kapeldreef 75, B-3001 Leuven (Belgium); Metallurgy and Materials Engineering Department, KU Leuven, Kasteelpark Arenberg 44, Leuven B-3001 (Belgium); Hantschel, Thomas; Bender, Hugo [IMEC, Kapeldreef 75, B-3001 Leuven (Belgium); Van Tendeloo, Gustaaf [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium)

    2009-10-15

    A powerful method to study carbon nanotubes (CNTs) grown in patterned substrates for potential interconnects applications is transmission electron microscopy (TEM). However, high-quality TEM samples are necessary for such a study. Here, TEM specimen preparation by focused ion beam (FIB) has been used to obtain lamellae of patterned samples containing CNTs grown inside contact holes. A dual-cap Pt protection layer and an extensive 5 kV cleaning procedure are applied in order to preserve the CNTs and avoid deterioration during milling. TEM results show that the inner shell structure of the carbon nanotubes has been preserved, which proves that focused ion beam is a useful technique to prepare TEM samples of CNT interconnects.

  4. Nucleation and Nanometric Inhomogeneity in Niobiogermanate Glass: In-Situ Inelastic Light Scattering and TEM Studies

    International Nuclear Information System (INIS)

    Takahashi, Y; Ihara, R; Fujiwara, T; Osada, M; Masai, H

    2011-01-01

    We performed in-situ inelastic light scattering measurement in KNbGeO 5 glass with a high nucleation ability during heating in order to elucidate nanocrystallization dynamics. The results of the in-situ measurement and TEM observation revealed that nanometric heterogeneous region (∼1-2 nm) consisting of the Nb-richer phase develops, i.e., K 3 Nb 7 O 19 , at the temperature, in which glassy-supercooled-liquid (SCL) phase-transition occurs, i.e., precursive stage of nanocrystallization. This strongly suggests that evolution of the nanometric Nb-richer phase in the SCL phase corresponds to nucleation in the KNbGeO 5 glass.

  5. TEM study of internal oxidation in an ODS-Eurofer alloy

    International Nuclear Information System (INIS)

    Klimenkov, M.; Lindau, R.; Moeslang, A.

    2009-01-01

    Analytical TEM investigations of samples from an oxide dispersion-strengthened Eurofer batch show the formation of new type of precipitates of Fe-Cr-V-O composition and a size of 40-250 nm. Structural HRTEM analysis reveals that the precipitates consist of (Mn,Fe)(Cr,V) 2 O 4 manganese chromium oxide of spinel structure. In some cases, the inclusions order along lines that can reach more than ten micrometers in length. Such lines of large particles might have a negative influence on the mechanical properties of the steel, as was observed. It is assumed that they form by internal oxidation during hot isostatic pressing due to the high oxygen content of the mechanically alloyed powder.

  6. TEM and AFM study of WO3 nanosize growth on α-Al2O3

    International Nuclear Information System (INIS)

    Al-Mohammad, A.

    2007-07-01

    WO 3 thin films have been deposited by thermal evaporation on (0001) and (1012 ) planes of alumina oxide single crystal and annealed either in Oxygen or in air atmosphere. The morphology and crystallographic structure of films (as-deposited and annealed films) have been characterized by Atomic Force Microscope (AFM), transmission electron microscope (TEM), and transmission electron diffraction (TED). During annealing, the films undergo important morphological and structural changes. The annealed films exhibit large grains. These grains have the monoclinic structure in epitaxial orientations. The grains are made of twinned microdomains elongated in the [100] direction resulting of a preferential growth. The microdomains are along the three different directions on the (0001) α-Al 2 O 3 surface and only one direction on the (1012 ) α-Al 2 O 3 one.(author)

  7. XPS and TEM study of W-DLC/DLC double-layered film

    International Nuclear Information System (INIS)

    Takeno, Takanori; Komiyama, Takao; Miki, Hiroyuki; Takagi, Toshiyuki; Aoyama, Takashi

    2009-01-01

    A double-layered film of tungsten-containing diamond-like carbon (W-DLC) and DLC, (W-DLC)/DLC, was investigated. A film of 1.6 μm in thickness was deposited onto silicon substrate. The investigate double-layered coating was deposited by using the combination of PECVD and co-sputtering of tungsten metal target. Structure, interface and chemical bonding state of the investigated film were analyzed by Transmission electron microscope (TEM) and X-ray photoelectron spectroscopy (XPS). From the results of the analyses, the structure of double-layered film is that amorphous phase of carbon is continued from DLC to W-DLC and tungsten metal clusters are dispersed in W-DLC layer.

  8. A TEM study of strained SiGe/Si and related heteroepitaxial structures

    International Nuclear Information System (INIS)

    Benedetti, Alessandro

    2002-01-01

    The role of SiGe/Si heterostructures and related materials has become increasingly important within the last few decades. In order to increase the scale of integration, however, devices with active elements not larger than few tens of nanometer have been recently introduced. There is, therefore, a strong need for an analytical technique capable of giving information about submicron-sized components. An investigation on a nanometre scale can be performed by the combination of a fully equipped Transmission Electron Microscope (TEM) with a Field Emission Gun (PEG) electron source, which enables one to use a wide range of analytical techniques with an electron probe as small as 0.5 nm. In this work, two different types of SiGe/Si-based devices were investigated. Strained-Si n-channel MOSFETs. The use of Strained-Si n-channel grown on SiGe should improve both carrier mobility and transconductance with respect to conventional MOSFETs. Materials analysed in this work showed an extremely high transconductance but a rather low mobility. In order to relate their microstructural properties to their electrical performance, as well as to improve the device design, a full quantitative and qualitative structural characterisation was performed. SiGe Multiple Quantum Wells (MQW) IR detectors Light detection is achieved by collecting the photogenerated carriers, injected from the SiGe QWs layers into the Si substrate. A key factor is the Ge profile across a single QW, since it governs the band structure and therefore the device performances. Four different TEM techniques were used to determine the Ge distribution across a single well, showing an overall good agreement among the results. The Ge profiles broadening, consistent with data available in literature, was successfully explained and theoretically predicted by the combined effect of Ge segregation and gas dwell times within the reactor. (author)

  9. Transmission electron microscopy study of Listeria monocytogenes serotype 1/2a cells exposed to sublethal heat stress and carvacrol

    Science.gov (United States)

    The objective of this study was to investigate the morphological changes that occurred in Listeria monocytogenes serotype 1/2a cells as visualized by transmission electron microscopy (TEM) after exposure to sublethal heat stress at 48°C for 60 min and in combination with lethal concentration of carv...

  10. Electron microscopy for Engineers

    International Nuclear Information System (INIS)

    Jones, I P

    2009-01-01

    This paper reviews the application of (mainly) Transmission Electron Microscopy (TEM) in an engineering context. The first two sections are TEM and chemical in nature; the final three sections are more general and include aspects of Scanning Electron Microscopy (SEM).

  11. Proceedings of 11. Conference on Electron Microscopy of Solids

    International Nuclear Information System (INIS)

    2002-01-01

    The conference is the cyclically organised discussion forum on problems connected with application of different electron microscopy techniques for the study of solid state materials. The main topics of 11 conference on Electron Microscopy of Solids held in Krynica (PL) in 2002 was: application of TEM in materials science; analytical techniques and orientation imaging in materials science; high resolution TEM in electronic materials; TEM and SEM application in ceramic and composites; advanced TEM techniques; advanced analytical and orientation imaging techniques; application of TEM in investigations of amorphous and nanocrystalline material; Intermetallic and superalloys; TEM application in martensite alloys; TEM and SEM application in research of iron base alloys; TEM studies of deformed alloys; TEM application in thin films and surface layer studies; TEM and SEM application in materials science

  12. The Development of an In-Situ TEM Technique for Studying Corrosion Behavior as Applied to Zirconium-Based Alloys

    Science.gov (United States)

    Harlow, Wayne

    Zirconium-based alloys are a commonly used material for nuclear fuel rod cladding, due to its low neutron cross section and good corrosion properties. However, corrosion is still a limiting factor in fuel rod lifespan, which restricts burn up levels, and thus efficiency, that can be achieved. While long-term corrosion behavior has been studied through both reactor and autoclave samples, the oxide nucleation and growth behavior has not been extensively studied. This work develops a new technique to study the initial stages of corrosion in zirconium-based alloys and the microstructural effects on this process by developing an environmental cell system for the TEM. Nanoscale oxidation parameters are developed, as is a new FIB technique to support this method. Precession diffraction is used in conjunction with in-situ TEM to observe the initial stages of corrosion in these alloys, and oxide thickness is estimated using low-loss EELS. In addition, the stress stabilization of tetragonal ZrO 2 is explored in the context of sample preparation for TEM. It was found that in-situ environmental TEM using an environmental cell replicates the oxidation behavior observed in autoclaved samples in both oxide structure and phases. Utilizing this technique, it was shown that cracking of the oxide layer in zirconium-based alloys is related to oxide relaxation, and not thermal changes. The effect of secondary phase particles on oxidation behavior did not present significant results, however a new method for studying initial oxidation rates using low-loss EELS was developed.

  13. TEM Study of the Orientation Relationship Between Cementite and Ferrite in a Bainitic Low Carbon High Strength Low Alloy Steel

    OpenAIRE

    Illescas Fernandez, Silvia; Brown, A.P.; He, K.; Fernández, Javier; Guilemany Casadamon, Josep Maria

    2005-01-01

    Two different bainitic structures are observed in a steel depending on the sample heat treatment. The different types of bainitic structures exhibit different orientation relationships between cementite and the ferrite matrix. Upper bainite presents a Pitsch orientation relationship and lower bainite presents a Bagaryatski orientation relationship. Different heat treatments of low carbon HSLA steel samples have been studied using TEM in order to find the orientation relationshi...

  14. A FIB/TEM study of butterfly crack formation and white etching area (WEA) microstructural changes under rolling contact fatigue in 100Cr6 bearing steel

    International Nuclear Information System (INIS)

    Evans, M.-H.; Walker, J.C.; Ma, C.; Wang, L.; Wood, R.J.K.

    2013-01-01

    Butterflies are microscopic damage features forming at subsurface material imperfections induced during rolling contact fatigue (RCF) in rolling element bearings. Butterflies can lead to degradation of the load bearing capacity of the material by their associated cracks causing premature spalling failures. Recently, butterfly formation has been cited to be related to a premature failure mode in wind turbine gearbox bearings; white structure flaking (WSF). Butterflies consist of cracks with surrounding microstructural change called ‘white etching area’ (WEA) forming wings that revolve around their initiators. The formation mechanisms of butterflies in bearing steels have been studied over the last 50 years, but are still not fully understood. This paper presents a detailed microstructural analysis of a butterfly that has initiated from a void in standard 100Cr6 bearing steel under rolling contact fatigue on a laboratory two-roller test rig under transient operating conditions. Analysis was conducted using focused ion beam (FIB) tomography, 3D reconstruction and transmission electron microscopy (STEM/TEM) methods. FIB tomography revealed an extensive presence of voids/cavities immediately adjacent to the main crack on the non-WEA side and at the crack tip. This provides evidence for a void/cavity coalescence mechanism for the butterfly cracks formation. Spherical M 3 C carbide deformation and dissolution as part of the microstructural change in WEA were observed in both FIB and STEM/TEM analyses, where TEM analyses also revealed the formation of superfine nano-grains (3–15 nm diameter) intersecting a dissolving spherical M 3 C carbide. This is evidence of the early formation of nano-grains associated with the WEA formation mechanism

  15. A FIB/TEM study of butterfly crack formation and white etching area (WEA) microstructural changes under rolling contact fatigue in 100Cr6 bearing steel

    Energy Technology Data Exchange (ETDEWEB)

    Evans, M.-H., E-mail: martin.evans@soton.ac.uk [National Centre for Advanced Tribology at Southampton (nCATS), University of Southampton, SO17 1BJ (United Kingdom); Walker, J.C.; Ma, C.; Wang, L.; Wood, R.J.K. [National Centre for Advanced Tribology at Southampton (nCATS), University of Southampton, SO17 1BJ (United Kingdom)

    2013-05-15

    Butterflies are microscopic damage features forming at subsurface material imperfections induced during rolling contact fatigue (RCF) in rolling element bearings. Butterflies can lead to degradation of the load bearing capacity of the material by their associated cracks causing premature spalling failures. Recently, butterfly formation has been cited to be related to a premature failure mode in wind turbine gearbox bearings; white structure flaking (WSF). Butterflies consist of cracks with surrounding microstructural change called ‘white etching area’ (WEA) forming wings that revolve around their initiators. The formation mechanisms of butterflies in bearing steels have been studied over the last 50 years, but are still not fully understood. This paper presents a detailed microstructural analysis of a butterfly that has initiated from a void in standard 100Cr6 bearing steel under rolling contact fatigue on a laboratory two-roller test rig under transient operating conditions. Analysis was conducted using focused ion beam (FIB) tomography, 3D reconstruction and transmission electron microscopy (STEM/TEM) methods. FIB tomography revealed an extensive presence of voids/cavities immediately adjacent to the main crack on the non-WEA side and at the crack tip. This provides evidence for a void/cavity coalescence mechanism for the butterfly cracks formation. Spherical M{sub 3}C carbide deformation and dissolution as part of the microstructural change in WEA were observed in both FIB and STEM/TEM analyses, where TEM analyses also revealed the formation of superfine nano-grains (3–15 nm diameter) intersecting a dissolving spherical M{sub 3}C carbide. This is evidence of the early formation of nano-grains associated with the WEA formation mechanism.

  16. Stability of Porous Platinum Nanoparticles: Combined In Situ TEM and Theoretical Study

    DEFF Research Database (Denmark)

    Chang, Shery L. Y.; Barnard, Amanda S.; Dwyer, Christian

    2012-01-01

    Porous platinum nanoparticles provide a route for the development of catalysts that use less platinum without sacrificing catalytic performance. Here, we examine porous platinum nanoparticles using a combination of in situ transmission electron microscopy and calculations based on a first-principles......-parametrized thermodynamic model. Our experimental observations show that the initially irregular morphologies of the as-sythesized porous nanoparticles undergo changes at high temperatures to morphologies having faceted external surfaces with voids present in the interior of the particles. The increasing size of stable...

  17. Dysprosium disilicide nanostructures on silicon(001) studied by scanning tunneling microscopy and transmission electron microscopy

    International Nuclear Information System (INIS)

    Ye Gangfeng; Nogami, Jun; Crimp, Martin A.

    2006-01-01

    The microstructure of self-assembled dysprosium silicide nanostructures on silicon(001) has been studied by scanning tunneling microscopy and transmission electron microscopy. The studies focused on nanostructures that involve multiple atomic layers of the silicide. Cross-sectional high resolution transmission electron microscopy images and fast Fourier transform analysis showed that both hexagonal and orthorhombic/tetragonal silicide phases were present. Both the magnitude and the anisotropy of lattice mismatch between the silicide and the substrate play roles in the morphology and epitaxial growth of the nanostructures formed

  18. Grain Nucleation and Growth in Deformed NiTi Shape Memory Alloys: An In Situ TEM Study

    Science.gov (United States)

    Burow, J.; Frenzel, J.; Somsen, C.; Prokofiev, E.; Valiev, R.; Eggeler, G.

    2017-12-01

    The present study investigates the evolution of nanocrystalline (NC) and ultrafine-grained (UFG) microstructures in plastically deformed NiTi. Two deformed NiTi alloys were subjected to in situ annealing in a transmission electron microscope (TEM) at 400 and 550 °C: an amorphous material state produced by high-pressure torsion (HPT) and a mostly martensitic partly amorphous alloy produced by wire drawing. In situ annealing experiments were performed to characterize the microstructural evolution from the initial nonequilibrium states toward energetically more favorable microstructures. In general, the formation and evolution of nanocrystalline microstructures are governed by the nucleation of new grains and their subsequent growth. Austenite nuclei which form in HPT and wire-drawn microstructures have sizes close to 10 nm. Grain coarsening occurs in a sporadic, nonuniform manner and depends on the physical and chemical features of the local environment. The mobility of grain boundaries in NiTi is governed by the local interaction of each grain with its microstructural environment. Nanograin growth in thin TEM foils seems to follow similar kinetic laws to those in bulk microstructures. The present study demonstrates the strength of in situ TEM analysis and also highlights aspects which need to be considered when interpreting the results.

  19. T6 and T78 tempers of AA6065 alloy: a quantitative TEM study

    Energy Technology Data Exchange (ETDEWEB)

    Tanaka, M.; Warner, T. [Compagnie de Produits Chimiques et Electrometallurgiques Pechiney, Centre de Recherches de Voreppe, 38 (France)

    2000-07-01

    Quantitative transmission electron microscopy is used to characterize the microstructure of an industrial Al-Mg-Si-Cu alloy (AA6056) in a state (T78 temper) desensitized to intergranular corrosion in comparison with the peak aged state (T6 temper). Analysis of dark-field images and of zero-loss filtered selected-area-diffraction patterns, along with EDX spectroscopy, indicates an advanced precipitation of the quaternary phase containing Si and Cu in the T78-tempered alloy compared to the T6 one. This supports the current theory of the desensitization of AA6056 alloy. However, the application of EDX analysis to provide direct evidence of the chemical composition variation in the solid solution across the grain boundary appears less satisfactory. (orig.)

  20. TEM study of the indentation behaviour of thin Au film on GaAs

    International Nuclear Information System (INIS)

    Patriarche, G.; Le Bourhis, E.; Faurie, D.; Renault, P.O.

    2004-01-01

    Au films of 8.9 nm thickness have been sputter deposited onto a (001) GaAs substrate at room temperature. An average grain size of 10 nm and no texture were obtained. Subsequent, nanoindentation tests were performed on the coated specimens and the mechanical response was compared to that of a bulk GaAs sample with the same crystallographic orientation. Furthermore, the loading-unloading curves were analysed in view of transmission electron microscopy plan-view images obtained on the deformed substrate-film specimens and compared to results previously reported in the literature for bulk sample. Constrained plasticity of the films was observed to occur for residual depth to thickness ratio below 0.67. Further, plastic deformation of the substrate happened on coated specimens at loads less than those required to plastically deform bare substrate

  1. Structural characterization and gas reactions of small metal particles by high resolution in-situ TEM (Transmission Electron Microscopy) and TED (Transmission Electron Diffraction)

    Science.gov (United States)

    Heinemann, K.

    1987-01-01

    The detection and size analysis of small metal particles supported on amorphous substrates becomes increasingly difficult when the particle size approaches that of the phase contrast background structures of the support. An approach of digital image analysis, involving Fourier transformation of the original image, filtering, and image reconstruction was studied with respect to the likelihood of unambiguously detecting particles of less than 1 nm diameter on amorphous substrates from a single electron micrograph.

  2. Zeolites - a high resolution electron microscopy study

    International Nuclear Information System (INIS)

    Alfredsson, V.

    1994-10-01

    High resolution transmission electron microscopy (HRTEM) has been used to investigate a number of zeolites (EMT, FAU, LTL, MFI and MOR) and a member of the mesoporous M41S family. The electron optical artefact, manifested as a dark spot in the projected centre of the large zeolite channels, caused by insufficient transfer of certain reflections in the objective lens has been explained. The artefact severely hinders observation of materials confined in the zeolite channels and cavities. It is shown how to circumvent the artefact problem and how to image confined materials in spite of disturbance caused by the artefact. Image processing by means of a Wiener filter has been applied for removal of the artefact. The detailed surface structure of FAU has been investigated. Comparison of experimental micrographs with images simulated using different surface models indicates that the surface can be terminated in different ways depending on synthesis methods. The dealuminated form of FAU (USY) is covered by an amorphous region. Platinum incorporated in FAU has a preponderance to aggregate in the (111) twin planes, probably due to a local difference in cage structure with more spacious cages. It is shown that platinum is intra-zeolitic as opposed to being located on the external surface of the zeolite crystal. This could be deduced from tomography of ultra-thin sections among observations. HRTEM studies of the mesoporous MCM-41 show that the pores have a hexagonal shape and also supports the mechanistic model proposed which involves a cooperative formation of a mesophase including the silicate species as well as the surfactant. 66 refs, 24 figs

  3. Microscopy based studies on the interaction of bio-based silver nanoparticles with Bombyx mori Nuclear Polyhedrosis virus.

    Science.gov (United States)

    Tamilselvan, Selvaraj; Ashokkumar, Thirunavukkarasu; Govindaraju, Kasivelu

    2017-04-01

    In the present investigation, silver nanoparticles (AgNPs) interactions with Bombyx mori Nuclear Polyhedrosis virus (BmNPV) were characterized using High-Resolution Scanning Electron Microscopy (HR-SEM), Energy Dispersive X-ray Analysis (EDAX), Transmission Electron Microscopy (TEM), Atomic Force Microcopy (AFM) and Confocal Microscope (CM). HR-SEM study reveals that the biosynthesized AgNPs have interacted with BmNPV and were found on the surface. TEM micrographs of normal and viral polyhedra treated with AgNPs showed that the nanoparticles were accumulated in the membrane and it was noted that some of the AgNPs successfully penetrated the membrane by reaching the capsid of BmNPV. AFM and confocal microscopy studies reveal that the disruption in the shell membrane tends to lose its stability due to exposure of AgNPs to BmNPV. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Implementation of a Light Source in a TEM Sample Holder for In-situ Studies of Photocatalytic Materials

    DEFF Research Database (Denmark)

    Cavalca, Filippo; Hansen, Thomas Willum; Wagner, Jakob Birkedal

    can be used inside an environmental TEM (ETEM) allowing specimens to be analyzed during exposure to a controlled gas atmosphere and illumination. The holder is presently being used to study a variety of photoreactive materials and structures, including photocatalysts, photonic devices and solar cells....... For example, electron holography is being used to study p-n junctions both in the presence and in the absence of light in order to assess electron beam induced charging and discharging effects during laser light exposure [3]. Here, we present results from ETEM studies of light-induced phenomena that include...

  5. Structural studies of glasses by transmission electron microscopy and electron diffraction

    International Nuclear Information System (INIS)

    Kashchieva, E.P.

    1997-01-01

    The purpose of this work is to present information about the applications of transmission electron microscopy (TEM) and electron diffraction (ED) for structural investigations of glasses. TEM investigations have been carried out on some binary and on a large number of ternary borate-telluride systems where glass-forming oxides, oxides of transitional elements and modified oxides of elements from I, II and III groups in the periodic table, are used as third component. The large experimental data given by TEM method allows the fine classification of the micro-heterogeneities. A special case of micro-heterogeneous structure with technological origin occurs near the boundary between the 2 immiscible liquids obtained at macro-phase separation. TEM was also used for the direct observation of the glass structure and we have studied the nano-scale structure of borate glasses obtained at slow and fast cooling of the melts. The ED possesses advantages for analysis of amorphous thin films or micro-pastilles and it is a very useful technique for study in materials containing simultaneously light and heavy elements. A comparison between the possibilities of the 3 diffraction techniques (X-ray diffraction, neutron diffraction and ED) is presented

  6. TEM/STEM study of Zircaloy-2 with protective FeAl(Cr) layers under simulated BWR environment and high-temperature steam exposure

    Science.gov (United States)

    Park, Donghee; Mouche, Peter A.; Zhong, Weicheng; Mandapaka, Kiran K.; Was, Gary S.; Heuser, Brent J.

    2018-04-01

    FeAl(Cr) thin-film depositions on Zircaloy-2 were studied using transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) with respect to oxidation behavior under simulated boiling water reactor (BWR) conditions and high-temperature steam. Columnar grains of FeAl with Cr in solid solution were formed on Zircaloy-2 coupons using magnetron sputtering. NiFe2O4 precipitates on the surface of the FeAl(Cr) coatings were observed after the sample was exposed to the simulated BWR environment. High-temperature steam exposure resulted in grain growth and consumption of the FeAl(Cr) layer, but no delamination at the interface. Outward Al diffusion from the FeAl(Cr) layer occurred during high-temperature steam exposure (700 °C for 3.6 h) to form a 100-nm-thick alumina oxide layer, which was effective in mitigating oxidation of the Zircaloy-2 coupons. Zr intermetallic precipitates formed near the FeAl(Cr) layer due to the inward diffusion of Fe and Al. The counterflow of vacancies in response to the Al and Fe diffusion led to porosity within the FeAl(Cr) layer.

  7. Transmission Electron Microscopy Study of Individual Carbon Nanotube Breakdown Caused by Joule Heating in Air

    DEFF Research Database (Denmark)

    Mølhave, Kristian; Gudnason, S.B.; Pedersen, Anders Tegtmeier

    2006-01-01

    We present repeated structural and electrical measurements on individual multiwalled carbon nanotubes, alternating between electrical measurements under ambient conditions and transmission electron microscopy (TEM). The multiwalled carbon nanotubes made by chemical vapor deposition were manipulated...

  8. FE-SEM, FIB and TEM Study of Surface Deposits of Apollo 15 Green Glass Volcanic Spherules

    Science.gov (United States)

    Ross, Daniel K.; Thomas-Keprta, K. L.; Rahman, Z.; Wentworth, S. J.; McKay, D. S.

    2011-01-01

    Surface deposits on lunar pyroclastic green (Apollo 15) and orange (Apollo 17) glass spherules have been attributed to condensation from the gas clouds that accompanied fire-fountain eruptions. The fire fountains cast molten lava high above the lunar surface and the silicate melt droplets quenched before landing producing the glass beads. Early investigations showed that these deposits are rich in sulfur and zinc. The deposits are extremely fine-grained and thin, so that it was never possible to determine their chemical compositions cleanly by SEM/EDX or electron probe x-ray analysis because most of the excited volume was in the under-lying silicate glass. We are investigating the surface deposits by TEM, using focused ion beam (FIB) microscopy to extract and thin the surface deposits. Here we report on chemical mapping of a FIB section of surface deposits of an Apollo green glass bead 15401using the ultra-high resolution JEOL 2500 STEM located at NASA Johnson Space Center.

  9. TEM study of xenon bubbles evolution in Xe-implanted Cu. Bubbles shape, epitaxial orientation and adsorption phenomenon

    International Nuclear Information System (INIS)

    Guillot, J.; Cartraud, M.; Garem, H.; Templier, C.; Desoyer, J.C.

    1987-01-01

    TEM is used to perform a study of xenon clusters changes in Xe-implanted Cu. After implantation, xenon is gathered into f.c.c. crystalline precipitates with a lattice parameter value of 0.580 nm. During annealing at 600 0 C large (110) facetted bubbles appear (2r≅35 nm) which contain fluid xenon. When cooling down to 100 K, xenon solidifies on bubbles facets in form of a thin membrane. The epitaxial orientations between solid xenon and copper are the same as adsorbed Xe on Cu(110) [fr

  10. AFM and TEM study of cyclic slip localization in fatigued ferritic X10CrAl24 stainless steel

    International Nuclear Information System (INIS)

    Man, J.; Petrenec, M.; Obrtlik, K.; Polak, J.

    2004-01-01

    Atomic force microscopy and high resolution scanning electron microscopy were applied to the study of surface relief evolution at emerging persistent slip bands (PSBs) in individual grains of ferritic X10CrAl24 stainless steel cycled with constant plastic strain amplitude. Only the combination of both methods can reveal the true shape and fine details of extrusions and intrusions. Quantitative data on the changes of the surface topography of persistent slip markings and on the kinetics of extrusion growth during the fatigue life were obtained. Transmission electron microscopy of surface foils revealed PSBs with the typical, well-known ladder structure. Experimental data on cyclic slip localization in PSBs are compared with those in fcc metals and discussed in terms of vacancy models of surface relief evolution and fatigue crack initiation

  11. TEM study of the nucleation of bubbles induced by He implantation in 316L industrial austenitic stainless steel

    International Nuclear Information System (INIS)

    Jublot-Leclerc, S.; Lescoat, M.-L.; Fortuna, F.; Legras, L.; Li, X.; Gentils, A.

    2015-01-01

    10 keV He ions were implanted in-situ in a TEM into thin foils of 316L industrial austenitic stainless steel at temperatures ranging from 200 to 550 °C. As a result, overpressurized nanometric bubbles are created with density and size depending strongly on both the temperature and fluence of implantation. An investigation on their nucleation and growth is reported through a rigorous statistical analysis whose procedure, including the consideration of free surface effects, is detailed. In the parameter range considered, the results show that an increase of fluence promotes both the nucleation and growth of the bubbles whilst an increase of temperature enhances the growth of the bubbles at the expense of their nucleation. The confrontation of resulting activation energies with existing models for bubble nucleation enables the identification of the underlying mechanisms. In spite of slight differences resulting from different conditions of implantation among which the He concentration, He production rate and He/dpa ratio, it appears that the dominating mechanisms are the same as those obtained in metals in previous studies, which, in addition to corroborating literature results, shows the suitability of in-situ TEM experiments to simulate the production of helium in nuclear materials. - Highlights: • A rigorous TEM statistical analysis, including free surface effects, is reported. • Increasing He fluence promotes both the nucleation and growth of bubbles. • Increasing implantation temperature enhances the growth of bubbles. • Activation energies describing the evolution of the bubble population are obtained. • A He diffusion controlled nucleation through a replacement mechanism is suggested.

  12. A detailed TEM and SEM study of Ni-base alloys oxide scales formed in primary conditions of pressurized water reactor

    International Nuclear Information System (INIS)

    Sennour, Mohamed; Marchetti, Loic; Martin, Frantz; Perrin, Stephane; Molins, Regine; Pijolat, Michele

    2010-01-01

    The oxide film formed on nickel-based alloys in pressurized water reactors (PWR) primary coolant conditions (325 o C, aqueous media) is very thin, in the range of 1-100 nm thick, depending on the surface state and on the corrosion test duration. The nature and the structure of this scale have been investigated by Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM). TEM observations revealed an oxide layer divided in two parts. The internal layer was mainly composed of a continuous spinel layer, identified as a mixed iron and nickel chromite (Ni (1-x) Fe x Cr 2 O 4 ). Moreover, nodules of Cr 2 O 3 , with a size about 5 nm, were present at the interface between this spinel and the alloy. No chromium depletion was observed in the alloy, at the alloy/oxide interface. The external layer is composed of large crystallites corresponding to a spinel structure rich in iron (Ni (1-z) Fe (2+z) O 4 ) resulting from precipitation phenomena. SEM and TEM observations showed a link between the nucleation and/or the growth of crystallites of nickel ferrite and the crystallographic orientation of the substrate. A link between the presence of surface defects and the nucleation of the crystallites was also underlined by SEM observations. Partially hydrated nickel hydroxide, was also observed by TEM in the external scale. Based on these results, some considerations about the mechanism of formation of this oxide layer are discussed.

  13. Electron microscopy study of microbial mat in the North Fiji basin hydrothermal vent

    Science.gov (United States)

    Park, H.; Kim, J. W.; Lee, J. W.

    2017-12-01

    Hydrothermal vent systems consisting of hydrothermal vent, hydrothermal sediment and microbial mat are widely spread around the ocean, particularly spreading axis, continental margin and back-arc basin. Scientists have perceived that the hydrothermal systems, which reflect the primeval earth environment, are one of the best places to reveal the origin of life and extensive biogeochemical process of microbe-mineral interaction. In the present study multiline of analytical methods (X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM)) were utilized to investigate the mineralogy/chemistry of microbe-mineral interaction in hydrothermal microbial mat. Microbial mat samples were recovered by Canadian scientific submersible ROPOS on South Pacific North Fiji basin KIOST hydrothermal vent expedition 1602. XRD analysis showed that red-colored microbial mat contains Fe-oxides and Fe-oxyhydroxides. Various morphologies of minerals in the red-colored microbial mat observed by SEM are mainly showed sheath shaped, resembled with Leptothrix microbial structure, stalks shaped, similar with Marioprofundus microbial structure and globule shaped microbial structures. They are also detected with DNA analysis. The cross sectional observation of microbial structures encrusted with Fe-oxide and Fe-oxyhydroxide at a nano scale by Transmission Electron Microscopy (TEM) and Focused Ion Beam (FIB) technique was developed to verify the structural/biogeochemical properties in the microbe-mineral interaction. Systematic nano-scale measurements on the biomineralization in the microbial mat leads the understandings of biogeochemical environments around the hydrothermal vent.

  14. In Situ TEM Electrical Measurements

    DEFF Research Database (Denmark)

    Canepa, Silvia; Alam, Sardar Bilal; Ngo, Duc-The

    2016-01-01

    understanding of complex physical and chemical interactions in the pursuit to optimize nanostructure function and device performance. Recent developments of sample holder technology for TEM have enabled a new field of research in the study of functional nanomaterials and devices via electrical stimulation...... influence the sample by external stimuli, e.g. through electrical connections, the TEM becomes a powerful laboratory for performing quantitative real time in situ experiments. Such TEM setups enable the characterization of nanostructures and nanodevices under working conditions, thereby providing a deeper...... and measurement of the specimen. Recognizing the benefits of electrical measurements for in situ TEM, many research groups have focused their effort in this field and some of these methods have transferred to ETEM. This chapter will describe recent advances in the in situ TEM investigation of nanostructured...

  15. TEM studies of nanostructure in melt-spun Mg-Ni-La alloy manifesting enhanced hydrogen desorbing kinetics

    International Nuclear Information System (INIS)

    Tanaka, K.; Miwa, T.; Sasaki, K.; Kuroda, K.

    2009-01-01

    The hydrogen storage properties of a magnesium-rich Mg-Ni-La alloy prepared by melt-spinning are significantly improved by nanostructure formation during crystallization and activation. It can absorb and desorb ∼5 wt% hydrogen at temperatures as low as 200 deg. C in moderate time periods. Transmission electron microscopic (TEM) studies on this alloy indicate that the nanostructure, consisting of LaH 3 and Mg 2 NiH 4 nano-particles dispersed homogeneously in MgH 2 matrices after hydrogenation, is rather stable at temperatures below 300 deg. C but undergoes coarsening and segregation of these particles and matrices above ∼400 deg. C. These structural changes have been confirmed by electron energy-loss spectroscopic (EELS) imaging as well as high-resolution TEM techniques. A new EELS peak associated with a plasmon excitation in the MgH 2 phase (H-plasmon) is found for the first time in this study. By imaging the H-plasmon peak, the hydrogen distribution in the alloy has been clearly visualized. We have succeeded in observing the hydrogen desorption process at ∼400 deg. C in-situ in the microscope using this EELS imaging technique.

  16. Biominerals at the nanoscale: transmission electron microscopy methods for studying the special properties of biominerals

    DEFF Research Database (Denmark)

    Posfai, Mihaly; Kasama, Takeshi; Dunin-Borkowski, Rafal E.

    2013-01-01

    Biominerals have important functions in living organisms: apatite crystals are responsible for the strength of our bones and the hardness of our teeth, calcite and aragonite are used by many organisms for making shells, and magnetite and greigite help bacteria and birds to navigate in magnetic...... fields. In order to fulfill their roles in organisms, biominerals have strictly controlled physical and chemical properties. Transmission electron microscopy (TEM) is ideally suited for the study of the structures, arrangements, compositions, morphologies, crystallographic orientations, crystallographic...... minerals that form in the cells of magnetotactic bacteria....

  17. Electron microscopy studies in a high corrosion resistant Ti-Ta-Nb alloy

    International Nuclear Information System (INIS)

    Mythili, R.; Saroja, S.; Vijayalakshmi, M.

    2010-01-01

    Electron microscopy has played an important role in the indigenous development of Ti-5Ta-1.8Nb, an α+β alloy, for reprocessing applications. TEM was used to study the Widmanstatten, martensitic, and the omega phase transformations in the system. A wide spectrum of phase transformations could be introduced into the system, by modifying the composition of the β phase and the cooling rate. PEELS was used to understand the corrosion mechanism, by characterizing the passive film after the corrosion reactions

  18. In-situ Transmission Electron Microscopy and Spectroscopy Studies of Interfaces in Li-ion Batteries: Challenges and Opportunities

    International Nuclear Information System (INIS)

    Wang, Chong M.; Xu, Wu; Liu, Jun; Choi, Daiwon; Arey, Bruce W.; Saraf, Laxmikant V.; Zhang, Jiguang; Yang, Zhenguo; Thevuthasan, Suntharampillai; Baer, Donald R.; Salmon, Norman

    2010-01-01

    The critical challenge facing the lithium ion battery development is the basic understanding of the structural evolution during the cyclic operation of the battery and the consequence of the structural evolution on the properties of the battery. Although transmission electron microscopy (TEM) and spectroscopy have been evolved to a stage such that it can be routinely used to probe into both the structural and chemical composition of the materials with a spatial resolution of a single atomic column, a direct in-situ TEM observation of structural evolution of the materials in lithium ion battery during the dynamic operation of the battery has never been reported. This is related to three factors: high vacuum operation of a TEM; electron transparency requirement of the region to be observed, and the difficulties dealing with the liquid electrolyte of lithium ion battery. In this paper, we report the results of exploring the in-situ TEM techniques for observation of the interface in lithium ion battery during the operation of the battery. A miniature battery was fabricated using a nanowire and an ionic liquid electrolyte. The structure and chemical composition of the interface across the anode and the electrolyte was studied using TEM imaging, electron diffraction, and electron energy loss spectroscopy. In addition, we also explored the possibilities of carrying out in-situ TEM studies of lithium ion batteries with a solid state electrolyte.

  19. Multiple sectioning and perforation techniques for TEM sub-surface studies

    International Nuclear Information System (INIS)

    Lee, E.H.; Rowcliffe, A.F.

    1978-01-01

    Techniques for preparing multiple electron transparent regions at several depth levels below the surface of a metal disk specimen are described. These techniques are relatively rapid and find application in many areas involving surface studies. Examples are shown of multiple thin areas produced at intervals of approximately 200 nm below the original surface of a stainless steel bombarded with 4 MeV Ni +2 ions for void swelling studies

  20. Atomic force microscopy applied to study macromolecular content of embedded biological material

    Energy Technology Data Exchange (ETDEWEB)

    Matsko, Nadejda B. [Electron Microscopy Centre, Institute of Applied Physics, HPM C 15.1, ETH-Hoenggerberg, CH-8093, Zurich (Switzerland)]. E-mail: matsko@iap.phys.ethz.ch

    2007-02-15

    We demonstrate that atomic force microscopy represents a powerful tool for the estimation of structural preservation of biological samples embedded in epoxy resin, in terms of their macromolecular distribution and architecture. The comparison of atomic force microscopy (AFM) and transmission electron microscopy (TEM) images of a biosample (Caenorhabditis elegans) prepared following to different types of freeze-substitution protocols (conventional OsO{sub 4} fixation, epoxy fixation) led to the conclusion that high TEM stainability of the sample results from a low macromolecular density of the cellular matrix. We propose a novel procedure aimed to obtain AFM and TEM images of the same particular organelle, which strongly facilitates AFM image interpretation and reveals new ultrastructural aspects (mainly protein arrangement) of a biosample in addition to TEM data.

  1. Combined TEM and NC-AFM study of Al2O3-supported Pt nanoparticles

    DEFF Research Database (Denmark)

    Jensen, Thomas Nørregaard; Simonsen, Søren Bredmose; Chorkendorff, Ib

    Sintering, the growth of large particles at the expense of smaller ones, is one of the main causes of catalysts deactivation, since the physicochemical properties of a nanoparticle may depend strongly on its size, shape and composition. For application as heterogeneous catalysts, the nanoparticle...... kinks and edges often play an important role for the catalytic activity. In order to preserve these sites, it is important to stabilize the supported nanoparticles with sizes of a few nanometers during operational conditions at often high temperatures and in the relevant gas environments. A prototypical...... nanocatalyst system for studying coarsening consists of Pt nanoparticles supported on an Al2O3 material which is relevant as an oxidation catalyst in diesel and lean-burn engine exhaust after-treatment technologies. In this study we address the effect on sintering of the shape of Pt nanoparticles supported...

  2. SFM-FDTD analysis of triangular-lattice AAA structure: Parametric study of the TEM mode

    Science.gov (United States)

    Hamidi, M.; Chemrouk, C.; Belkhir, A.; Kebci, Z.; Ndao, A.; Lamrous, O.; Baida, F. I.

    2014-05-01

    This theoretical work reports a parametric study of enhanced transmission through annular aperture array (AAA) structure arranged in a triangular lattice. The effect of the incidence angle in addition to the inner and outer radii values on the evolution of the transmission spectra is carried out. To this end, a 3D Finite-Difference Time-Domain code based on the Split Field Method (SFM) is used to calculate the spectral response of the structure for any angle of incidence. In order to work through an orthogonal unit cell which presents the advantage to reduce time and space of computation, special periodic boundary conditions are implemented. This study provides a new modeling of AAA structures useful for producing tunable ultra-compact devices.

  3. Comparing different preparation methods to study human fibrin fibers and platelets using TEM.

    Science.gov (United States)

    Buys, Antoinette V; Pretorius, Etheresia

    2012-06-01

    For the study of cellular ultrastructure, the sample needs to be stabilized by fixation, with the ultimate aim to preserve the native tissue organization and to protect the tissue against later stages of preparation. Chemical and freezing fixation are most used, and chemical fixation employs agents that permeate tissues and cells by diffusion and covalently bind with their major biochemical constituents to fix them. Most widely used chemical fixatives are aldehydes, e.g., formaldehyde and glutaraldehyde, which are noncoagulating, crosslinking agents. Cryofixation methods for ultrastructural studies are also popular, and high-pressure freezing immobilizes all cell constituents and arrests biological activity by removing the thermal energy from the system. In the current research, we used platelet-rich plasma (PRP) to study expansive fibrin fibers and platelet ultrastructure to compare the two fixation techniques. We also used thrombin and calcium chloride as a clotting agent to determine the technique most suitable for the formation of extensive fibrin networks. Chemically fixated fibrin fibers were more compact and condensed and also showed a banding pattern on longitudinal sections. High-pressure frozen samples were more dispersed while platelets fixated showed better preserved cellular membranes and organelle structure. PRP coagulated by addition of CaCl(2) showed blood platelets that are noticeably more activated compared with PRP; however, with thrombin, a sharp ultrastructure was seen. We conclude that PRP mixed with thrombin, and freeze substituted, is the most suitable method for the study of extensive fibrin fibers as well as platelets. Copyright © 2011 Wiley Periodicals, Inc.

  4. In-Situ TEM Study of Interface Sliding and Migration in an Ultrafine Lamellar Structure

    Energy Technology Data Exchange (ETDEWEB)

    Hsiung, L M

    2005-12-06

    The instability of interfaces in an ultrafine TiAl-({gamma})/Ti{sub 3}Al-({alpha}{sub 2}) lamellar structure by straining at room temperature has been investigated using in-situ straining techniques performed in a transmission electron microscope. The purpose of this study is to obtain experimental evidence to support the creep mechanisms based upon the interface sliding in association with a cooperative movement of interfacial dislocations previously proposed to interpret the nearly linear creep behavior observed from ultrafine lamellar TiAl alloys. The results have revealed that both the sliding and migration of lamellar interfaces can take place simultaneously as a result of the cooperative movement of interfacial dislocations.

  5. Electrical sintering of silver nanoparticle ink studied by in-situ TEM probing.

    Directory of Open Access Journals (Sweden)

    Magnus Hummelgård

    Full Text Available Metallic nanoparticle inks are used for printed electronics, but to reach acceptable conductivity the structures need to be sintered, usually using a furnace. Recently, sintering by direct resistive heating has been demonstrated. For a microscopic understanding of this Joule heating sintering method, we studied the entire process in real time inside a transmission electron microscope equipped with a movable electrical probe. We found an onset of Joule heating induced sintering and coalescence of nanoparticles at power levels of 0.1-10 mW/μm³. In addition, a carbonization of the organic shells that stabilize the nanoparticles were found, with a conductivity of 4 10⁵ Sm⁻¹.

  6. Experimental analysis of a TEM plane transmission line for DNA studies at 900 MHz EM fields

    International Nuclear Information System (INIS)

    Belloni, F; Doria, D; Lorusso, A; Nassisi, V; Velardi, L; Alifano, P; Monaco, C; Tala, A; Tredici, M; Raino, A

    2006-01-01

    A suitable plane transmission line was developed and its behaviour analysed at 900 MHz radiofrequency fields to study DNA mutability and the repair of micro-organisms. In this work, utilizing such a device, we investigated the behaviour of DNA mutability and repair of Escherichia coli strains. The transmission line was very simple and versatile in changing its characteristic resistance and field intensity by varying its sizes. In the absence of cell samples inside the transmission line, the relative modulation of the electric and/or magnetic field was ±31% with respect to the mean values, allowing the processing of more samples at different exposure fields in a single run. A slight decrease in spontaneous mutability to rifampicin-resistance of the E. coli JC411 strain was demonstrated in mismatch-repair proficient samples exposed to the radio-frequency fields during their growth on solid medium

  7. Field emission scanning electron microscopy and transmission electron microscopy studies of the chorion, plasma membrane and syncytial layers of the gastrula-stage embryo of the zebrafish Brachydanio rerio : a consideration of the structural and functional relationships with respect to cryoprotectant penetration

    NARCIS (Netherlands)

    Rawson, DM; Zhang, T; Kalicharan, D; Jongebloed, WL

    The structure of the chorion and plasma membranes of gastrula-stage zebrafish Brachydanio rerio embryos were studied using field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). These studies confirm the outer chorion membrane complex to be 1.5-2.5 mu m in

  8. Telemedical support for prehospital Emergency Medical Service (TEMS trial): study protocol for a randomized controlled trial.

    Science.gov (United States)

    Stevanovic, Ana; Beckers, Stefan Kurt; Czaplik, Michael; Bergrath, Sebastian; Coburn, Mark; Brokmann, Jörg Christian; Hilgers, Ralf-Dieter; Rossaint, Rolf

    2017-01-26

    Increasing numbers of emergency calls, shortages of Emergency Medical Service (EMS), physicians, prolonged emergency response times and regionally different quality of treatment by EMS physicians require improvement of this system. Telemedical solutions have been shown to be beneficial in different emergency projects, focused on specific disease patterns. Our previous pilot studies have shown that the implementation of a holistic prehospital EMS teleconsultation system, between paramedics and experienced tele-EMS physicians, is safe and feasible in different emergency situations. We aim to extend the clinical indications for this teleconsultation system. We hypothesize that the use of a tele-EMS physician is noninferior regarding the occurrence of system-induced patient adverse events and superior regarding secondary outcome parameters, such as the quality of guideline-conforming treatment and documentation, when compared to conventional EMS-physician treatment. Three thousand and ten patients will be included in this single-center, open-label, randomized controlled, noninferiority trial with two parallel arms. According to the inclusion criteria, all emergency cases involving adult patients who require EMS-physician treatment, excluding life-threatening cases, will be randomly assigned by the EMS dispatching center into two groups. One thousand five hundred and five patients in the control group will be treated by a conventional EMS physician on scene, and 1505 patients in the intervention group will be treated by paramedics who are concurrently instructed by the tele-EMS physicians at the teleconsultation center. The primary outcome measure will include the rate of treatment-specific adverse events in relation to the kind of EMS physician used. The secondary outcome measures will record the specific treatment-associated quality indicators. The evidence underlines the better quality of service using telemedicine networks between medical personnel and medical

  9. Towards optimization of experimental parameters for studying Li-O2 battery discharge products in TEM using in situ EELS.

    Science.gov (United States)

    Basak, Shibabrata; Jansen, Jacob; Kabiri, Yoones; Zandbergen, Henny W

    2018-05-01

    The key to understanding the performance of Li-O 2 batteries is to study the chemical and structural properties of their discharge product(s) at the nanometer scale. Using TEM for this purpose poses challenges due to the sensitivity of samples to air and electron beams. This paper describes our use of in situ EELS to evaluate experimental procedures to reduce electron-beam degradation and presents methods to deal with air sensitivity. Our results show that Li 2 O 2 decomposition is dependent on the total dose and is approximately 4-5 times more pronounced at 80 than at 200 kV. We also demonstrate the benefits of using low-dose-rate STEM. We show further that a "graphene cell", which encapsulates the sample within graphene sheets, can protect the sample against air and e-beam damage. Copyright © 2018 Elsevier B.V. All rights reserved.

  10. Secondary phases in Al_xCoCrFeNi high-entropy alloys: An in-situ TEM heating study and thermodynamic appraisal

    International Nuclear Information System (INIS)

    Rao, J. C.

    2017-01-01

    Secondary phases, either introduced by alloying or heat treatment, are commonly present in most high-entropy alloys (HEAs). Understanding the formation of secondary phases at high temperatures, and their effect on mechanical properties, is a critical issue that is undertaken in the present paper, using the Al_xCoCrFeNi (x = 0.3, 0.5, and 0.7) as a model alloy. The in-situ transmission-electron-microscopy (TEM) heating observation, an atom-probe-tomography (APT) study for the reference starting materials (Al_0_._3 and Al_0_._5 alloys), and thermodynamic calculations for all three alloys, are performed to investigate (1) the aluminum effect on the secondary-phase fractions, (2) the annealing-twinning formation in the face-centered-cubic (FCC) matrix, (3) the strengthening effect of the secondary ordered body-centered-cubic (B2) phase, and (4) the nucleation path of the σ secondary phase thoroughly. Finally, the present work will substantially optimize the alloy design of HEAs and facilitate applications of HEAs to a wide temperature range.

  11. Surface physics studied by means of scanning tunneling microscopy

    International Nuclear Information System (INIS)

    Besenbacher, F.; Laegsgaard, E.; Stensgaard, I.

    1993-01-01

    Scanning tunneling microscopy has been applied to study silicon crystal structures, oxygen on Cu (110), and real industrial catalyst surfaces. For the latter purpose an Atomic Force Microscope is being developed. (EG)

  12. A study on effects of size and structure on hygroscopicity of nanoparticles using a tandem differential mobility analyzer and TEM

    Energy Technology Data Exchange (ETDEWEB)

    Park, Kihong, E-mail: kpark@gist.ac.kr; Kim, Jae-Seok [Gwangju Institute of Science and Technology (GIST), Research Center for Biomolecular Nanotechnology, Department of Environmental Science and Engineering (Korea, Republic of); Miller, Arthur L. [National Institute for Occupational Safety and Health/Spokane Research Lab (United States)

    2009-01-15

    A hygroscopicity tandem differential mobility analyzer (HTDMA) technique is used to determine size-effect of nanoparticles (NaCl, (NH{sub 4}){sub 2}SO{sub 4}, KCl, NH{sub 4}NO{sub 3}, MgCl{sub 2}, CaCl{sub 2}) on their hygroscopic properties (deliquescence relative humidity (DRH) and hygroscopic growth factor (GF)). The HTDMA system uses a combination of two nano DMAs and two regular DMAs to measure particle size change in a wide dynamic particle size range. Particles are subsequently analyzed with a transmission electron microscopy to investigate the potential effect of particle structure or morphology on the hygroscopic properties. We found that structural properties of NaCl and (NH{sub 4}){sub 2}SO{sub 4} particles also play an important role in determination of the DRH and GF and are more pronounced at smaller diameters. Data show that the DRH of NaCl nanoparticles increased from {approx}75% up to {approx}83% RH at 8 nm and that their GF decreased with decreasing size. The extent to which the GF of NaCl nanoparticles decreased with decreasing size was greater than theoretically predicted with the Kelvin correction. The GF of furnace-generated NaCl nanoparticles that have pores and aggregate shape was found to be smaller than that of atomizer-generated particles that are close to perfectly cubic. For the case of atomizer-generated (NH{sub 4}){sub 2}SO{sub 4} nanoparticles, we observed no significant size-effect on their DRH, and the measured GF agreed well with predicted values using the Kelvin correction. For furnace-generated (NH{sub 4}){sub 2}SO{sub 4} nanoparticles, a gradual growth at moderate RH without noticeable deliquescence behavior occurred. Their TEM images showed that contrary to atomizer-generated (NH{sub 4}){sub 2}SO{sub 4} nanoparticles the furnace-generated (NH{sub 4}){sub 2}SO{sub 4} nanoparticles are not perfectly spherical and are often aggregates having pores and holes, which may favor holding residual water even in the dried condition. For

  13. Efficient reading in standardized tests for EFL learners : a case study of reading strategies used by Chinese English major students in TEM-4

    OpenAIRE

    Xia, Yan

    2011-01-01

    The aim of this study is to investigate the reading strategies used by Chinese English major students in the reading component in standardized national tests of TEM-4 with regard to reading efficiency. The research questions include: 1) what strategies are used by the students in TEM-4 test context; 2) whether there is a significant correlation between strategy use and efficient reading in the test; 3) what kinds of reading problems are revealed in the students’ use of processing strategies; ...

  14. High-speed atomic force microscopy combined with inverted optical microscopy for studying cellular events.

    Science.gov (United States)

    Suzuki, Yuki; Sakai, Nobuaki; Yoshida, Aiko; Uekusa, Yoshitsugu; Yagi, Akira; Imaoka, Yuka; Ito, Shuichi; Karaki, Koichi; Takeyasu, Kunio

    2013-01-01

    A hybrid atomic force microscopy (AFM)-optical fluorescence microscopy is a powerful tool for investigating cellular morphologies and events. However, the slow data acquisition rates of the conventional AFM unit of the hybrid system limit the visualization of structural changes during cellular events. Therefore, high-speed AFM units equipped with an optical/fluorescence detection device have been a long-standing wish. Here we describe the implementation of high-speed AFM coupled with an optical fluorescence microscope. This was accomplished by developing a tip-scanning system, instead of a sample-scanning system, which operates on an inverted optical microscope. This novel device enabled the acquisition of high-speed AFM images of morphological changes in individual cells. Using this instrument, we conducted structural studies of living HeLa and 3T3 fibroblast cell surfaces. The improved time resolution allowed us to image dynamic cellular events.

  15. Merkel-like cell distribution in the epithelium of the human vagina. An immunohistochemical and TEM study.

    Science.gov (United States)

    Polakovičová, Simona; Csöbönyeiová, Mária; Filova, Barbora; Borovský, Miroslav; Maršík, Ladislav; Kvasilová, Alena; Polák, Štefan

    2018-02-16

    Human Merkel cells (MCs) were first described by Friedrich S. Merkel in 1875 and named "Tastzellen" (touch cells). Merkel cells are primarily localized in the basal layer of the epidermis and concentrated in touch-sensitive areas. In our previous work, we reported on the distribution of MCs in the human esophagus, so therefore we chose other parts of the human body to study them. We selected the human vagina, because it has a similar epithelium as the esophagus and plays very important roles in reproduction and sexual pleasure. Due to the fact that there are very few research studies focusing on the innervation of this region, we decided to investigate the occurrence of MCs in the anterior wall of the vagina. The aim of our research was to identify MCs in the stratified squamous non-keratinized epithelium of the human vagina in 20 patients. For the identification of Merkel cells by light microscopy, we used antibodies against simple-epithelial cytokeratins (especially anti-cytokeratin 20). We also tried to identify them using transmission electron microscopy. Our investigation confirmed that 10 (50 %) of 20 patients had increased number of predominantly intraepithelial CK20 positive "Merkel-like" cells (MLCs) in the human vaginal epithelium. Subepithelial CK20 positive MLCs were observed in only one patient (5%). We tried to identify them also using transmission electron microscopy. Our investigation detected some unique cells that may be MCs. The purpose of vaginal innervation is still unclear. There are no data available concerning the distribution of MCs in the human vagina, so it would be interesting to study the role of MCs in the vaginal epithelium, in the context of innervation and epithelial biology.

  16. Dark field X-ray microscopy for studies of recrystallization

    DEFF Research Database (Denmark)

    Ahl, Sonja Rosenlund; Simons, Hugh; Jakobsen, Anders Clemen

    2015-01-01

    We present the recently developed technique of Dark Field X-Ray Microscopy that utilizes the diffraction of hard X-rays from individual grains or subgrains at the (sub)micrometre- scale embedded within mm-sized samples. By magnifying the diffracted signal, 3D mapping of orientations and strains...... external influences. The capabilities of Dark Field X- Ray Microscopy are illustrated by examples from an ongoing study of recrystallization of 50% cold-rolled Al1050 specimens....

  17. Electron microscopy studies of ion implanted silicon

    International Nuclear Information System (INIS)

    Seshan, K.

    1975-11-01

    The nature of defects resulting from the implantation of phosphorous ions into doped silicon and a model of how they form are reported. This involved an electron microscope study of the crystallographic defects (in the 300A size range in concentration of 10 15 /cm 3 ) that form upon annealing. Images formed by these crystallographic defects are complex and that nonconventional imaging techniques are required for their characterization. The images of these small defects (about 300A) are sensitive to various parameters, such as foil thickness, their position in the foil, and diffracting conditions. The defects were found to be mostly interstitial hexagonal Frank loops lying on the four [111] planes and a few perfect interstitial loops; these loops occurred in concentrations of about 10 16 /cm 3 . In addition, ''rod like'' linear defects that are shown to be interstitial are also found in concentrations of 10 13 /cm 3 . It was found that the linear defects require boron for their formation. A model is proposed to account for the interstitial defects. The number of point defects that make up the defects is of the same order as the number of implanted ions. The model predicts that only interstitial loops ought to be observed in agreement with several recent investigations. Dislocation models of the loops are examined and it is shown that phosphorous ions could segregate to the Frank loops, changing their displacement vectors to a/x[111]. (x greater than 3) thus explaining the contrast effects observed. It would also explain the relative electrical inactivity of P + ion implants

  18. TEM Studies of Boron-Modified 17Cr-7Ni Precipitation-Hardenable Stainless Steel via Rapid Solidification Route

    Science.gov (United States)

    Gupta, Ankur; Bhargava, A. K.; Tewari, R.; Tiwari, A. N.

    2013-09-01

    Commercial grade 17Cr-7Ni precipitation-hardenable stainless steel has been modified by adding boron in the range 0.45 to 1.8 wt pct and using the chill block melt-spinning technique of rapid solidification (RS). Application of RS has been found to increase the solid solubility of boron and hardness of 17Cr-7Ni precipitation-hardenable stainless steel. The hardness of the boron-modified rapidly solidified alloys has been found to increase up to ~280 pct after isochronal aging to peak hardness. A TEM study has been carried out to understand the aging behavior. The presence of M23(B,C)6 and M2(B,C) borocarbides and epsilon-carbide in the matrix of austenite and ferrite with a change in heat treatment temperature has been observed. A new equation for Creq is also developed which includes the boron factor on ferrite phase stability. The study also emphasizes that aluminum only takes part in ferrite phase stabilization and remains in the solution.

  19. In situ disordering of monoclinic titanium monoxide Ti5O5 studied by transmission electron microscope TEM.

    Science.gov (United States)

    Rempel, А А; Van Renterghem, W; Valeeva, А А; Verwerft, M; Van den Berghe, S

    2017-09-07

    The superlattice and domain structures exhibited by ordered titanium monoxide Ti 5 O 5 are disrupted by low energy electron beam irradiation. The effect is attributed to the disordering of the oxygen and titanium sublattices. This disordering is caused by the displacement of both oxygen and titanium atoms by the incident electrons and results in a phase transformation of the monoclinic phase Ti 5 O 5 into cubic B1 titanium monoxide. In order to determine the energies required for the displacement of titanium or oxygen atoms, i.e. threshold displacement energies, a systematic study of the disappearance of superstructure reflections with increasing electron energy and electron bombardment dose has been performed in situ in a transmission electron microscope (TEM). An incident electron energy threshold between 120 and 140 keV has been observed. This threshold can be ascribed to the displacements of titanium atoms with 4 as well as with 5 oxygen atoms as nearest neighbors. The displacement threshold energy of titanium atoms in Ti 5 O 5 corresponding with the observed incident electron threshold energy lies between 6.0 and 7.5 eV. This surprisingly low value can be explained by the presence of either one or two vacant oxygen lattice sites in the nearest neighbors of all titanium atoms.

  20. Influence of gas atmospheres and ceria on the stability of nanoporous gold studied by environmental electron microscopy and In situ ptychography

    DEFF Research Database (Denmark)

    Baier, Sina; Wittstock, Arne; Damsgaard, Christian Danvad

    2016-01-01

    A novel complementary approach of electron microscopy/environmental TEM and in situ hard X-ray ptychography was used to study the thermally induced coarsening of nanoporous gold under different atmospheres, pressures and after ceria deposition. The temperature applied during ptychographic imaging...

  1. Study of microstructural evolution in friction-stir welded thin-sheet Al-Cu-Li alloy using transmission-electron microscopy

    International Nuclear Information System (INIS)

    Shukla, A.K.; Baeslack, W.A.

    2007-01-01

    Microstructure evolution in friction-stir welded thin-sheet Al-Cu-Li alloy was studied using transmission-electron microscopy (TEM) and the dissolution and coarsening of T 1 and θ' precipitates were related to the microhardness profile of the weld

  2. Texture evolution and microstructural changes during solid-state dewetting: A correlative study by complementary in situ TEM techniques

    International Nuclear Information System (INIS)

    Niekiel, Florian; Kraschewski, Simon M.; Schweizer, Peter; Butz, Benjamin; Spiecker, Erdmann

    2016-01-01

    The transition of a thin film into an energetically favorable set of particles at temperatures below the melting point of the bulk material is known as solid-state dewetting. In this work the dewetting behavior of 16 nm thick discontinuous Au thin films on amorphous silicon nitride membranes is quantitatively studied by complementary in situ transmission electron microscopy techniques taking advantage of the unique capabilities of a chip-based heating system. The combination of dedicated imaging and diffraction techniques is used to investigate the interplay of grain growth and texture evolution with the process of dewetting. The results show an initial coarsening of the microstructure preceding the other processes. Texture evolution is highly correlated to material retraction and agglomeration during the following dewetting process. In-plane grain rotation has been observed, acting as an additional mechanism for orientation changes. From a methodological perspective this work demonstrates the capabilities of today’s transmission electron microscopy in combination with state-of-the-art in situ instrumentation. In particular the combination of complementary information from different dedicated techniques in one and the same setup is demonstrated to be highly beneficial.

  3. Tem holder for sample transfer under reaction conditions

    DEFF Research Database (Denmark)

    Damsgaard, Christian Danvad; Zandbergen, Henny W.; Wagner, Jakob Birkedal

    Environmental transmission electron microscopy (ETEM) studies are usually performed using conventional sample holders in a dedicated ETEM [1] or in a traditional TEM by use of a dedicated high-pressure cell sample holder [2]. In both cases, the setup defines the conditions regarding gas, pressure......]. Furthermore, dedicated transfer holders have been used to transfer catalyst samples between reactor set-ups and TEM at room temperature in inert atmosphere [5]. To take the full advantage of complementary in situ techniques, transfer under reactions conditions is essential. This study introduces the in situ...... transfer concept by use of a dedicated TEM transfer holder capable of enclosing the sample in a gaseous environment at temperatures up to approx. 900C. By oxidation and reduction experiments of Cu nanoparticles it is shown possible to keep the reaction conditions during transfer outside the microscope...

  4. Preliminary Study of In Vivo Formed Dental Plaque Using Confocal Microscopy and Scanning Electron Microscopy

    Directory of Open Access Journals (Sweden)

    KA. Al-Salihi

    2009-12-01

    Full Text Available Objective: Confocal laser scanning microscopy (CLSM is relatively a new light microscopical imaging technique with a wide range of applications in biological sciences. The primary value of CLSM for the biologist is its ability to provide optical sections from athree-dimensional specimen. The present study was designed to assess the thickness and content of in vivo accumulated dental plaque using CLSM and scanning electron microscopy (SEM.Materials and Methods: Acroflat lower arch splints (acrylic appliance were worn by five participants for three days without any disturbance. The formed plaques were assessed using CLSM combined with vital fluorescence technique and SEM.Results: In this study accumulated dental plaque revealed varied plaque microflora vitality and thickness according to participant’s oral hygiene. The thickness of plaque smears ranged from 40.32 to 140.72 μm and 65.00 to 128.88 μm for live (vital and dead accumulated microorganisms, respectively. Meanwhile, the thickness of plaque on the appliance ranged from 101 μm to 653 μm. CLSM revealed both dead and vital bacteria on the surface of the dental plaque. In addition, SEM revealed layers of various bacterial aggregations in all dental plaques.Conclusion: This study offers a potent non-invasive tool to evaluate and assess the dental plaque biofilm, which is a very important factor in the development of dental caries.

  5. A TEM study of morphological and structural degradation phenomena in LiFePO4-CB cathodes

    DEFF Research Database (Denmark)

    Ngo, Duc-The; Scipioni, Roberto; Simonsen, Søren Bredmose

    2016-01-01

    ) electrolyte are investigated by transmission electron microscopy at various preparation, assembling, storage, and cycling stages. High-resolution transmission electron microscopy imaging shows that continuous SEI layers are formed on the LiFePO4 particles and that both storage and cycling affect the formation...

  6. TEM study of β′ precipitate interaction mechanisms with dislocations and β′ interfaces with the aluminium matrix in Al–Mg–Si alloys

    International Nuclear Information System (INIS)

    Teichmann, Katharina; Marioara, Calin D.; Andersen, Sigmund J.; Marthinsen, Knut

    2013-01-01

    The interaction mechanisms between dislocations and semi-coherent, needle-shaped β′ precipitates in Al–Mg–Si alloys have been studied by High Resolution Transmission Electron Microscopy (HRTEM). Dislocation loops appearing as broad contrast rings around the precipitate cross-sections were identified in the Al matrix. A size dependency of the interaction mechanism was observed; the precipitates were sheared when the longest dimension of their cross-section was shorter than approximately 15 nm, and looped otherwise. A more narrow ring located between the Al matrix and bulk β′ indicates the presence of a transition interface layer. Together with the bulk β′ structure, this was further investigated by High Angle Annular Dark Field Scanning TEM (HAADF-STEM). In the bulk β′ a higher intensity could be correlated with a third of the Si-columns, as predicted from the published structure. The transition layer incorporates Si columns in the same arrangement as in bulk β′, although it is structurally distinct from it. The Z-contrast information and arrangement of these Si-columns demonstrate that they are an extension of the Si-network known to structurally connect all the precipitate phases in the Al–Mg–Si(–Cu) system. The width of the interface layer was estimated to about 1 nm. - Highlights: ► β′ is found to be looped at sizes larger than 15 nm (cross section diameter). ► β′ is found to be sheared at sizes smaller than 15 nm (cross section diameter). ► The recently determined crystal structure of β′ is confirmed by HAADF-STEM. ► Between β′ and the Al-matrix a transition layer of about 1 nm is existent. ► The β′/matrix layer is structurally distinct from bulk β′ and the aluminium matrix.

  7. Discontinuous precipitation in a Ni-In alloy studied by analytical field ion microscopy

    International Nuclear Information System (INIS)

    Geber, G.P.; Kirchheim, R.

    1997-01-01

    Discontinuous precipitation (DP) in a Ni-7.5 at.% In alloy has been studied by means of atom probe field ion microscopy (APFIM). The morphology of the lamellar microstructure and the growth kinetics of the decomposition reaction have been investigated by optical and scanning electron microscopy (LM, SEM). A back polishing method has been developed to prepare APFIM specimens in a systematic manner for transmission electron microscopy (TEM), in order to obtain a definite inclination of different interfaces in the tip apex for subsequent analysis of their chemical composition. APFIM results of the Ni- and In-concentration across the interfaces are presented. Based on the APFIM results it is possible to distinguish between the theoretical description of the concentration profiles given by the models of Cahn and Hillert. It is shown by both FIM images and concentration depth profiles that the α/β-interface has a thickness of about 0.5 nm. In addition it is shown for the first time that the concentration across a β-lamella is not constant. This experimental finding was used to develop a generalization of Cahn's model on discontinuous precipitation including the solute flux within the interface between β and the parent phase α 0

  8. Study of nanoscale structural biology using advanced particle beam microscopy

    Science.gov (United States)

    Boseman, Adam J.

    This work investigates developmental and structural biology at the nanoscale using current advancements in particle beam microscopy. Typically the examination of micro- and nanoscale features is performed using scanning electron microscopy (SEM), but in order to decrease surface charging, and increase resolution, an obscuring conductive layer is applied to the sample surface. As magnification increases, this layer begins to limit the ability to identify nanoscale surface structures. A new technology, Helium Ion Microscopy (HIM), is used to examine uncoated surface structures on the cuticle of wild type and mutant fruit flies. Corneal nanostructures observed with HIM are further investigated by FIB/SEM to provide detailed three dimensional information about internal events occurring during early structural development. These techniques are also used to reconstruct a mosquito germarium in order to characterize unknown events in early oogenesis. Findings from these studies, and many more like them, will soon unravel many of the mysteries surrounding the world of developmental biology.

  9. Head-facial hemangiomas studied with scanning electron microscopy.

    Science.gov (United States)

    Cavallotti, Carlo; Cavallotti, Chiara; Giovannetti, Filippo; Iannetti, Giorgio

    2009-11-01

    Hemangiomas of the head or face are a frequent vascular pathology, consisting in an embryonic dysplasia that involves the cranial-facial vascular network. Hemangiomas show clinical, morphological, developmental, and structural changes during their course. Morphological, structural, ultrastructural, and clinical characteristics of head-facial hemangiomas were studied in 28 patients admitted in our hospital. Nineteen of these patients underwent surgery for the removal of the hemangiomas, whereas 9 patients were not operated on. All the removed tissues were transferred in our laboratories for the morphological staining. Light microscopy, transmission electron microscopy, and scanning electron microscopy techniques were used for the observation of all microanatomical details. All patients were studied for a clinical diagnosis, and many were subjected to surgical therapy. The morphological results revealed numerous microanatomical characteristics of the hemangiomatous vessels. The observation by light microscopy shows the afferent and the efferent vessels for every microhemangioma. All the layers of the arterial wall are uneven. The lumen of the arteriole is entirely used by a blood clot. The observation by transmission electron microscopy shows that it was impossible to see the limits of the different layers (endothelium, medial layer, and adventitia) in the whole wall of the vessels. Moreover, both the muscular and elastic components are disarranged and replaced with connective tissue. The observation by scanning electron microscopy shows that the corrosion cast of the hemangioma offers 3 periods of filling: initially with partial filling of the arteriolar and of the whole cast, intermediate with the entire filling of the whole cast (including arteriole and venule), and a last period with a partial emptying of the arteriolar and whole cast while the venule remains totally injected with resin. Our morphological results can be useful to clinicians for a precise

  10. The structure of spinach Photosystem I studied by electron microscopy

    NARCIS (Netherlands)

    Boekema, Egbert J.; Wynn, R. Max; Malkin, Richard

    1990-01-01

    The structure of three types of Photosystem I (PS I) complex isolated from spinach chloroplasts was studied by electron microscopy and computer image analysis. Molecular projections (top views and side views) of a native PS I complex (PSI-200), an antenna-depleted PS I complex (PSI-100) and the PS I

  11. Phytophthora ramorum tissue colonization studied with fluorescense microscopy

    Science.gov (United States)

    M. Riedel; S. Wagner; M. Gotz; L. Belbahri; F. Lefort; S. Werres

    2009-01-01

    The proceeding worldwide spread and the expanding host spectrum of P. ramorum has become a serious threat to natural plant communities. To encounter this threat detailed knowledge about infection pathways and tissue colonization is essential. To analyze these issues, histological studies of infected tissue with epifluorescence microscopy have been...

  12. Electron microscopy studies on MoS2 nanocrystals

    DEFF Research Database (Denmark)

    Hansen, Lars Pilsgaard

    Industrial-style MoS2-based hydrotreating catalysts are studied using electron microscopy. The MoS2 nanostructures are imaged with single-atom sensitivity to reveal the catalytically important edge structures. Furthermore, the in-situ formation of MoS2 crystals is imaged for the first time....

  13. Nano-structured thin films : a Lorentz transmission electron microscopy and electron holography study

    NARCIS (Netherlands)

    Hosson, J.Th.M. de; Raedt, H.A. De; Zhong, ZY; Saka, H; Kim, TH; Holm, EA; Han, YF; Xie, XS

    2005-01-01

    This paper aims at applying advanced transmission electron microscopy (TEM) to functional materials, such as ultra-soft magnetic films for high-frequency inductors, to reveal the structure-property relationship. The ultimate goal is to delineate a more quantitative way to obtain information of the

  14. Topology and internal structure of PEGylated lipid nanocarriers for neuronal transfection: synchrotron radiation SAXS and cryo-TEM studies

    Czech Academy of Sciences Publication Activity Database

    Angelov, Borislav; Angelova, A.; Filippov, Sergey K.; Karlsson, G.; Terrill, N.; Lesieur, S.; Štěpánek, Petr

    2011-01-01

    Roč. 7, č. 20 (2011), s. 9714-9720 ISSN 1744-683X R&D Projects: GA ČR GA202/09/2078; GA ČR GAP208/10/1600 Institutional research plan: CEZ:AV0Z40500505 Keywords : DNA-lipid-surfactant complexes * CryoTEM * small-angle X-ray scattering Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 4.390, year: 2011

  15. High resolution electron microscopy study of as-prepared and annealed tungsten-carbon multilayers

    International Nuclear Information System (INIS)

    Nguyen, T.D.; Gronsky, R.; Kortright, J.B.

    1988-12-01

    A series of sputtered tungsten-carbon multilayer structures with periods ranging from 2 to 12 nm in the as-prepared state and after annealing at 500/degree/C for 4 hours has been studied with high resolution transmission electron microscopy. The evolution with annealing of the microstructure of these multilayers depends on their period. As-prepared structures appear predominantly amorphous from TEM imaging and diffraction. Annealing results in crystallization of the W-rich layers into WC in the larger period samples, and less complete or no crystallization in the smaller period samples. X-ray scattering reveals that annealing expands the period in a systematic way. The layers remain remarkably well-defined after annealing under these conditions. 12 refs., 4 figs., 1 tab

  16. Microscopic studies on Y2Ba4Cu7O15-δ by use of TEM and NQR techniques

    International Nuclear Information System (INIS)

    Kato, Masaki; Nakanishi, Makoto; Yoshimura, Kazuyoshi; Kosuge, Koji; Miyano, Toshio; Kakihana, Masato

    1998-01-01

    Y 2 Ba 4 Cu 7 O 15-δ compounds were characterized by microscopic investigation using TEM and NQR techniques. The authors synthesized Y247 compounds by two kinds of preparation methods: the conventional solid-state reaction (sample A) and the polymerized-complex method (sample B). The value of T c for sample A was found o be 65 K and that for sample B as 93 K by ac-χ measurements. As a result of TEM experiments, stacking faults along the c axis were observed more frequently in sample B than in sample A. These stacking faults resulted in microdomains containing pure Y123 or Y124 thin blocks of several unit cells. NQR experiments revealed that the microscopic environment of Cu(2) sites in sample A differed from either of those in the Y123 and Y124 compounds. NQR frequency values (ν Q ) of Cu(2) sites agreed well with those calculated by the point charge model applied for the Y247 structure. The spectra of Cu(2) sites in sample B could be regarded, however, as a combination of those of pure Y123, Y124, and also Y247 compounds. This fact was coincident with the result of TEM experiments. The authors concluded that the superconductivity of Y247 with higher T c originates from the thin block of Y123

  17. Structure and chemistry of epitaxial ceria thin films on yttria-stabilized zirconia substrates, studied by high resolution electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Sinclair, Robert, E-mail: bobsinc@stanford.edu [Department of Materials Science and Engineering, Stanford University, Stanford, CA 94305 (United States); Lee, Sang Chul, E-mail: sclee99@stanford.edu [Department of Materials Science and Engineering, Stanford University, Stanford, CA 94305 (United States); Shi, Yezhou; Chueh, William C. [Department of Materials Science and Engineering, Stanford University, Stanford, CA 94305 (United States); Stanford Synchrotron Radiation Lightsource, SLAC National Accelerator Laboratory, Menlo Park, CA 94025 (United States); Stanford Institute for Materials and Energy Sciences, SLAC National Accelerator Laboratory, Menlo Park, CA 94025 (United States)

    2017-05-15

    We have applied aberration-corrected transmission electron microscopy (TEM) imaging and electron energy loss spectroscopy (EELS) to study the structure and chemistry of epitaxial ceria thin films, grown by pulsed laser deposition onto (001) yttria-stabilized zirconia (YSZ) substrates. There are few observable defects apart from the expected mismatch interfacial dislocations and so the films would be expected to have good potential for applications. Under high electron beam dose rate (above about 6000 e{sup -}/Å{sup 2}s) domains of an ordered structure appear and these are interpreted as being created by oxygen vacancy ordering. The ordered structure does not appear at lower lose rates (ca. 2600 e{sup -}/Å{sup 2}s) and can be removed by imaging under 1 mbar oxygen gas in an environmental TEM. EELS confirms that there is both oxygen deficiency and the associated increase in Ce{sup 3+} versus Ce{sup 4+} cations in the ordered domains. In situ high resolution TEM recordings show the formation of the ordered domains as well as atomic migration along the ceria thin film (001) surface. - Highlights: • The local structure and chemistry of ceria can be studied by TEM combined with EELS. • At lower electron, there are no observable changes in the ceria thin films. • At higher dose rates, an ordered phase is created due to oxygen vacancy ordering. • In situ HRTEM shows the oxygen vacancy ordering and the movement of surface atoms.

  18. In Situ TEM Creation of Nanowire Devices

    DEFF Research Database (Denmark)

    Alam, Sardar Bilal

    Integration of silicon nanowires (SiNWs) as active components in devices requires that desired mechanical, thermal and electrical interfaces can be established between the nanoscale geometry of the SiNW and the microscale architecture of the device. In situ transmission electron microscopy (TEM),...

  19. A Washback Study of the "Test for English Majors for Grade Eight" (TEM8) in China--From the Perspective of University Program Administrators

    Science.gov (United States)

    Zou, Shen; Xu, Qian

    2017-01-01

    Washback and fairness are interrelated in validity research, and thus an investigation into washback inevitably involves fairness. This article reports Phase One of a washback study of "Test for English Majors for Grade Eight" (TEM8). Phase One was a questionnaire survey administered to university program administrators. Two research…

  20. NiO/YSZ Reduction for SOFC/SOEC Studied In Situ by Environmental Transmission Electron Microscopy

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose; Agersted, Karsten; Hansen, Karin Vels

    2014-01-01

    SOFCs/SOECs are typically composed of ceramic materials, which are highly complex at the nano-scale. Scanning and transmission electron microscopy (SEM and TEM) are routinely applied for studying these nano-scaled structures post mortem, but only few SOFC/SOEC studies have applied environmental T...... and constant temperature ramping rate of 1°C/min. The NiO observed in the first image at 320°C is dense. From the lower left corner a front of porous Ni is progressing until full reduction at 340°C. [Formula]...

  1. X-ray microscopy and spectromicroscopy - tools for environmental studies

    International Nuclear Information System (INIS)

    Thieme, J.

    2002-01-01

    Full text: X-ray microscopy achieves a much higher resolution than light microscopy. This is due to the much shorter wavelength of X-rays compared to visible light. The smallest structures that can be seen in an X-ray microscope at present are about 20 nm in size. X-ray microscopy is also capable of imaging specimens directly in aqueous media. By choosing the wavelength of the X-radiation appropriately, it is possible to perform spectromicroscopy studies. Comprising, it is a tool very well suited to study colloidal structures in the environment. X-ray microscopy can be performed with two types of instruments. An X-ray microscope quickly takes high-resolution images of objects to be studied, whereas a scanning X-ray microscope is an analytical instrument for spectromicroscopy. Here, an object can be imaged using energies above and below the absorption edge of an element. Dividing both images gives rise to a map of the distribution of this element in the sample. Using near-edge resonances it is possible to conduct NEXAFS studies. As the X-ray energy is raised to match the absorption edge resonances are found, that reflect the chemical bonding state of the element. Therefore, it is possible with X-ray microscopy to combine high spatial resolution with high spectral resolution for studies of colloidal structures. The Institute of X-ray physics builds up an X-ray microscopy beamline at the electron storage ring BESSY II with both, an X-ray microscope and a scanning X-ray microscope. The status of this beamline will be presented in this talk. Colloidal structures play an important role in the environment. Due to their surface activity they are involved in various processes. Substances can be bound and immobilized or transported, colloids can attach to microorganisms building up microhabitats, and organic substances as humics can flocculate due the interaction with metals. A great variety of colloidal structures from the environment have been studied using X

  2. The role of yttrium and titanium during the development of ODS ferritic steels obtained through the STARS route: TEM and XAS study

    Science.gov (United States)

    Ordás, Nerea; Gil, Emma; Cintins, Arturs; de Castro, Vanessa; Leguey, Teresa; Iturriza, Iñigo; Purans, Juris; Anspoks, Andris; Kuzmin, Alexei; Kalinko, Alexandr

    2018-06-01

    Oxide Dispersion Strengthened Ferritic Steels (ODS FS) are candidate materials for structural components in future fusion reactors. Their high strength and creep resistance at elevated temperatures and their good resistance to neutron radiation damage is obtained through extremely fine microstructures containing a high density of nanometric precipitates, generally yttrium and titanium oxides. This work shows transmission electron microscopy (TEM) and extended X-ray absorption fine structure (EXAFS) characterization of Fe-14Cr-2W-0.3Ti-0.24Y ODS FS obtained by the STARS route (Surface Treatment of gas Atomized powder followed by Reactive Synthesis), an alternative method to obtain ODS alloys that avoids the mechanical alloying to introduce Y2O3 powder particles. In this route, FS powders already containing Ti and Y, precursors of the nanometric oxides, are obtained by gas atomization. Then, a metastable Cr- and Fe-rich oxide layer is formed on the surface of the powder particles. During consolidation by HIP at elevated temperatures, and post-HIP heat treatments above the HIP temperature, this oxide layer at Prior Particle Boundaries (PPBs) dissociates, the oxygen diffuses, and Y-Ti-O nano-oxides precipitate in the ferritic matrix. TEM characterization combined with XAFS and XANES analyses have proven to be suitable tools to follow the evolution of the nature of the different oxides present in the material during the whole processing route and select appropriate HIP and post-HIP parameters to promote profuse and fine Y-Ti-O nanometric precipitates.

  3. High-speed atomic force microscopy combined with inverted optical microscopy for studying cellular events.

    OpenAIRE

    Suzuki, Yuki; Sakai, Nobuaki; Yoshida, Aiko; Uekusa, Yoshitsugu; Yagi, Akira; Imaoka, Yuka; Ito, Shuichi; Karaki, Koichi; Takeyasu, Kunio

    2013-01-01

    A hybrid atomic force microscopy (AFM)-optical fluorescence microscopy is a powerful tool for investigating cellular morphologies and events. However, the slow data acquisition rates of the conventional AFM unit of the hybrid system limit the visualization of structural changes during cellular events. Therefore, high-speed AFM units equipped with an optical/fluorescence detection device have been a long-standing wish. Here we describe the implementation of high-speed AFM coupled with an optic...

  4. Study of the niobium dehydrogenation process by transmission electron microscopy

    International Nuclear Information System (INIS)

    Bulhoes, I.A.M.; Akune, K.

    1983-01-01

    The evolution of the micro-structure of Nb-H, during the dehydrogenation process through thermal treatment, has been studied by Transmission Electron Microscopy. The results are used in order to interpret the variation of the line resolution of Electron Channeling Pattern (ECP) of Nb-H as a function of isochronous annealing temperature. It is concluded that the improvement of the ECP line resolution is enhanced of β hydrate in Nb. (Author) [pt

  5. Effects of Piper cubeba L. essential oil on methicillin-resistant Staphylococcus aureus: an AFM and TEM study.

    Science.gov (United States)

    Alharbi, Naiyf S; Khaled, Jamal M; Alzaharni, Khalid E; Mothana, Ramzi A; Alsaid, Mansour S; Alhoshan, Mansour; Dass, Lawrence Arockiasamy; Kadaikunnan, Shine; Alobaidi, Ahmed S

    2017-01-01

    The increasing prevalence of antibiotic-resistant bacteria is creating a real challenge for health care systems worldwide, making the development of novel antibiotics a necessity. In addition to the development of new antibiotics, there is an urgent need for in-depth characterization of the mechanisms of bacterial resistance toward new drugs. Here, we used essential oils extracted in our laboratory from Piper cubeba against methicillin-resistant Staphylococcus aureus ATCC 43300, one of the most prominent antibiotic-resistant bacteria. Effects of the essential oils extracted from P cubeba on bacteria were mainly evaluated using 2 powerful microscopy techniques: atomic force microscopy and transmission electron microscopy. High-resolution atomic force microscopy images of the cells were obtained close to their native environment by immobilizing the cells on porous Polyether sulfone membranes, which were prepared in our laboratory with a wide range and distribution of pore sizes and depth. Inhibition zones (mm) and minimum inhibitory concentrations were determined. Two different concentrations of the oil were used to treat the cells: 50 μg/mL minimum inhibitory concentration and 25 μg/mL. The 50 μg/mL oil solution caused severe damage to the bacterial cells at microscopic levels while the 25 μg/mL solution showed no effects compared to the control. However, at nanoscopic levels, the 25 μg/mL oil solution caused significant changes in the cell wall, which could potentially impair bacterial activities. These results were also confirmed by transmission electron microscopy micrographs. Our results indicate that the extract has a good biological activity against methicillin- and oxacillin-resistant S aureus and that it acts on the cell wall and plasma (cytoplasmic) membrane. Copyright © 2016 John Wiley & Sons, Ltd.

  6. Importance of microscopy in durability studies of solidified and stabilized contaminated soils

    Science.gov (United States)

    Klich, I.; Wilding, L.P.; Drees, L.R.; Landa, E.R.

    1999-01-01

    Solidification/stabilization (S/S) is recognized by the U.S. EPA as a best demonstrated available technology for the containment of contaminated soils and other hazardous wastes that cannot be destroyed by chemical, thermal, or biological means. Despite the increased use of S/S technologies, little research has been conducted on the weathering and degradation of solidified and stabilized wastes once the treated materials have been buried. Published data to verify the performance and durability of landfilled treated wastes over time are rare. In this preliminary study, optical and electron microscopy (scanning electron microscopy [SEM], transmission electron microscopy [TEM] and electron probe microanalyses [EPMA]) were used to evaluate weathering features associated with metal-bearing contaminated soil that had been solidified and stabilized with Portland cement and subsequently buried on site, stored outdoors aboveground, or achieved in a laboratory warehouse for up to 6 yr. Physical and chemical alteration processes identified include: freeze-thaw cracking, cracking caused by the formation of expansive minerals such as ettringite, carbonation, and the movement of metals from waste aggregates into the cement micromass. Although the extent of degradation after 6 yr is considered slight to moderate, results of this study show that the same environmental concerns that affect the durability of concrete must be considered when evaluating the durability and permanence of the solidification and stabilization of contaminated soils with cement. In addition, such evaluations cannot be based on leaching and chemical analyses alone. The use of all levels of microscopic analyses must be incorporated into studies of the long-term performance of S/S technologies.Solidification/stabilization (S/S) is recognized by the U.S. EPA as a best demonstrated available technology for the containment of contaminated soils and other hazardous wastes that cannot be destroyed by chemical

  7. Pathological findings in the lens capsules and intraocular lens in chronic pseudophakic endophthalmitis: an electron microscopy study.

    Science.gov (United States)

    Adán, A; Casaroli-Marano, R P; Gris, O; Navarro, R; Bitrian, E; Pelegrin, L; Sanchez-Dalmau, B

    2008-01-01

    The aim of this study was to describe the pathological findings in lens capsules and intraocular lens (IOL) studied by scanning and/or transmission electron microscopy (SEM and TEM, respectively) in a series of four eyes with chronic pseudophakic endophthalmitis (CPE). We performed a retrospective study of four patients presenting CPE in whom surgical treatment with pars plana vitrectomy, capsulectomy with extraction of the IOL, and intravitreous antibiotic therapy was thereafter performed. The extracted IOL and the capsular remains were studied by SEM and/or TEM and microbiologic analysis of aqueous humour and vitreous aspirate was also carried out in all the cases. The presence of microorganisms was observed in the material analysed in all the cases studied. The use of TEM identified bacterial contamination by Staphylococcus spp and mixed contamination with microorganisms presenting a bacillar morphology suggestive of infection by Propionibacterium acnes in addition to the presence of cocci in the capsular remains. In another two cases, SEM localized colonies of Staphylococcus spp on the surface of the IOL in one case and mixed bacterial colonization with cocci plus filamentous bacteria in the other. The presence of macrophages associated with bacteria was observed in the capsular remains. Microorganisms were found in the IOL or the capsular material in the four cases studied, thereby explaining the refractoriness and severity of infection. The possible presence of polymicrobial infections, especially in the cases with filamentous bacteria, also explains the recurrence of infection.

  8. Super-resolved linear fluorescence localization microscopy using photostable fluorophores: A virtual microscopy study

    Science.gov (United States)

    Birk, Udo; Szczurek, Aleksander; Cremer, Christoph

    2017-12-01

    Current approaches to overcome the conventional limit of the resolution potential of light microscopy (of about 200 nm for visible light), often suffer from non-linear effects, which render the quantification of the image intensities in the reconstructions difficult, and also affect the quantification of the biological structure under investigation. As an attempt to face these difficulties, we discuss a particular method of localization microscopy which is based on photostable fluorescent dyes. The proposed method can potentially be implemented as a fast alternative for quantitative localization microscopy, circumventing the need for the acquisition of thousands of image frames and complex, highly dye-specific imaging buffers. Although the need for calibration remains in order to extract quantitative data (such as the number of emitters), multispectral approaches are largely facilitated due to the much less stringent requirements on imaging buffers. Furthermore, multispectral acquisitions can be readily obtained using commercial instrumentation such as e.g. the conventional confocal laser scanning microscope.

  9. TEM and HRTEM study of oxide particles in an Al-alloyed high-Cr oxide dispersion strengthened ferritic steel with Hf addition

    Energy Technology Data Exchange (ETDEWEB)

    Dou, Peng, E-mail: doup@tsinghua.edu.cn [School of Materials Science and Engineering, Chongqing University, Chongqing 400044 (China); Institute of Advanced Energy, Kyoto University, Gokasho, Uji, Kyoto 611-0011 (Japan); Kimura, Akihiko, E-mail: kimura@iae.kyoto-u.ac.jp [Institute of Advanced Energy, Kyoto University, Gokasho, Uji, Kyoto 611-0011 (Japan); Kasada, Ryuta, E-mail: r-kasada@iae.kyoto-u.ac.jp [Institute of Advanced Energy, Kyoto University, Gokasho, Uji, Kyoto 611-0011 (Japan); Okuda, Takanari, E-mail: okuda.takanari@kki.kobelco.com [Kobelco Research Institute, 1-5-5 Takatsukadai, Nishi-ku, Kobe, Hyogo 651-2271 (Japan); Inoue, Masaki, E-mail: inoue.masaki@jaea.go.jp [Advanced Nuclear System R& D Directorate, Japan Atomic Energy Agency, 4002 Narita, O-arai, Ibaraki 311-1393 (Japan); Ukai, Shigeharu, E-mail: s-ukai@eng.hokudai.ac.jp [Graduate School of Engineering, Hokkaido University, N13, W8, Kita-ku, Sapporo 060-8628 (Japan); Ohnuki, Somei, E-mail: ohnuki@eng.hokudai.ac.jp [Graduate School of Engineering, Hokkaido University, N13, W8, Kita-ku, Sapporo 060-8628 (Japan); Fujisawa, Toshiharu, E-mail: fujisawa@esi.nagoya-u.ac.jp [EcoTopia Science Institute, Nagoya University, Furo, Chikusa-ku, Nagoya 464-8603 (Japan); Abe, Fujio, E-mail: ABE.Fujio@nims.go.jp [Structural Metals Center, National Institute for Materials Science, 1-2-1 Sengen, Tsukuba, Ibaraki 305-0047 (Japan); Jiang, Shan, E-mail: js93518@gmail.com [School of Materials Science and Engineering, Chongqing University, Chongqing 400044 (China); Yang, Zhigang, E-mail: zgyang@tsinghua.edu.cn [Key Laboratory of Advanced Materials (MOE), School of Materials Sciences and Engineering, Tsinghua University, Beijing 100084 (China)

    2017-03-15

    The nanoparticles in an Al-alloyed high-Cr oxide dispersion strengthened (ODS) ferritic steel with Hf addition, i.e., SOC-16 (Fe-15Cr-2W-0.1Ti-4Al-0.62Hf-0.35Y{sub 2}O{sub 3}), have been examined by transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). Relative to an Al-alloyed high-Cr ODS ferritic steel without Hf addition, i.e., SOC-9 (Fe-15.5Cr-2W-0.1Ti-4Al-0.35Y{sub 2}O{sub 3}), the dispersion morphology and coherency of the oxide nanoparticles in SOC-16 were significantly improved. Almost all the small nanoparticles (diameter <10 nm) in SOC-16 were found to be consistent with cubic Y{sub 2}Hf{sub 2}O{sub 7} oxides with the anion-deficient fluorite structure and coherent with the bcc steel matrix. The larger particles (diameter >10 nm) were also mainly identified as cubic Y{sub 2}Hf{sub 2}O{sub 7} oxides with the anion-deficient fluorite structure. The results presented here are compared with those of SOC-9 with a brief discussion of the underlying mechanisms of the unusual thermal and irradiation stabilities of the oxides as well as the superior strength, excellent irradiation tolerance and extraordinary corrosion resistance of SOC-16.

  10. TEM and HRTEM study of oxide particles in an Al-alloyed high-Cr oxide dispersion strengthened ferritic steel with Hf addition

    International Nuclear Information System (INIS)

    Dou, Peng; Kimura, Akihiko; Kasada, Ryuta; Okuda, Takanari; Inoue, Masaki; Ukai, Shigeharu; Ohnuki, Somei; Fujisawa, Toshiharu; Abe, Fujio; Jiang, Shan; Yang, Zhigang

    2017-01-01

    The nanoparticles in an Al-alloyed high-Cr oxide dispersion strengthened (ODS) ferritic steel with Hf addition, i.e., SOC-16 (Fe-15Cr-2W-0.1Ti-4Al-0.62Hf-0.35Y 2 O 3 ), have been examined by transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). Relative to an Al-alloyed high-Cr ODS ferritic steel without Hf addition, i.e., SOC-9 (Fe-15.5Cr-2W-0.1Ti-4Al-0.35Y 2 O 3 ), the dispersion morphology and coherency of the oxide nanoparticles in SOC-16 were significantly improved. Almost all the small nanoparticles (diameter <10 nm) in SOC-16 were found to be consistent with cubic Y 2 Hf 2 O 7 oxides with the anion-deficient fluorite structure and coherent with the bcc steel matrix. The larger particles (diameter >10 nm) were also mainly identified as cubic Y 2 Hf 2 O 7 oxides with the anion-deficient fluorite structure. The results presented here are compared with those of SOC-9 with a brief discussion of the underlying mechanisms of the unusual thermal and irradiation stabilities of the oxides as well as the superior strength, excellent irradiation tolerance and extraordinary corrosion resistance of SOC-16.

  11. A study of internal oxidation in carburized steels by glow discharge optical emission spectroscopy and scanning electron microscopy

    CERN Document Server

    An, X; Rainforth, W M; Chen, L

    2003-01-01

    The internal oxidation of Cr-Mn carburizing steel was studied. Internal oxidation was induced using a commercial carburizing process. Sputter erosion coupled with glow discharge optical emission spectroscopy (GDOES) was used to determine the depth profile elemental distribution within the internal oxidation layer (<10 mu m). In addition, scanning electron microscopy (SEM) equipped with energy dispersive spectrometer (EDS) studies were carried out on selected sputter eroded surfaces. Oxide type was identified primarily by transmission electron microscopy (TEM). The carburized surface was found to consist of a continuous oxide layer, followed by a complex internal oxidation layer, where Cr and Mn oxides were found to populate grain boundaries in a globular form in the near surface region. At greater depths (5-10 mu m), Si oxides formed as a grain boundary network. The internal oxides (mainly complex oxides) grew quickly during the initial stages of the carburizing process (2 h, 800 deg. C+3 h, 930 deg. C). G...

  12. Complete Tem-Tomography: 3D Structure of Gems Cluster

    Science.gov (United States)

    Matsuno, J.; Miyake, A.; Tsuchiyama, A.; Messenger, S.; Nakamura-Messenger, K.

    2015-01-01

    GEMS (glass with embedded metal and sulfide) grains in interplanetary dust particles (IDPs) are considered to be one of the ubiquitous and fundamental building blocks of solids in the Solar System. They have been considered to be interstellar silicate dust that survived various metamorphism or alteration processes in the protoplanetary disk but the elemental and isotopic composition measurements suggest that most of them have been formed in the protoplanetary disk as condensates from high temperature gas. This formation model is also supported by the formation of GEMS-like grains with respect to the size, mineral assemblage, texture and infrared spectrum by condensation experiments from mean GEMS composition materials. Previous GEMS studies were performed only with 2D observation by transmission electron microscopy (TEM) or scanning TEM (STEM). However, the 3D shape and structure of GEMS grains and the spatial distribution of Fe/FeS's has critical information about their formation and origin. Recently, the 3D structure of GEMS grains in ultrathin sections of cluster IDPs was revealed by electron tomography using a TEM/STEM (JEM-2100F, JEOL). However, CT images of thin sections mounted on Cu grids acquired by conventional TEM-tomography are limited to low tilt angles (e. g., less than absolute value of 75 deg. In fact, previous 3D TEM observations of GEMS were affected by some artifacts related to the limited tilt range in the TEM used. Complete tomographic images should be acquired by rotating the sample tilt angle over a range of more than absolute value of 80 deg otherwise the CT images lose their correct structures. In order to constrain the origin and formation process of GEMS grains more clearly, we performed complete electron tomography for GEMS grains. Here we report the sample preparation method we have developed for this study, and the preliminary results.

  13. Mechanisms of CFR composites destruction studying with pulse acoustic microscopy

    Science.gov (United States)

    Petronyuk, Y. S.; Morokov, E. S.; Levin, V. M.; Ryzhova, T. B.; Chernov, A. V.

    2016-05-01

    Non-destructive inspection of carbon-fiber-reinforced (CFR) composites applied in aerospace industry attracts a wide attention. In the paper, high frequency focused ultrasound (50-100 MHz) has been applied to study the bulk microstructure of the CFR material and mechanisms of its destruction under the mechanical loading. It has been shown impulse acoustic microscopy provides detecting the areas of adhesion loss at millimeter and micron level. Behavior of the CFR laminate structure fabricated by prepreg or infusion technology has been investigated under the tensile and impact loading.

  14. A TEM study of D+-implanted Cu following Ar+-ion milling: Microstructure and epitaxial Cu2O formation

    International Nuclear Information System (INIS)

    Johnson, P.B.; Corfiatis, T.; Long, N.J.; Nelson, D.G.A.; Victoria Univ., Wellington; Thomson, R.W.

    1988-01-01

    In examining the microstructure of TEM specimens prepared from D + -implanted Cu for the presence of bubbles it was found that cuprous oxide (Cu 2 O) layers had formed over large areas of the specimen surfaces. The Cu was irradiated at normal incidence with 200 keV D + ions at a temperature of 120 K to a dose of ≅ 2x10 21 D + /m 2 . Ar + ion milling at 330 K was used to erode irradiated surfaces to various depths prior to chemical back-thinning in a jet electropolishing bath. There was no evidence for the formation in the Cu of bubbles of either deuterium or argon, but dislocations at high density and planar defects were evident. Lattice fringes from {110}, {111} and {200} planes in Cu 2 O and moire patterns formed by double diffraction in the Cu and overlaid Cu 2 O film were obvious features in bright-field micrographs. The moire patterns include examples of magnified images of lattice defects. (orig.)

  15. In situ TEM study of G-phase precipitates under heavy ion irradiation in CF8 cast austenitic stainless steel

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Wei-Ying [Argonne National Laboratory, Argonne, IL 60439 (United States); University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States); Li, Meimei; Zhang, Xuan; Kirk, Marquis A.; Baldo, Peter M. [Argonne National Laboratory, Argonne, IL 60439 (United States); Lian, Tiangan [Electric Power Research Institute, Palo Alto, CA 94304 (United States)

    2015-09-15

    Thermally-aged cast austenitic stainless steels (CASS) CF8 was irradiated with 1 MeV Kr ions at 300, 350 and 400 °C to 1.88 × 10{sup 19} ions/m{sup 2} (∼3 dpa) at the IVEM-Tandem Facility at the Argonne National Laboratory. Before irradiation, the distribution of G-phase precipitates in the ferrite showed spatial variations, and both their size and density were affected by the ferrite–austenite phase boundary and presence of M{sub 23}C{sub 6} carbides. Under 300 °C irradiation, in situ TEM observation showed G-phase precipitates were relatively unchanged in the vicinity of the phase boundary M{sub 23}C{sub 6} carbides, while the density of G-phase precipitates increased with increasing dose within the ferrite matrix. Coarsening of G-phase precipitates was observed in the vicinity of phase boundary M{sub 23}C{sub 6} carbides at 350 °C and 400 °C.

  16. In situ TEM study of G-phase precipitates under heavy ion irradiation in CF8 cast austenitic stainless steel

    Science.gov (United States)

    Chen, Wei-Ying; Li, Meimei; Zhang, Xuan; Kirk, Marquis A.; Baldo, Peter M.; Lian, Tiangan

    2015-09-01

    Thermally-aged cast austenitic stainless steels (CASS) CF8 was irradiated with 1 MeV Kr ions at 300, 350 and 400 °C to 1.88 × 1019 ions/m2 (∼3 dpa) at the IVEM-Tandem Facility at the Argonne National Laboratory. Before irradiation, the distribution of G-phase precipitates in the ferrite showed spatial variations, and both their size and density were affected by the ferrite-austenite phase boundary and presence of M23C6 carbides. Under 300 °C irradiation, in situ TEM observation showed G-phase precipitates were relatively unchanged in the vicinity of the phase boundary M23C6 carbides, while the density of G-phase precipitates increased with increasing dose within the ferrite matrix. Coarsening of G-phase precipitates was observed in the vicinity of phase boundary M23C6 carbides at 350 °C and 400 °C.

  17. Powder agglomeration study in RF silane plasmas by in situ polarization-sensitive laser light scattering and TEM measurements

    Energy Technology Data Exchange (ETDEWEB)

    Courteille, C; Hollenstein, C; Dorier, J L; Gay, P; Schwarzenbach, W; Howling, A A [Ecole Polytechnique Federale, Lausanne (Switzerland). Centre de Recherche en Physique des Plasma (CRPP); Bertran, E; Viera, G [Barcelona Univ., Dep. de de Fisica Aplicada I Electronica, Barcelona (Spain); Martins, R; Macarico, A [FCTUNL, Materials Science Dep., Monte de Caparica (Portugal)

    1966-03-01

    To determine self-consistently the time evolution of particle size and their number density in situ multi-angle polarization laser light scattering was used. Cross-polarization intensities (incident and scattered light intensities with opposite polarization) measured at 135{sup o} and ex-situ TEM analysis demonstrate the existence of non-spherical agglomerates during the early phase of agglomeration. Later in the particle time development both techniques reveal spherical particles again. The presence of strong cross-polarization intensities is accompanied by low frequency instabilities detected on the scattered light intensities and plasma emission. It is found that the particle radius and particle number density during the agglomeration phase can be well described by the Brownian Free Molecule Coagulation model. Application of this neutral particle coagulation model is justified by calculation of the particle charge whereby it is shown that particles of a few tens of nanometer can be considered as neutral under our experimental conditions. The measured particle dispersion can be well described by a Brownian Free Molecule Coagulation model including a log-normal particle size distribution. (author) 11 figs., 48 refs.

  18. Powder agglomeration study in RF silane plasmas by in situ polarization-sensitive laser light scattering and TEM measurements

    International Nuclear Information System (INIS)

    Courteille, C.; Hollenstein, C.; Dorier, J.L.; Gay, P.; Schwarzenbach, W.; Howling, A.A.; Bertran, E.; Viera, G.; Martins, R.; Macarico, A.

    1966-03-01

    To determine self-consistently the time evolution of particle size and their number density in situ multi-angle polarization laser light scattering was used. Cross-polarization intensities (incident and scattered light intensities with opposite polarization) measured at 135 o and ex-situ TEM analysis demonstrate the existence of non-spherical agglomerates during the early phase of agglomeration. Later in the particle time development both techniques reveal spherical particles again. The presence of strong cross-polarization intensities is accompanied by low frequency instabilities detected on the scattered light intensities and plasma emission. It is found that the particle radius and particle number density during the agglomeration phase can be well described by the Brownian Free Molecule Coagulation model. Application of this neutral particle coagulation model is justified by calculation of the particle charge whereby it is shown that particles of a few tens of nanometer can be considered as neutral under our experimental conditions. The measured particle dispersion can be well described by a Brownian Free Molecule Coagulation model including a log-normal particle size distribution. (author) 11 figs., 48 refs

  19. Application and development of advanced Lorentz microscopy techniques for the study of magnetic nanostructures

    Science.gov (United States)

    Beacham, Robert J.

    This PhD project presents an investigation into the development of magnetic imaging methods in the TEM and their application in imaging narrow domain walls in multilayer magnetic structures. Lorentz microscopy techniques are limited in quantitative magnetic imaging as this generally requires using scanning imaging modes which limits the capability of imaging dynamic processes. The first imaging method developed in this study is a phase gradient technique with the aim of producing quantitative magnetic contrast proportional to the magnetic induction of the sample whilst maintaining a live imaging mode. This method uses a specifically engineered, semi-electron-transparent graded wedge aperture to controllably perturb intensity in the back focal plane. The results of this study found that this method could produce magnetic contrast proportional to the sample induction, however the required gradient of the wedge aperture made this contrast close to the noise level with large associated errors. In the second part of this study we investigated the development of a technique aimed at gaining sub-microsecond temporal resolution within TEMs based on streak imaging. We are using ramped pulsed magnetic fields, applied across nanowire samples to both induce magnetic behaviour and detect the electron beam across the detector with respect to time. We are coupling this with a novel pixelated detector on the TEM in the form of a Medipix/Timepix chip capable of microsecond exposure times without adding noise. Running this detector in integral mode and allowing for practical limitations such as experiment time and aperture stability, the resultant streak images were taken in Fresnel, Foucault and low angle diffraction imaging modes. We found that while this method is theoretically viable, the limiting factor was the contrast of the magnetic signal in the streak and therefore the total image counts. Domain walls (DWs) in synthetic antiferromagnetically (SAF) coupled films patterned

  20. Stereoscopic methods in TEM

    International Nuclear Information System (INIS)

    Thomas, L.E.

    1975-07-01

    Stereoscopic methods used in TEM are reviewed. The use of stereoscopy to characterize three-dimensional structures observed by TEM has become widespread since the introduction of instruments operating at 1 MV. In its emphasis on whole structures and thick specimens this approach differs significantly from conventional methods of microstructural analysis based on three-dimensional image reconstruction from a number of thin-section views. The great advantage of stereo derives from the ability to directly perceive and measure structures in three-dimensions by capitalizing on the unsurpassed human ability for stereoscopic matching of corresponding details on picture pairs showing the same features from different viewpoints. At this time, stereo methods are aimed mainly at structural understanding at the level of dislocations, precipitates, and irradiation-induced point-defect clusters in crystal and on the cellular irradiation-induced point-defect clusters in crystal and on the cellular level of biological specimens. 3-d reconstruction methods have concentrated on the molecular level where image resolution requirements dictate the use of very thin specimens. One recent application of three-dimensional coordinate measurements is a system developed for analyzing depth variations in the numbers, sizes and total volumes of voids produced near the surfaces of metal specimens during energetic ion bombardment. This system was used to correlate the void volumes at each depth along the ion range with the number of atomic displacements produced at that depth, thereby unfolding the entire swelling versus dose relationship from a single stereo view. A later version of this system incorporating computer-controlled stereo display capabilities is now being built

  1. The application of in situ analytical transmission electron microscopy to the study of preferential intergranular oxidation in Alloy 600

    Energy Technology Data Exchange (ETDEWEB)

    Burke, M.G., E-mail: m.g.burke@manchester.ac.uk; Bertali, G.; Prestat, E.; Scenini, F.; Haigh, S.J.

    2017-05-15

    In situ analytical transmission electron microscopy (TEM) can provide a unique perspective on dynamic reactions in a variety of environments, including liquids and gases. In this study, in situ analytical TEM techniques have been applied to examine the localised oxidation reactions that occur in a Ni-Cr-Fe alloy, Alloy 600, using a gas environmental cell at elevated temperatures. The initial stages of preferential intergranular oxidation, shown to be an important precursor phenomenon for intergranular stress corrosion cracking in pressurized water reactors (PWRs), have been successfully identified using the in situ approach. Furthermore, the detailed observations correspond to the ex situ results obtained from bulk specimens tested in hydrogenated steam and in high temperature PWR primary water. The excellent agreement between the in situ and ex situ oxidation studies demonstrates that this approach can be used to investigate the initial stages of preferential intergranular oxidation relevant to nuclear power systems. - Highlights: • In situ analytical TEM has been performed in 1 bar H{sub 2}-H{sub 2}O vapor at 360–480 °C. • Nanoscale GB migration and solute partitioning correlate with ex situ data for Alloy 600 in H{sub 2}-steam. • This technique can provide new insights into localised reactions associated with localised oxidation.

  2. A TEM based study of the microstructure during room temperature and low temperature hydrogen storage cycling in MgH2 promoted by Nb–V

    International Nuclear Information System (INIS)

    Tan Xuehai; Zahiri, Beniamin; Holt, Chris M.B.; Kubis, Alan; Mitlin, David

    2012-01-01

    Magnesium hydride combined with a new bimetallic Nb–V catalyst displays remarkably rapid and stable low temperature (200 °C) hydrogen storage kinetics, even after 500 full volumetric absorption/desorption cycles. The system is also able to fairly rapidly absorb hydrogen at room temperature at a pressure of 1 bar. This unprecedented absorption behavior was demonstrated for 20 cycles. We employed extensive cryo-stage transmission electron microscopy (TEM) analysis on fully and partially sorbed materials to provide insight into the rapid Mg to MgH 2 phase transformation. After extended cycling of what was initially a 1.5 μm thick fully dense alloy film, the sample structure becomes analogous to that of a weakly agglomerated nanocomposite powder. The cycled Mg–V–Nb structure consists of a dense distribution of catalytic Nb–V nanocrystallites covering the surfaces of larger Mg and MgH 2 particles. The partially absorbed 20 °C and 200 °C microstructures both show this morphology. TEM results combined with Johnson–Mehl–Avrami-type kinetic analysis point to the surface catalyst distribution and stability against coarsening as being a key influence on the two-stage hydriding kinetics. Remarkably, the mean size of the Nb 0.5 V 0.5 H nanocrystallites stays essentially invariant throughout cycling; it is 3 nm after 45 cycles and 4 nm after 500 cycles. A mechanistic description is provided for the cycling-induced microstructural evolution in the ternary alloy as well as in the binary baselines.

  3. Indium hydroxide to oxide decomposition observed in one nanocrystal during in situ transmission electron microscopy studies

    International Nuclear Information System (INIS)

    Miehe, Gerhard; Lauterbach, Stefan; Kleebe, Hans-Joachim; Gurlo, Aleksander

    2013-01-01

    The high-resolution transmission electron microscopy (HR-TEM) is used to study, in situ, spatially resolved decomposition in individual nanocrystals of metal hydroxides and oxyhydroxides. This case study reports on the decomposition of indium hydroxide (c-In(OH) 3 ) to bixbyite-type indium oxide (c-In 2 O 3 ). The electron beam is focused onto a single cube-shaped In(OH) 3 crystal of {100} morphology with ca. 35 nm edge length and a sequence of HR-TEM images was recorded during electron beam irradiation. The frame-by-frame analysis of video sequences allows for the in situ, time-resolved observation of the shape and orientation of the transformed crystals, which in turn enables the evaluation of the kinetics of c-In 2 O 3 crystallization. Supplementary material (video of the transformation) related to this article can be found online at (10.1016/j.jssc.2012.09.022). After irradiation the shape of the parent cube-shaped crystal is preserved, however, its linear dimension (edge) is reduced by the factor 1.20. The corresponding spotted selected area electron diffraction (SAED) pattern representing zone [001] of c-In(OH) 3 is transformed to a diffuse strongly textured ring-like pattern of c-In 2 O 3 that indicates the transformed cube is no longer a single crystal but is disintegrated into individual c-In 2 O 3 domains with the size of about 5–10 nm. The induction time of approximately 15 s is estimated from the time-resolved Fourier transforms. The volume fraction of the transformed phase (c-In 2 O 3 ), calculated from the shrinkage of the parent c-In(OH) 3 crystal in the recorded HR-TEM images, is used as a measure of the kinetics of c-In 2 O 3 crystallization within the framework of Avrami–Erofeev formalism. The Avrami exponent of ∼3 is characteristic for a reaction mechanism with fast nucleation at the beginning of the reaction and subsequent three-dimensional growth of nuclei with a constant growth rate. The structural transformation path in reconstructive

  4. Structure and composition of magnetocaloric Ni-Mn-In-Co thin films on the nanoscale - a TEM study

    Energy Technology Data Exchange (ETDEWEB)

    Erkartal, Burak; Schuermann, Ulrich; Kienle, Lorenz [Institute for Materials Science, Synthesis and Real Structure, Christian Albrechts University, Kiel (Germany); Duppel, Viola [Nanochemistry Max Planck Institute for Solid State Research, Stuttgart (Germany); Niemann, Robert; Schultz, Ludwig; Faehler, Sebastian [IFW Dresden (Germany)

    2012-08-15

    A complementary set of electron microscopy techniques is applied for the determination of structural and chemical segregation phenomena within a 300 nm thick metamagnetic Ni-Mn-In-Co thin film. The structure is predominantly composed of distinct modulated martensites of the 5M-, 6M-, 7M-, and 8M-type. Additionally these modulated structures exhibit twinning and stacking disordering. The nature of the disordering and the structural misfit at the twin interface were analyzed via high resolution micrographs. Next to an adhesion layer of Cr interdiffusion on the nanoscale was observed producing a penternary chemically and structurally homogeneous precipitate. The structure can be assigned to a twinned non-modulated pseudocubic model. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  5. A study of internal oxidation in carburized steels by glow discharge optical emission spectroscopy and scanning electron microscopy

    International Nuclear Information System (INIS)

    An, X; Cawley, J.; Rainforth, W.M.; Chen, L.

    2003-01-01

    The internal oxidation of Cr-Mn carburizing steel was studied. Internal oxidation was induced using a commercial carburizing process. Sputter erosion coupled with glow discharge optical emission spectroscopy (GDOES) was used to determine the depth profile elemental distribution within the internal oxidation layer (<10 μm). In addition, scanning electron microscopy (SEM) equipped with energy dispersive spectrometer (EDS) studies were carried out on selected sputter eroded surfaces. Oxide type was identified primarily by transmission electron microscopy (TEM). The carburized surface was found to consist of a continuous oxide layer, followed by a complex internal oxidation layer, where Cr and Mn oxides were found to populate grain boundaries in a globular form in the near surface region. At greater depths (5-10 μm), Si oxides formed as a grain boundary network. The internal oxides (mainly complex oxides) grew quickly during the initial stages of the carburizing process (2 h, 800 deg. C+3 h, 930 deg. C). GDOES proved to be an excellent tool for the quantification of oxidation and element distribution as a function of depth, particularly when combined with SEM and TEM to identify oxide type and morphology

  6. Transmission Electron Microscopy Studies on Titanium-doped Sodium Aluminum Hydride

    Science.gov (United States)

    Culnane, Lance F.

    Hydrogen fuel cells play an important role in today's diverse and blossoming alternative energy industry. One of the greatest technological barriers for vehicular applications is the storage of hydrogen (which is required to power hydrogen fuel cells). Storing hydrogen as a gas is not volume efficient, and storing it as a liquid is not cost effective, therefore solid-state storage of hydrogen, such as in metal hydrides offers the most potential for success since many metal hydrides have attractive qualities for hydrogen storage such as: high volumetric capacity, cost efficiency, weight efficiency, low refueling times, and most importantly, high safety. Unfortunately, a compound has not been discovered which contains all of the attractive hydrogen storage qualities for vehicular applications. Sodium aluminum hydride (NaAlH 4) is one of the few compounds which is close to meeting requirements for car manufacturers, and has perhaps been researched the most extensively out of all metal hydrides in the last 15 years. This arises from the remarkable discovery by Bogdanovic who found that doping NaAlH4 with Ti dopants enabled the reversible dehydrogenation and hydrogenation of NaAlH 4 at mild conditions. Various evidence and theories have been proposed to suggest explanations for the enhanced kinetic effect that Ti-doping and ball-milling provide. However, the research community has not reached a consensus as to the exact role of Ti-dopants. If the role of titanium in the NaAlH4 dehydrogenation/hydrogenation mechanism could be understood, then more attractive metal hydrides could be designed. To this end, we conducted Transmission Electron Microscopy (TEM) studies to explain the role of the Ti dopants. The first known thorough particle size analysis of the NaAlH4 system was conducted, as well as TEM-EELS (Electron Energy Loss Spectroscopy), TEM-EDS (Energy Dispersive X-ray Spectroscopy), and in-situ imaging studies. Preparation methods were found to be important for the

  7. Indium hydroxide to oxide decomposition observed in one nanocrystal during in situ transmission electron microscopy studies

    Science.gov (United States)

    Miehe, Gerhard; Lauterbach, Stefan; Kleebe, Hans-Joachim; Gurlo, Aleksander

    2013-02-01

    The high-resolution transmission electron microscopy (HR-TEM) is used to study, in situ, spatially resolved decomposition in individual nanocrystals of metal hydroxides and oxyhydroxides. This case study reports on the decomposition of indium hydroxide (c-In(OH)3) to bixbyite-type indium oxide (c-In2O3). The electron beam is focused onto a single cube-shaped In(OH)3 crystal of {100} morphology with ca. 35 nm edge length and a sequence of HR-TEM images was recorded during electron beam irradiation. The frame-by-frame analysis of video sequences allows for the in situ, time-resolved observation of the shape and orientation of the transformed crystals, which in turn enables the evaluation of the kinetics of c-In2O3 crystallization. Supplementary material (video of the transformation) related to this article can be found online at 10.1016/j.jssc.2012.09.022. After irradiation the shape of the parent cube-shaped crystal is preserved, however, its linear dimension (edge) is reduced by the factor 1.20. The corresponding spotted selected area electron diffraction (SAED) pattern representing zone [001] of c-In(OH)3 is transformed to a diffuse strongly textured ring-like pattern of c-In2O3 that indicates the transformed cube is no longer a single crystal but is disintegrated into individual c-In2O3 domains with the size of about 5-10 nm. The induction time of approximately 15 s is estimated from the time-resolved Fourier transforms. The volume fraction of the transformed phase (c-In2O3), calculated from the shrinkage of the parent c-In(OH)3 crystal in the recorded HR-TEM images, is used as a measure of the kinetics of c-In2O3 crystallization within the framework of Avrami-Erofeev formalism. The Avrami exponent of ˜3 is characteristic for a reaction mechanism with fast nucleation at the beginning of the reaction and subsequent three-dimensional growth of nuclei with a constant growth rate. The structural transformation path in reconstructive decomposition of c-In(OH)3 to c

  8. Combining in situ transmission electron microscopy irradiation experiments with cluster dynamics modeling to study nanoscale defect agglomeration in structural metals

    International Nuclear Information System (INIS)

    Xu Donghua; Wirth, Brian D.; Li Meimei; Kirk, Marquis A.

    2012-01-01

    We present a combinatorial approach that integrates state-of-the-art transmission electron microscopy (TEM) in situ irradiation experiments and high-performance computing techniques to study irradiation defect dynamics in metals. Here, we have studied the evolution of visible defect clusters in nanometer-thick molybdenum foils under 1 MeV krypton ion irradiation at 80 °C through both cluster dynamics modeling and in situ TEM experiments. The experimental details are reported elsewhere; we focus here on the details of model construction and comparing the model with the experiments. The model incorporates continuous production of point defects and/or small clusters, and the accompanying interactions, which include clustering, recombination and loss to the surfaces that result from the diffusion of the mobile defects. To account for the strong surface effect in thin TEM foils, the model includes one-dimensional spatial dependence along the foil depth, and explicitly treats the surfaces as black sinks. The rich amount of data (cluster number density and size distribution at a variety of foil thickness, irradiation dose and dose rate) offered by the advanced in situ experiments has allowed close comparisons with computer modeling and permitted significant validation and optimization of the model in terms of both physical model construct (damage production mode, identities of mobile defects) and parameterization (diffusivities of mobile defects). The optimized model exhibits good qualitative and quantitative agreement with the in situ TEM experiments. The combinatorial approach is expected to bring a unique opportunity for the study of radiation damage in structural materials.

  9. Protein–nanoparticle interaction in bioconjugated silver nanoparticles: A transmission electron microscopy and surface enhanced Raman spectroscopy study

    Energy Technology Data Exchange (ETDEWEB)

    Reymond-Laruinaz, Sébastien; Saviot, Lucien; Potin, Valérie; Marco de Lucas, María del Carmen, E-mail: delucas@u-bourgogne.fr

    2016-12-15

    Highlights: • Synthesis of protein-conjugated Ag nanoparticles (NPs) in absence of citrates. • NPs size and protein layer thickness determined by TEM. • SERS spectra showed the chemisorption of proteins on the surface of Ag-NPs. - Abstract: Understanding the mechanisms of interaction between proteins and noble metal nanoparticles (NPs) is crucial to extend the use of NPs in biological applications and nanomedicine. We report the synthesis of Ag-NPs:protein bioconjugates synthesized in total absence of citrates or other stabilizing agents in order to study the NP-protein interaction. Four common proteins (lysozyme, bovine serum albumin, cytochrome-C and hemoglobin) were used in this work. Transmission electron microscopy (TEM) and surface enhanced Raman spectroscopy (SERS) were mainly used to study these bioconjugated NPs. TEM images showed Ag NPs with sizes in the 5–40 nm range. The presence of a protein layer surrounding the Ag NPs was also observed by TEM. Moreover, the composition at different points of single bioconjugated NPs was probed by electron energy loss spectroscopy (EELS). The thickness of the protein layer varies in the 3–15 nm range and the Ag NPs are a few nanometers away. This allowed to obtain an enhancement of the Raman signal of the proteins in the analysis of water suspensions of bioconjugates. SERS results showed a broadening of the Raman bands of the proteins which we attribute to the contribution of different configurations of the proteins adsorbed on the Ag NPs surface. Moreover, the assignment of an intense and sharp peak in the low-frequency range to Ag–N vibrations points to the chemisorption of the proteins on the Ag-NPs surface.

  10. Protein–nanoparticle interaction in bioconjugated silver nanoparticles: A transmission electron microscopy and surface enhanced Raman spectroscopy study

    International Nuclear Information System (INIS)

    Reymond-Laruinaz, Sébastien; Saviot, Lucien; Potin, Valérie; Marco de Lucas, María del Carmen

    2016-01-01

    Highlights: • Synthesis of protein-conjugated Ag nanoparticles (NPs) in absence of citrates. • NPs size and protein layer thickness determined by TEM. • SERS spectra showed the chemisorption of proteins on the surface of Ag-NPs. - Abstract: Understanding the mechanisms of interaction between proteins and noble metal nanoparticles (NPs) is crucial to extend the use of NPs in biological applications and nanomedicine. We report the synthesis of Ag-NPs:protein bioconjugates synthesized in total absence of citrates or other stabilizing agents in order to study the NP-protein interaction. Four common proteins (lysozyme, bovine serum albumin, cytochrome-C and hemoglobin) were used in this work. Transmission electron microscopy (TEM) and surface enhanced Raman spectroscopy (SERS) were mainly used to study these bioconjugated NPs. TEM images showed Ag NPs with sizes in the 5–40 nm range. The presence of a protein layer surrounding the Ag NPs was also observed by TEM. Moreover, the composition at different points of single bioconjugated NPs was probed by electron energy loss spectroscopy (EELS). The thickness of the protein layer varies in the 3–15 nm range and the Ag NPs are a few nanometers away. This allowed to obtain an enhancement of the Raman signal of the proteins in the analysis of water suspensions of bioconjugates. SERS results showed a broadening of the Raman bands of the proteins which we attribute to the contribution of different configurations of the proteins adsorbed on the Ag NPs surface. Moreover, the assignment of an intense and sharp peak in the low-frequency range to Ag–N vibrations points to the chemisorption of the proteins on the Ag-NPs surface.

  11. In-situ study of cascade defects in silver by simultaneous transmission electron microscopy and electrical resistivity measurements at low temperatures

    International Nuclear Information System (INIS)

    Haga, K.; King, W.E.; Merkle, K.L.; Meshii, M.

    1985-12-01

    A helium-cooled double-tilt specimen stage for transmission electron microscopy (TEM) with the capability of simultaneous electrical resistivity measurements was constructed and used to study defect-production, migration, clustering and recovery processes in ion-irradiated silver. Vacuum-evaporated thin film specimens were irradiated with 1 MeV Kr + -ions up to a dose of 4.0 x 10 10 ions/cm 2 , at T = 10 0 K in the microscope, using the HVEM-tandem accelerator ion beam interface system in the Argonne National Laboratory Electron Microscopy Center. Cascade defect formation during ion bombardment at the low temperature was directly observed both by TEM and electrical resistivity measurements. Ion bombardment created groups of defect clusters with strong strain fields which gave rise to TEM contrast. The specimen resistivity was increased by 16% during the irradiation. Subsequent microstructural changes and resistivity recovery during isochronal annealing were monitored up to room temperature. 58.3% of the irradiation induced resistivity was recovered, while significant reduction in the size of black spot defect clusters was observed by TEM. A small fraction of clusters disappeared, while no nucleation of new defect clusters was observed

  12. Multifrequency scanning probe microscopy study of nanodiamond agglomerates

    Science.gov (United States)

    Aravind, Vasudeva; Lippold, Stephen; Li, Qian; Strelcov, Evgheny; Okatan, Baris; Legum, Benjamin; Kalinin, Sergei; Clarion University Team; Oak Ridge National Laboratory Team

    Due to their rich surface chemistry and excellent mechanical properties and non-toxic nature, nanodiamond particles have found applications such as biomedicine, tribology and lubrication, targeted drug delivery systems, tissue scaffolds and surgical implants. Although single nanodiamond particles have diameters about 4-5nm, they tend to form agglomerates. While these agglomerates can be useful for some purposes, many applications of nanodiamonds require single particle, disaggregated nanodiamonds. This work is oriented towards studying forces and interactions that contribute to agglomeration in nanodiamonds. In this work, using multifrequency scanning probe microscopy techniques, we show that agglomerate sizes can vary between 50-100nm in raw nanodiamonds. Extremeties of particles and Interfaces between agglomerates show dissipative forces with scanning probe microscope tip, indicating agglomerates could act as points of increased adhesion, thus reducing lubricating efficiency when nanodiamonds are used as lubricant additives. This research was conducted at the Center for Nanophase Materials Sciences, which is a DOE Office of Science User Facility.

  13. Scanning tunneling microscopy and spectroscopy studies of graphite edges

    International Nuclear Information System (INIS)

    Niimi, Y.; Matsui, T.; Kambara, H.; Tagami, K.; Tsukada, M.; Fukuyama, Hiroshi

    2005-01-01

    We studied experimentally and theoretically the electronic local density of states (LDOS) near single-step edges at the surface of exfoliated graphite. In scanning tunneling microscopy measurements, we observed the (3x3)R30 o and honeycomb superstructures extending over 3-4-bar nm both from the zigzag and armchair edges. Calculations based on a density-functional-derived non-orthogonal tight-binding model show that these superstructures can coexist if the two types of edges admix each other in real graphite step edges. Scanning tunneling spectroscopy measurements near the zigzag edge reveal a clear peak in the LDOS at an energy below the Fermi energy by 20-bar meV. No such a peak was observed near the armchair edge. We concluded that this peak corresponds to the 'edge state' theoretically predicted for graphene ribbons, since a similar prominent LDOS peak due to the edge state is obtained by the first principles calculations

  14. The scanning probe microscopy study of thin polymer films

    International Nuclear Information System (INIS)

    Harron, H.R.

    1995-08-01

    Scanning Tunnelling Microscopy and Atomic Force Microscopy were used systematically to investigate the morphology, uniformity, coverage and structure of the thin films of several commercially important insulating polymers. Despite the poorly conducting nature of the polymer sample, detailed and convincing images of this class of materials were achieved by STM without the need to coat the samples with a conductive layer. The polymer regions of the sample were further investigated by the use of surface profiling with 'line scans'. The fluctuations of the amplitude therein enabled important film characteristics to be assessed. An environmental stage was designed for the STM to enable the effect of various vapour-sample interactions to be observed during the imaging process. Using the data from the environmental stage in addition to the surface profiling with line scans, an insight into the conduction mechanism and image interpretation was gained. Results suggest that the water content of the sample and its immediate surroundings is an important factor in achieving reliable STM images in air. The initial study culminated with the observation by STM alone of the plasticizer induced crystallization of uncoated PC thin films. The 'amorphous' PC films were observed before crystallization and small ordered regions in roughly the same proportion as that predicted by diffraction studies [Prietschk, 1959 and Schnell, 1964] were imaged. This has never been observed by a microscopy technique. Furthermore, images of the crystalline film contained elongated units that were attributed to the lamellae formations that form the basic building blocks of polymer spherulites. The study continued with the AFM imaging of the growth of crystalline entities in a PC film, without the need for harsh sample treatment or metal coating. A method of casting and crystallizing the films was developed such that the growth was predominantly in two dimensions and consequently ideal for observation by

  15. TEM Imaging of Mass-selected Polymer Molecules

    International Nuclear Information System (INIS)

    Nasibulin, Albert G.; Kauppinen, Esko I.; Thomson, Bruce A.; Fernandez de la Mora, J.

    2002-01-01

    Polyethylene glycol (PEG) molecules with masses below 1300 amu are electrosprayed (ES) from solution, mobility-selected at high resolution in a differential mobility analyzer (DMA), collected on a grid and imaged by transmission electron microscopy (ES-DMA-TEM). The DMA resolves individual n-mers, and selects only one out of the many present in the original sample. Ion identity is established from parallel mass spectra (ES-MS). The images reveal spherical particles 1.46 nm in diameter, in good agreement with the known ion mass and bulk density. The DMA-selection technique opens new paths for the study of very small particles

  16. Corneal endothelium in xeroderma pigmentosum: clinical specular microscopy study.

    Science.gov (United States)

    Mohamed, Ashik; Peguda, Rajini; Ramappa, Muralidhar; Ali, Mohammad Javed; Chaurasia, Sunita

    2016-06-01

    Xeroderma pigmentosum is a condition caused due to a defective DNA repair mechanism when exposed to ultraviolet radiation. Many of the patients with this disorder develop severely oedematous cornea with varying degrees of anterior corneal haze, which necessitates a full-thickness keratoplasty or selective endothelial keratoplasty. Presence of corneal oedema suggests that these patients have a dysfunctional endothelium. The purpose of this study is to evaluate the corneal endothelium in the patients with xeroderma pigmentosum when clinical specular microscopy was feasible. Thirteen patients with classic skin changes of xeroderma pigmentosum were included in the study conducted during January 2010-December 2012. An age-matched group of 13 volunteers were included as controls who were emmetropes without any history of ocular or systemic illness. Corneal endothelium was assessed using specular microscopy from the central clear area of cornea. The mean age of the patients with xeroderma pigmentosum was 16.6±7.2 years and that of the controls was 17.4±6.9 years (p=0.78). The number of analysed cells and endothelial cell density were significantly higher in controls (pxeroderma pigmentosum (p≤0.007). The specular microscopic findings in patients with xeroderma pigmentosum are suggestive of an accelerated endothelial cell loss. It is pertinent that the treating physicians must be involved in emphasising proper ocular protection from ultraviolet radiation to prevent avoidable blindness from xeroderma pigmentosum. Published by the BMJ Publishing Group Limited. For permission to use (where not already granted under a licence) please go to http://www.bmj.com/company/products-services/rights-and-licensing/

  17. Electron microscopy study of advanced heterostructures for optoelectronics

    NARCIS (Netherlands)

    Katcki, J.; Ratajczak, J.; Phillipp, F.; Muszalski, J.; Bugajski, M.; Chen, J.X.; Fiore, A.

    2003-01-01

    The application of cross-sectional transmission electron microscopy and SEM to the investigation of optoelectronic devices are reviewed. Special attention was paid to the electron microscopy assessment of the growth perfection of such crucial elements of the devices like quantum wells, quantum dots,

  18. 40 keV atomic resolution TEM

    International Nuclear Information System (INIS)

    Bell, David C.; Russo, Christopher J.; Kolmykov, Dmitry V.

    2012-01-01

    Here we present the first atomic resolution TEM imaging at 40 keV using an aberration-corrected, monochromated source TEM. Low-voltage High-Resolution Electron Microscopy (LVHREM) has several advantages, including increased cross-sections for inelastic and elastic scattering, increased contrast per electron and improved spectroscopy efficiency, decreased delocalization effects and reduced knock-on damage. Together, these often improve the contrast to damage ratio obtained on a large class of samples. Third-order aberration correction now allows us to operate the TEM at low energies while retaining atomic resolution, which was previously impossible. At low voltage the major limitation to resolution becomes the chromatic aberration limit. We show that using a source monochromator we are able to reduce the effect of chromatic aberration and achieve a usable high-resolution limit at 40 keV to less than 1 Å. We show various materials' examples of the application of the technique to image graphene and silicon, and compare atomic resolution images with electron multislice simulations. -- Highlights: ► We present the first atomic resolution images recorded at 40 keV using an aberration-corrected, monochromated TEM. ► We show information transfer measured to better than 1 Å. ► At 40 keV an aberration-corrected monochromated TEM is limited by fifth-order spherical aberration. ► We show that using a monochromator the effect of chromatic aberration is reduced to enable high resolution imaging. ► Low voltage high resolution electron microscopy will be beneficial for imaging the organic/inorganic materials interface.

  19. Scanning tunneling microscopy studies of glucose oxidase on gold surface

    International Nuclear Information System (INIS)

    Losic, D.; Shapter, J.G.; Gooding, J.J.

    2002-01-01

    Full text: Three immobilization methods have been used for scanning tunneling microscopy (STM) studies of glucose oxidase (GOD) on gold. They are based on a) physical adsorption from solution, b) microcontact printing and c) covalent bonding onto self-assembled monolayers (SAM) of 3-mercaptopropionic acid (MPA). The STM images are used to provide information about the organization of individual GOD molecules and more densely packed monolayers of GOD on electrode surfaces, thus providing information of the role of interfacial structure on biosensor performance. The use of atomically flat gold substrates enables easy distinction of deposited enzyme features from the flat gold substrate. Microcontact printing is found to be a more reliable method than adsorption from solution for preparing individual GOD molecules on the gold surface STM images of printed samples reveal two different shapes of native GOD molecules. One is a butterfly shape with dimensions of 10 ± 1 nm x 6 ± 1 nm, assigned to the lying position of molecule while the second is an approximately spherical shape with dimensions of 6.5 ± 1 nm x 5 ± 1nm assigned to a standing position. Isolated clusters of 5 to 6 GOD molecules are also observed. With monolayer coverage, GOD molecules exhibit a tendency to organize themselves into a two dimensional array with adequate sample stability to obtain high-resolution STM images. Within these two-dimensional arrays are clearly seen repeating clusters of five to six enzyme molecules in a unit STM imaging of GOD monolayers covalently immobilized onto SAM (MPA) are considerably more difficult than when the enzyme is adsorbed directly onto the metal. Cluster structures are observed both high and low coverage despite the fact that native GOD is a negatively charged molecule. Copyright (2002) Australian Society for Electron Microscopy Inc

  20. Multimodal microscopy of immune cells and melanoma for longitudinal studies

    Science.gov (United States)

    Entenberg, David; Aranda, Iana; Li, Yongbiao; Toledo-Crow, Ricardo; Schaer, David; Li, Yanyun

    2006-02-01

    Intravital microscopy of cancer is a well established tool that provides direct visualization of the tumor cycle. It traditionally involves one of several strategies: invasive subcutaneous (SC) implantation of tumors followed by surgical opening of skin flaps for imaging, techniques utilizing skin fold chambers and implanted optical windows or intradermal injections under 200μm from the skin surface. All of these techniques allow the use of fluorescent proteins as markers for biologically significant constituents. However, observation methods utilizing skin-flaps, skin-fold chambers and optical windows are invasive and tend to alter the immune environment of the tissue and/or limit the duration of studies that can be performed. If implanted correctly, intradermally injected tumors can be minimally invasive, will not require biopsies or surgical intervention to observe and are accessible for direct transdermal imaging with a number of in vivo modalities. We present our work in the development of a small animal intravital microscopy workstation that allows the acquisition of different contrast imaging modalities: reflectance confocal, wide field epifluorescence, multiphoton and second harmonic generation (SHG). The images are acquired pair-wise simultaneously and sequentially in time. The aim of our instrumentation is to gather all information generated by the single probing beam via the reflected or back-scattered signal, SHG signal and various fluorescence signals. Additionally, we also present our development of a microscopic tissue navigation technique to mark, label and track sites of interest. This technique enables us to revisit sites periodically and record, with different imaging contrasts, their biological changes over time.

  1. A New Approach to Studying Biological and Soft Materials Using Focused Ion Beam Scanning Electron Microscopy (FIB SEM)

    International Nuclear Information System (INIS)

    Stokes, D J; Morrissey, F; Lich, B H

    2006-01-01

    Over the last decade techniques such as confocal light microscopy, in combination with fluorescent labelling, have helped biologists and life scientists to study biological architectures at tissue and cell level in great detail. Meanwhile, obtaining information at very small length scales is possible with the combination of sample preparation techniques and transmission electron microscopy (TEM) or scanning transmission electron microscopy (STEM). Scanning electron microscopy (SEM) is well known for the determination of surface characteristics and morphology. However, the desire to understand the three dimensional relationships of meso-scale hierarchies has led to the development of advanced microscopy techniques, to give a further complementary approach. A focused ion beam (FIB) can be used as a nano-scalpel and hence allows us to reveal internal microstructure in a site-specific manner. Whilst FIB instruments have been used to study and verify the three-dimensional architecture of man made materials, SEM and FIB technologies have now been brought together in a single instrument representing a powerful combination for the study of biological specimens and soft materials. We demonstrate the use of FIB SEM to study three-dimensional relationships for a range of length scales and materials, from small-scale cellular structures to the larger scale interactions between biomedical materials and tissues. FIB cutting of heterogeneous mixtures of hard and soft materials, resulting in a uniform cross-section, has proved to be of particular value since classical preparation methods tend to introduce artefacts. Furthermore, by appropriate selection, we can sequentially cross-section to create a series of 'slices' at specific intervals. 3D reconstruction software can then be used to volume-render information from the 2D slices, enabling us to immediately see the spatial relationships between microstructural components

  2. Global gyrokinetic simulations of TEM microturbulence

    Science.gov (United States)

    Vernay, T.; Brunner, S.; Villard, L.; McMillan, B. F.; Jolliet, S.; Bottino, A.; Görler, T.; Jenko, F.

    2013-07-01

    Global gyrokinetic simulations of electrostatic temperature-gradient-driven trapped-electron-mode (TEM) turbulence using the δf particle-in-cell code ORB5 are presented. The electron response is either fully kinetic or hybrid, i.e. considering kinetic trapped and adiabatic passing electrons. A linear benchmark in the TEM regime against the Eulerian-based code GENE is presented. Two different methods for controlling the numerical noise, based, respectively, on a Krook operator and a so-called coarse-graining approach, are discussed and successfully compared. Both linear and non-linear studies are carried out for addressing the issue of finite-ρ*-effects and finite electron collisionality on TEM turbulence. Electron collisions are found to damp TEMs through the detrapping process, while finite-ρ*-effects turn out to be important in the non-linear regime but very small in the linear regime. Finally, the effects of zonal flows on TEM turbulence are briefly considered as well and shown to be unimportant in the temperature-gradient-driven TEM regime. Consistently, basically no difference is found between linear and non-linear critical electron temperature gradients in the TEM regime.

  3. Anisotropic structures of some microorganisms studied by polarization microscopy

    Czech Academy of Sciences Publication Activity Database

    Žižka, Zdeněk

    2014-01-01

    Roč. 59, č. 5 (2014), s. 363-368 ISSN 0015-5632 Institutional support: RVO:61388971 Keywords : Polarization microscopy * microorganism Subject RIV: EE - Microbiology, Virology Impact factor: 1.000, year: 2014

  4. Mössbauer, XRD and TEM Study on the Intercalation and the Release of Drugs in/from Layered Double Hydroxides

    Directory of Open Access Journals (Sweden)

    E. Kuzmann

    2015-12-01

    Full Text Available Layered double hydroxides (LDHs are one of the very important nano-carriers for drug delivery, due to their many advantageous features, such as the ease and low-cost of preparation, low cytotoxicity, good biocompatibility, protection for the intercalated drugs, and the capacity to facilitate the uptake of the loaded drug in the cells. In our previous studies, Mössbauer spectroscopy was applied to monitor structural changes occurring during the incorporation of Fe(III in MgFe- and CaFe-LDHs, and the intercalation of various organic compounds in anionic form. Recently, we have successfully elaborated a protocol for the intercalation and release of indol-2-carboxylate and L-cysteinate in CaFe-LDH. The corresponding structural changes in the LDH samples were studied by XRD, HR-TEM and 57Fe Mössbauer spectroscopy. The Mössbauer spectra reflected small but significant changes upon both the intercalation and the release of drugs. The changes in the basal distances could be followed by XRD measurements, and HR-TEM images made these changes visible.

  5. Suspended DNA structural characterization by TEM diffraction

    KAUST Repository

    Marini, Monica

    2017-12-01

    In this work, micro-fabrication, super-hydrophobic properties and a physiologically compatible preparation step are combined and tailored to obtain background free biological samples to be investigated by Transmission Electron Microscopy (TEM) diffraction technique. The validation was performed evaluating a well-known parameter such as the DNA interbases value. The diffraction spacing measured is in good agreement with those obtained by HRTEM direct metrology and by traditional X-Ray diffraction. This approach addresses single molecule studies in a simplified and reproducible straightforward way with respect to more conventional and widely used techniques. In addition, it overcomes the need of long and elaborated samples preparations: the sample is in its physiological environment and the HRTEM data acquisition occurs without any background interference, coating, staining or additional manipulation. The congruence in the results reported in this paper makes the application of this approach extremely promising towards those molecules for which crystallization remains a hurdle, such as cell membrane proteins and fibrillar proteins.

  6. Suspended DNA structural characterization by TEM diffraction

    KAUST Repository

    Marini, Monica; Allione, Marco; Lopatin, Sergei; Moretti, Manola; Giugni, Andrea; Torre, Bruno; Di Fabrizio, Enzo M.

    2017-01-01

    In this work, micro-fabrication, super-hydrophobic properties and a physiologically compatible preparation step are combined and tailored to obtain background free biological samples to be investigated by Transmission Electron Microscopy (TEM) diffraction technique. The validation was performed evaluating a well-known parameter such as the DNA interbases value. The diffraction spacing measured is in good agreement with those obtained by HRTEM direct metrology and by traditional X-Ray diffraction. This approach addresses single molecule studies in a simplified and reproducible straightforward way with respect to more conventional and widely used techniques. In addition, it overcomes the need of long and elaborated samples preparations: the sample is in its physiological environment and the HRTEM data acquisition occurs without any background interference, coating, staining or additional manipulation. The congruence in the results reported in this paper makes the application of this approach extremely promising towards those molecules for which crystallization remains a hurdle, such as cell membrane proteins and fibrillar proteins.

  7. Detecting single-electron events in TEM using low-cost electronics and a silicon strip sensor.

    Science.gov (United States)

    Gontard, Lionel C; Moldovan, Grigore; Carmona-Galán, Ricardo; Lin, Chao; Kirkland, Angus I

    2014-04-01

    There is great interest in developing novel position-sensitive direct detectors for transmission electron microscopy (TEM) that do not rely in the conversion of electrons into photons. Direct imaging improves contrast and efficiency and allows the operation of the microscope at lower energies and at lower doses without loss in resolution, which is especially important for studying soft materials and biological samples. We investigate the feasibility of employing a silicon strip detector as an imaging detector for TEM. This device, routinely used in high-energy particle physics, can detect small variations in electric current associated with the impact of a single charged particle. The main advantages of using this type of sensor for direct imaging in TEM are its intrinsic radiation hardness and large detection area. Here, we detail design, simulation, fabrication and tests in a TEM of the front-end electronics developed using low-cost discrete components and discuss the limitations and applications of this technology for TEM.

  8. Micro-Scale Characteristics of Insoluble Organic Matter in Chondrites: A Coordinated TEM, STXM and SIMS Study

    Science.gov (United States)

    Nittler, L. R.; Alexander, C. M. O'd.; Cody, G. D.; de Gregorio, B. T.; Kilcoyne, A. L. D.; Stroud, R. M.; Tiwari, A.

    2009-03-01

    A coordinated study of meteoritic insoluble organic matter reveals that hollow organic globules are chemically similar to other IOM, but abundances and sizes of globules vary between meteorites. IOM is sensitive to electron and X-ray induced beam damage.

  9. MAE measurements and studies of magnetic domains by electron microscopy

    International Nuclear Information System (INIS)

    Lo, C.C.H.

    1998-01-01

    There is a pressing need for non-destructive testing (NDT) methods for monitoring steel microstructures as they determine the mechanical properties of steel products. Magnetoacoustic emission (MAE) has potential for this application since it is sensitive to steel microstructure. The aim of this project is to study systematically the dependence of MAE upon steel microstructure, and to apply the technique to examine the industrial steel components which have complicated microstructures. Studies of MAE and Barkhausen emission (BE) were made on several systems including fully pearlitic, fully ferritic, ferritic/pearlitic and spheroidized steels. Results suggest that there is a correlation between the microstructural parameters and the MAE and BE profiles. The study of fully pearlitic steel shows that both MAE and BE are sensitive to the interlamellar spacing of pearlite. Low-carbon ferritic steel samples give different MAE and BE profiles which are dependent on ferrite grain size. Lorentz microscopy reveals that there are differences in domain structures and magnetization processes between fully ferritic and fully pearlitic samples. Study of ferritic/pearlitic samples indicates that both MAE and BE depend on the ferrite content. In the case of spheroidized steel samples MAE and BE profiles were found to be sensitive to the changes in the morphology and size of carbides. Samples of industrial steel products including pearlitic rail steel and decarburized billet were investigated. The MAE profiles obtained from the rail are consistent with those measured from the fully pearlitic rod samples. This suggests that MAE can be used for monitoring the microstructure of large steel components, provided that another technique such as BE is also used to complement the MAE measurements. In the study of the billet samples, MAE and BE were found to be dependent on the decarburization depth. The results are discussed in the context of the change in ferrite content of the surface layer

  10. Fluorescent ligands for studying neuropeptide receptors by confocal microscopy

    Directory of Open Access Journals (Sweden)

    A. Beaudet

    1998-11-01

    Full Text Available This paper reviews the use of confocal microscopy as it pertains to the identification of G-protein coupled receptors and the study of their dynamic properties in cell cultures and in mammalian brain following their tagging with specific fluorescent ligands. Principles that should guide the choice of suitable ligands and fluorophores are discussed. Examples are provided from the work carried out in the authors' laboratory using custom synthetized fluoresceinylated or BODIPY-tagged bioactive peptides. The results show that confocal microscopic detection of specifically bound fluorescent ligands permits high resolution appraisal of neuropeptide receptor distribution both in cell culture and in brain sections. Within the framework of time course experiments, it also allows for a dynamic assessment of the internalization and subsequent intracellular trafficking of bound fluorescent molecules. Thus, it was found that neurotensin, somatostatin and mu- and delta-selective opioid peptides are internalized in a receptor-dependent fashion and according to receptor-specific patterns into their target cells. In the case of neurotensin, this internalization process was found to be clathrin-mediated, to proceed through classical endosomal pathways and, in neurons, to result in a mobilization of newly formed endosomes from neural processes to nerve cell bodies and from the periphery of cell bodies towards the perinuclear zone. These mechanisms are likely to play an important role for ligand inactivation, receptor regulation and perhaps also transmembrane signaling.

  11. Morphology and chemical characteristics of micro- and Nano-particles in the haze in Beijing studied by XPS and TEM/EDX

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Peng [Beijing Key Laboratory for Green Catalysis and Separation, Key Laboratory of Beijing on Regional Air Pollution Control, Key Laboratory of Advanced Functional Materials, Education Ministry of China, and Laboratory of Catalysis Chemistry and Nanoscience, Department of Chemistry and Chemical Engineering, College of Environmental and Energy Engineering, Beijing University of Technology, Beijing 100124 (China); CAS Key Laboratory of Standardization and Measurement for Nanotechnology, National Center for Nanoscience and Technology, Beijing, 100190 (China); Xu, Jianxun; He, Meng [CAS Key Laboratory of Standardization and Measurement for Nanotechnology, National Center for Nanoscience and Technology, Beijing, 100190 (China); Song, Lexin [Department of Chemistry, University of Science and Technology of China, Hefei, 230026 (China); Chen, Dongliang, E-mail: chendl@mail.buct.edu.cn [College of Mechanical and Electrical Engineering, Beijing University of Chemical Technology, Beijing 100029 (China); Guo, Guangsheng, E-mail: guogs@bjut.edu.cn [Beijing Key Laboratory for Green Catalysis and Separation, Key Laboratory of Beijing on Regional Air Pollution Control, Key Laboratory of Advanced Functional Materials, Education Ministry of China, and Laboratory of Catalysis Chemistry and Nanoscience, Department of Chemistry and Chemical Engineering, College of Environmental and Energy Engineering, Beijing University of Technology, Beijing 100124 (China); Dai, Hongxing, E-mail: hxdai@bjut.edu.cn [Beijing Key Laboratory for Green Catalysis and Separation, Key Laboratory of Beijing on Regional Air Pollution Control, Key Laboratory of Advanced Functional Materials, Education Ministry of China, and Laboratory of Catalysis Chemistry and Nanoscience, Department of Chemistry and Chemical Engineering, College of Environmental and Energy Engineering, Beijing University of Technology, Beijing 100124 (China)

    2016-09-15

    X-ray Photoelectron Spectroscopy (XPS) is a useful surface sensitive tool to explore the particulate matter with different particle sizes. In this work, we report the analysis of elemental species in particulate matter with size ranging from 100 nm to 10 μm during the autumn haze of 2014 in Beijing. The size dependence of element composition and chemical state distribution on the particle surface was investigated. It was found that the number of investigated element species decreased from 8 (at stage 2) to 4 (at stage 10) with the decrease of particle sizes down to 100 nm, which is in accordance with the result from Transmission electron microscopy (TEM/EDX) observations. Three chemical states of nitrogen, the amide group (399.9 eV), the ammonium group (401.6 eV), and the nitrate group (407.2 eV), were confirmed according to the different binding energies. Nitrate was the main composition on the coarse particles, while the percentage of amide and ammonium at stage 3 (13.9% and 10.8% respectively) increased on the fine particles at stage 9 (46.8% and 38.8% respectively). The relative ratio of sulfate and ammonium (calculated 1:1) in the fine particles suggests that there is no enough NH{sub 4}{sup +} to neutralize the sulfuric acid and the surface of the PM is acidic. The result is useful to investigate the generation processes and the sources of collected particles. - Highlights: • The element composition of particles from 100 nm to 10 μm in haze was discussed • The chemical state was dominated by the particle size • The surface of PM was acidity • XPS was shown a useful tool in the aerosol research.

  12. Comparative study on the effects of two antifungal drugs against Candida albicans by microcalorimetry and transmission electron microscopy

    International Nuclear Information System (INIS)

    Guo, Qing-Lian; Zhang, Juan; Xu, Zi-Qiang; Li, Ran; Jiang, Feng-Lei; Xiao, Qi; Liu, Yi

    2012-01-01

    Highlights: ► Microcalorimetry is a fast, simple method to study the antibiotic property of drugs. ► We noticed that the antibiotic effect of ITZ was slightly better than that of KTZ. ► We perform the TEM to study the morphology changes of C. albicans cells. - Abstract: In this work, a multi-channel thermal activity monitor (TAM 2277) was applied to study the growth metabolism of Candida albicans (C. albicans) in vitro in the absence and presence of different concentrations of ketoconazole (KTZ) and itraconazole (ITZ). The results showed that the half inhibiting concentrations (IC 50 ) of C. albicans by KTZ and ITZ are 73.5 and 66.3 μmol L −1 , respectively. So the antibiotic effect of ITZ was slightly better than that of KTZ. The morphology of C. albicans cells both in the absence and presence of antifungal agents was examined by transmission electron microscopy (TEM). Our research also suggests that microcalorimetry is a fast, simple, non-invasive, non-destructive and more sensitive method, and can be easily performed to study the antibiotic property of different species of drugs on microorganism compared to other biological and clinical methods.

  13. Comparative study on the effects of two antifungal drugs against Candida albicans by microcalorimetry and transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Guo, Qing-Lian [Zhongnan Hospital, Wuhan University, Wuhan 430071 (China); Zhang, Juan [Zhongnan Hospital, Wuhan University, Wuhan 430071 (China); Department of Stomatology, Hubei Provincial Maternal and Child Health Hospital, Wuhan 430070 (China); Xu, Zi-Qiang; Li, Ran [State Key Laboratory of Virology and Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072 (China); Jiang, Feng-Lei, E-mail: fljiang@whu.edu.cn [State Key Laboratory of Virology and Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072 (China); Xiao, Qi, E-mail: qi.xiao@whu.edu.cn [College of Chemistry and Life Science, Guangxi Teachers Education University, Nanning 530001 (China); Liu, Yi [State Key Laboratory of Virology and Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072 (China)

    2012-09-10

    Highlights: Black-Right-Pointing-Pointer Microcalorimetry is a fast, simple method to study the antibiotic property of drugs. Black-Right-Pointing-Pointer We noticed that the antibiotic effect of ITZ was slightly better than that of KTZ. Black-Right-Pointing-Pointer We perform the TEM to study the morphology changes of C. albicans cells. - Abstract: In this work, a multi-channel thermal activity monitor (TAM 2277) was applied to study the growth metabolism of Candida albicans (C. albicans) in vitro in the absence and presence of different concentrations of ketoconazole (KTZ) and itraconazole (ITZ). The results showed that the half inhibiting concentrations (IC{sub 50}) of C. albicans by KTZ and ITZ are 73.5 and 66.3 {mu}mol L{sup -1}, respectively. So the antibiotic effect of ITZ was slightly better than that of KTZ. The morphology of C. albicans cells both in the absence and presence of antifungal agents was examined by transmission electron microscopy (TEM). Our research also suggests that microcalorimetry is a fast, simple, non-invasive, non-destructive and more sensitive method, and can be easily performed to study the antibiotic property of different species of drugs on microorganism compared to other biological and clinical methods.

  14. In-situ TEM study on structural change and light emission of a multiwall carbon nanotube during Joule heating

    Science.gov (United States)

    Nishikawa, K.; Asaka, K.; Nakahara, H.; Saito, Y.

    2018-01-01

    Structure changes of a multiwall carbon nanotube (MWNT) during Joule heating were studied with simultaneous measurement of light emission spectra. The outer shells of the MWNT peeled off one by one because of excessive heating. All the peeled outer shells finally disappeared and inner shells whose tips were closed emerged, i.e., a new MWNT was formed. Each diameter of the shells comprising the MWNT decreased compared with those before the fracture. Light emission spectra during Joule heating of an MWNT were composed of both the blackbody radiation and characteristic peaks. The peaks in the light emission spectra shifted to higher energies in accordance with shrinkage of the inner shells. The energies of the peaks in the spectra corresponded to energy gaps between van Hove singularities calculated from the diameters of the shells, indicating that the peaks in the spectra are attributed to the interband electron transition in the MWNT.

  15. Super-resolution microscopy in studying neuroendocrine cell function

    Directory of Open Access Journals (Sweden)

    Anneka eBost

    2013-11-01

    Full Text Available The last two decades have seen a tremendous development in high resolution microscopy techniques giving rise to acronyms such as TIRFM, SIM, PALM, STORM, and STED. The goal of all these techniques is to overcome the physical resolution barrier of light microscopy in order to resolve precise protein localization and possibly their interaction in cells. Neuroendocrine cell function is to secrete hormones and peptides on demand. This fine-tuned multi-step process is mediated by a large array of proteins. Here, we review the new microscopy techniques used to obtain high resolution and how they have been applied to increase our knowledge of the molecular mechanisms involved in neuroendocrine cell secretion. Further the limitations of these methods are discussed and insights in possible new applications are provided.

  16. In situ transmission electron microscopy for magnetic nanostructures

    DEFF Research Database (Denmark)

    Ngo, Duc-The; Kuhn, Luise Theil

    2016-01-01

    Nanomagnetism is a subject of great interest because of both application and fundamental aspects in which understanding of the physical and electromagnetic structure of magnetic nanostructures is essential to explore the magnetic properties. Transmission electron microscopy (TEM) is a powerful tool...... that allows understanding of both physical structure and micromagnetic structure of the thin samples at nanoscale. Among TEM techniques, in situ TEM is the state-of-the-art approach for imaging such structures in dynamic experiments, reconstructing a real-time nanoscale picture of the properties......-structure correlation. This paper aims at reviewing and discussing in situ TEM magnetic imaging studies, including Lorentz microscopy and electron holography in TEM, applied to the research of magnetic nanostructures....

  17. A nonlinear filtering algorithm for denoising HR(S)TEM micrographs

    International Nuclear Information System (INIS)

    Du, Hongchu

    2015-01-01

    Noise reduction of micrographs is often an essential task in high resolution (scanning) transmission electron microscopy (HR(S)TEM) either for a higher visual quality or for a more accurate quantification. Since HR(S)TEM studies are often aimed at resolving periodic atomistic columns and their non-periodic deviation at defects, it is important to develop a noise reduction algorithm that can simultaneously handle both periodic and non-periodic features properly. In this work, a nonlinear filtering algorithm is developed based on widely used techniques of low-pass filter and Wiener filter, which can efficiently reduce noise without noticeable artifacts even in HR(S)TEM micrographs with contrast of variation of background and defects. The developed nonlinear filtering algorithm is particularly suitable for quantitative electron microscopy, and is also of great interest for beam sensitive samples, in situ analyses, and atomic resolution EFTEM. - Highlights: • A nonlinear filtering algorithm for denoising HR(S)TEM images is developed. • It can simultaneously handle both periodic and non-periodic features properly. • It is particularly suitable for quantitative electron microscopy. • It is of great interest for beam sensitive samples, in situ analyses, and atomic resolution EFTEM

  18. Microbial biofilm study by synchrotron X-ray microscopy

    International Nuclear Information System (INIS)

    Pennafirme, S.; Lima, I.; Bitencourt, J.A.; Crapez, M.A.C.; Lopes, R.T.

    2015-01-01

    Microbial biofilm has already being used to remove metals and other pollutants from wastewater. In this sense, our proposal was to isolate and cultivate bacteria consortia from mangrove’s sediment resistant to Zn (II) and Cu (II) at 50 mg L −1 and to observe, through synchrotron X-ray fluorescence microscopy (microXRF), whether the biofilm sequestered the metal. The biofilm area analyzed was 1 mm 2 and a 2D map was generated (pixel size 20×20 μm 2 , counting time 5 s/point). The biofilm formation and retention followed the sequence Zn>Cu. Bacterial consortium zinc resistant formed dense biofilm and retained 63.83% of zinc, while the bacterial consortium copper resistant retained 3.21% of copper, with lower biofilm formation. Dehydrogenase activity of Zn resistant bacterial consortium was not negatively affect by 50 mg ml −1 zinc input, whereas copper resistant bacterial consortium showed a significant decrease on dehydrogenase activity (50 mg mL −1 of Cu input). In conclusion, biofilm may protect bacterial cells, acting as barrier against metal toxicity. The bacterial consortia Zn resistant, composed by Nitratireductor spp. and Pseudomonas spp formed dense biofilm and sequestered metal from water, decreasing the metal bioavailability. These bacterial consortia can be used in bioreactors and in bioremediation programs. - Highlights: • We studied bacterial bioremediation by microXRF. • Dense biofilm may act sequestering metal while protecting bacterial metabolism. • Nitratireductor spp. and Pseudomonas spp decreased seawater metal bioavailability. • Bacterial consortia from polluted areas may be used in bioremediation programs.

  19. Study of Hydrated Lime in Environmental Scanning Electron Microscopy

    Czech Academy of Sciences Publication Activity Database

    Tihlaříková, Eva; Neděla, Vilém; Rovnaníková, P.

    2013-01-01

    Roč. 19, S2 (2013), s. 1644-1645 ISSN 1431-9276 R&D Projects: GA ČR GAP102/10/1410; GA MŠk ED0017/01/01 Institutional support: RVO:68081731 Keywords : Hydrated Lime * Environmental Scanning Electron Microscopy Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering Impact factor: 1.757, year: 2013

  20. Effects of Topography in Nano-Structured Thin Films : A Lorentz Transmission Electron Microscopy and Electron Holography Study

    NARCIS (Netherlands)

    Hosson, Jeff Th.M. De; Raedt, Hans A. De

    2003-01-01

    This paper aims at applying advanced transmission electron microscopy (TEM) to functional materials, such as ultra-soft magnetic films for high-frequency inductors, to reveal the structure-property relationship. The ultimate goal is to delineate a more quantitative way to obtain information of the

  1. Electron microscopy in metallurgy

    International Nuclear Information System (INIS)

    Loretto, M.H.

    1980-01-01

    The aim of this paper is to review briefly the contribution which (TEM) transmission electron microscopy (including high voltage electron microscopy (HVEM)) has made to metallurgy. Since it is straightforward with modern electron microscopes to extract the crystallographic information which provides the basis for any interpretation, the major problem in most metallurgical work lies in assessing how the structure (which TEM has characterised) has arisen and which properties of the specimen can be understood in terms of this structure. Radiation damage, quenching, phase transformations, grain boundaries and plastic deformation have been the main fields in which TEM has contributed significantly. After briefly summarising the role of TEM in each field, examples of recent work will be used to indicate current TEM activity in physical metallurgy. (author)

  2. In situ electron microscopy studies of electromechanical behavior in metals at the nanoscale using a novel microdevice-based system

    Energy Technology Data Exchange (ETDEWEB)

    Kang, Wonmo, E-mail: wonmo.kang.ctr.ks@nrl.navy.mil; Beniam, Iyoel; Qidwai, Siddiq M. [Naval Research Laboratory, Washington, DC 20375 (United States)

    2016-09-15

    Electrically assisted deformation (EAD) is an emerging technique to enhance formability of metals by applying an electric current through them. Despite its increasing importance in manufacturing applications, there is still an unresolved debate on the nature of the fundamental deformation mechanisms underlying EAD, mainly between electroplasticity (non-thermal effects) and resistive heating (thermal effects). This status is due to two critical challenges: (1) a lack of experimental techniques to directly observe fundamental mechanisms of material deformation during EAD, and (2) intrinsic coupling between electric current and Joule heating giving rise to unwanted thermally activated mechanisms. To overcome these challenges, we have developed a microdevice-based electromechanical testing system (MEMTS) to characterize nanoscale metal specimens in transmission electron microscopy (TEM). Our studies reveal that MEMTS eliminates the effect of Joule heating on material deformation, a critical advantage over macroscopic experiments, owing to its unique scale. For example, a negligible change in temperature (<0.02 °C) is predicted at ∼3500 A/mm{sup 2}. Utilizing the attractive features of MEMTS, we have directly investigated potential electron-dislocation interactions in single crystal copper (SCC) specimens that are simultaneously subjected to uniaxial loading and electric current density up to 5000 A/mm{sup 2}. Our in situ TEM studies indicate that for SCC, electroplasticity does not play a key role as no differences in dislocation activities, such as depinning and movement, are observed.

  3. Radiation defects in Te-implanted germanium. Electron microscopy and computer simulation studies

    International Nuclear Information System (INIS)

    Kalitzova, M.G.; Karpuzov, D.S.; Pashov, N.K.

    1985-01-01

    Direct observation of radiation damage induced by heavy ion implantation in crystalline germanium by means of high-resolution electron microscopy is reported. The dark-field lattice imaging mode is used, under conditions suitable for object-like imaging. Conventional TEM is used for estimating the efficiency of creating visibly damaged regions. Heavy ion damage clusters with three types of inner structure are observed: with near-perfect crystalline cores, and with metastable and stable amorphous cores. The MARLOWE computer code is used to simulate the atomic collision cascades and to obtain the lateral spread distributions of point defects created. A comparison of high-resolution electron microscopy (HREM) with computer simulation results shows encouraging agreement for the average cluster dimensions and for the lateral spread of vacancies and interstitials. (author)

  4. Synchronizing atomic force microscopy force mode and fluorescence microscopy in real time for immune cell stimulation and activation studies

    Energy Technology Data Exchange (ETDEWEB)

    Cazaux, Séverine; Sadoun, Anaïs; Biarnes-Pelicot, Martine; Martinez, Manuel; Obeid, Sameh [Aix Marseille Université, LAI UM 61, Marseille F-13288 (France); Inserm, UMR-S 1067, Marseille F-13288 (France); CNRS, UMR 7333, Marseille F-13288 (France); Bongrand, Pierre [Aix Marseille Université, LAI UM 61, Marseille F-13288 (France); Inserm, UMR-S 1067, Marseille F-13288 (France); CNRS, UMR 7333, Marseille F-13288 (France); APHM, Hôpital de la Conception, Laboratoire d’Immunologie, Marseille F-13385 (France); Limozin, Laurent [Aix Marseille Université, LAI UM 61, Marseille F-13288 (France); Inserm, UMR-S 1067, Marseille F-13288 (France); CNRS, UMR 7333, Marseille F-13288 (France); Puech, Pierre-Henri, E-mail: pierre-henri.puech@inserm.fr [Aix Marseille Université, LAI UM 61, Marseille F-13288 (France); Inserm, UMR-S 1067, Marseille F-13288 (France); CNRS, UMR 7333, Marseille F-13288 (France)

    2016-01-15

    A method is presented for combining atomic force microscopy (AFM) force mode and fluorescence microscopy in order to (a) mechanically stimulate immune cells while recording the subsequent activation under the form of calcium pulses, and (b) observe the mechanical response of a cell upon photoactivation of a small G protein, namely Rac. Using commercial set-ups and a robust signal coupling the fluorescence excitation light and the cantilever bending, the applied force and activation signals were very easily synchronized. This approach allows to control the entire mechanical history of a single cell up to its activation and response down to a few hundreds of milliseconds, and can be extended with very minimal adaptations to other cellular systems where mechanotransduction is studied, using either purely mechanical stimuli or via a surface bound specific ligand. - Highlights: • A signal coupling AFM and fluorescence microscopy was characterized for soft cantilevers. • It can be used as an intrinsic timer to synchronize images and forces. • Mechanical stimulation of single immune cells while recording calcium fluxes was detailed. • Light-induced mechanical modifications of lymphocytes using a PA-Rac protein were demonstrated. • The precautions and limitations of use of this effect were presented.

  5. Nanoscale changes in chromatin organization represent the initial steps of tumorigenesis: a transmission electron microscopy study

    International Nuclear Information System (INIS)

    Cherkezyan, Lusik; Backman, Vadim; Stypula-Cyrus, Yolanda; Subramanian, Hariharan; White, Craig; Dela Cruz, Mart; Wali, Ramesh K; Goldberg, Michael J; Bianchi, Laura K; Roy, Hemant K

    2014-01-01

    Nuclear alterations are a well-known manifestation of cancer. However, little is known about the early, microscopically-undetectable stages of malignant transformation. Based on the phenomenon of field cancerization, the tissue in the field of a tumor can be used to identify and study the initiating events of carcinogenesis. Morphological changes in nuclear organization have been implicated in the field of colorectal cancer (CRC), and we hypothesize that characterization of chromatin alterations in the early stages of CRC will provide insight into cancer progression, as well as serve as a biomarker for early detection, risk stratification and prevention. For this study we used transmission electron microscopy (TEM) images of nuclei harboring pre-neoplastic CRC alterations in two models: a carcinogen-treated animal model of early CRC, and microscopically normal-appearing tissue in the field of human CRC. We quantify the chromatin arrangement using approaches with two levels of complexity: 1) binary, where chromatin is separated into areas of dense heterochromatin and loose euchromatin, and 2) grey-scale, where the statistics of continuous mass-density distribution within the nucleus is quantified by its spatial correlation function. We established an increase in heterochromatin content and clump size, as well as a loss of its characteristic peripheral positioning in microscopically normal pre-neoplastic cell nuclei. Additionally, the analysis of chromatin density showed that its spatial distribution is altered from a fractal to a stretched exponential. We characterize quantitatively and qualitatively the nanoscale structural alterations preceding cancer development, which may allow for the establishment of promising new biomarkers for cancer risk stratification and diagnosis. The findings of this study confirm that ultrastructural changes of chromatin in field carcinogenesis represent early neoplastic events leading to the development of well

  6. Contact microscopy with synchrotron radiation

    International Nuclear Information System (INIS)

    Panessa-Warren, B.J.

    1985-10-01

    Soft x-ray contact microscopy with synchrotron radiation offers the biologist and especially the microscopist, a way to morphologically study specimens that could not be imaged by conventional TEM, STEM or SEM methods (i.e. hydrated samples, samples easily damaged by an electron beam, electron dense samples, thick specimens, unstained low contrast specimens) at spatial resolutions approaching those of the TEM, with the additional possibility to obtain compositional (elemental) information about the sample as well. Although flash x-ray sources offer faster exposure times, synchrotron radiation provides a highly collimated, intense radiation that can be tuned to select specific discrete ranges of x-ray wavelengths or specific individual wavelengths which optimize imaging or microanalysis of a specific sample. This paper presents an overview of the applications of x-ray contact microscopy to biological research and some current research results using monochromatic synchrotron radiation to image biological samples. 24 refs., 10 figs

  7. Macroscopy and Microscopy Study of Scopraia dulcis L.

    Directory of Open Access Journals (Sweden)

    Djoko Santosa

    2018-04-01

    Full Text Available A morphological diversity analysis of Scoparia dulcis by macroscopy and microscopy has been conducted. The aim of this research is to determine the morphological and anatomical character of S. dulcis which grow in Opak watershed, Special Region of Yogyakarta. Samples were taken from Sleman (Cangkringan, Ngemplak Kalasan, and Prambanan and Bantul (Imogiri and Pundong region. Selection of sampling location is based on altitude difference. The samples are the third leaf order from the tip of the stem. They were measured in length and width. Microscopy analysis was performed by observing the number of glandular trichomes, palisade cells in the epidermis and stomata in the upper and lower epidermis. The data obtained were analyzed using principal component analysis (PCA. The results show that based on morphological and anatomical assessment, there were found 3 clusters of S. dulcis, i.e. Cangkringan-Ngemplak-Prambanan, Kalasan, and Imogiri-Pundong cluster.

  8. Confocal laser scanning microscopy in study of bone calcification

    Science.gov (United States)

    Nishikawa, Tetsunari; Kokubu, Mayu; Kato, Hirohito; Imai, Koichi; Tanaka, Akio

    2012-12-01

    Bone regeneration in mandible and maxillae after extraction of teeth or tumor resection and the use of rough surface implants in bone induction must be investigated to elucidate the mechanism of calcification. The calcified tissues are subjected to chemical decalcification or physical grinding to observe their microscopic features with light microscopy and transmission electron microscopy where the microscopic tissue morphology is significantly altered. We investigated the usefulness of confocal laser scanning microscopy (CLSM) for this purpose. After staggering the time of administration of calcein and alizarin red to experimental rats and dogs, rat alveolar bone and dog femur grafted with coral as scaffold or dental implants were observed with CLSM. In rat alveolar bone, the calcification of newly-formed bone and net-like canaliculi was observed at the mesial bone from the roots progressed at the rate of 15 μm/day. In dog femur grafted with coral, newly-formed bones along the space of coral were observed in an orderly manner. In dog femur with dental implants, after 8 weeks, newly-formed bone proceeded along the rough surface of the implants. CLSM produced high-magnification images of newly-formed bone and thin sections were not needed.

  9. Human enamel structure studied by high resolution electron microscopy

    International Nuclear Information System (INIS)

    Wen, S.L.

    1989-01-01

    Human enamel structural features are characterized by high resolution electron microscopy. The human enamel consists of polycrystals with a structure similar to Ca10(PO4)6(OH)2. This article describes the structural features of human enamel crystal at atomic and nanometer level. Besides the structural description, a great number of high resolution images are included. Research into the carious process in human enamel is very important for human beings. This article firstly describes the initiation of caries in enamel crystal at atomic and unit-cell level and secondly describes the further steps of caries with structural and chemical demineralization. The demineralization in fact, is the origin of caries in human enamel. The remineralization of carious areas in human enamel has drawn more and more attention as its potential application is realized. This process has been revealed by high resolution electron microscopy in detail in this article. On the other hand, the radiation effects on the structure of human enamel are also characterized by high resolution electron microscopy. In order to reveal this phenomenon clearly, a great number of electron micrographs have been shown, and a physical mechanism is proposed. 26 references

  10. Accelerator-tem interface facility and application

    International Nuclear Information System (INIS)

    Li Ming; He Jun; Yang Zheng; Zhou Lin; Liu Chuansheng; Guo Liping; Jiang Changzhong; Yang Shibo; Fu Dejun; Fan Xiangjun; Liu Jiarui; Lee, J.C.

    2010-01-01

    An accelerator-TEM interface facility has been established at Wuhan University. The system consists of an H800 TEM linked to a 200 kV ion implanter and a 2 x 1.7 MV tandetron accelerator. Measures were taken to isolate the TEM from mechanical vibration transmitted from the ion beam lines and good resolution was maintained with the TEM machine when operated under high zoom modes during the ion implantation. Nitrogen ions at 115 keV were successfully transported from the implanter into the TEM chamber through the interface system, and the ion currents measured at the entrance of the TEM column were between 20 and 180 nA. Structural evolution caused by ion irradiation in Si, GaAs, nanocrystal Ag were observed in situ. The TEM sample could be tilted by 52 degree and for low energy ion irradiation, real time observation was realized. The in situ observation showed that the critical implant dose for amorphization of Si is 2 x 10 14 cm -2 and it became fully amorphized at 3 x 10 15 cm -2 . Amorphization of GaAs started at 1 x 10 14 cm -2 , whereas for nanocrystal Ag, the starting dose was 6 x 10 14 cm -2 . The nuclear material C276 samples implanted with 115 keV Ar+ was also studied and dislocation loops with sizes of 3-12 nm were clearly observed after implantation to doses higher than 1 x 10 15 cm -2 . The density of the loops increased with the increase in the implant dose and evolution to polycrystalline and amorphous structures were observed at 5 x 10 15 cm -2 and 3 x 10 16 cm -2 , respectively. An in situ RBS/C chamber has been installed on the transport line of the accelerator-TEM interface system. This makes it possible to in situ measure composition and location of impurities in the lattice of the implanted samples. In addition, a 50 kV low-energy gaseous ion generator was installed close to the TEM chamber, which facilitates in situ TEM observation of helium bubbles formed in materials by helium implantation. (authors)

  11. Correlative Light- and Electron Microscopy Using Quantum Dot Nanoparticles.

    Science.gov (United States)

    Killingsworth, Murray C; Bobryshev, Yuri V

    2016-08-07

    A method is described whereby quantum dot (QD) nanoparticles can be used for correlative immunocytochemical studies of human pathology tissue using widefield fluorescence light microscopy and transmission electron microscopy (TEM). To demonstrate the protocol we have immunolabeled ultrathin epoxy sections of human somatostatinoma tumor using a primary antibody to somatostatin, followed by a biotinylated secondary antibody and visualization with streptavidin conjugated 585 nm cadmium-selenium (CdSe) quantum dots (QDs). The sections are mounted on a TEM specimen grid then placed on a glass slide for observation by widefield fluorescence light microscopy. Light microscopy reveals 585 nm QD labeling as bright orange fluorescence forming a granular pattern within the tumor cell cytoplasm. At low to mid-range magnification by light microscopy the labeling pattern can be easily recognized and the level of non-specific or background labeling assessed. This is a critical step for subsequent interpretation of the immunolabeling pattern by TEM and evaluation of the morphological context. The same section is then blotted dry and viewed by TEM. QD probes are seen to be attached to amorphous material contained in individual secretory granules. Images are acquired from the same region of interest (ROI) seen by light microscopy for correlative analysis. Corresponding images from each modality may then be blended to overlay fluorescence data on TEM ultrastructure of the corresponding region.

  12. Environmental TEM for Materials Research

    DEFF Research Database (Denmark)

    Hansen, Thomas Willum

    Over the last decades, electron microscopy has played a large role in materials research. The increasing use of particularly environmental transmission electron microscopy (ETEM) in materials science provides new possibilities for investigating nanoscale components at work. Careful experimentation...

  13. Environmental TEM in Materials Research

    DEFF Research Database (Denmark)

    Hansen, Thomas Willum; Wagner, Jakob Birkedal

    Over the last decades, electron microscopy has played a large role in materials research. The increasing use of particularly environmental transmission electron microscopy (ETEM) in materials science provides new possibilities for investigating nanoscale components at work. Careful experimentation...

  14. Accelerator-TEM interface facility and application

    International Nuclear Information System (INIS)

    Liu Chuansheng; Li Ming; He Jun; Yang Zheng; Zhou Lin; Wang Zesong; Guo Liping; Jiang Changzhong; Yang Shibo; Fu Dejun; Fan Xiangjun; Liu Jiarui; Lee J C

    2010-01-01

    An accelerator-TEM interface facility has been established at Wuhan University in 2008. The system consists of an H800 TEM linked to a 200 kV ion implanter and a 2 x 1.7 MV tandem accelerator. Nitrogen ions at 115 keV were successfully transported from the implanter into the TEM chamber through the interface system, and the ion currents measured at the entrance of the TEM column were between 20 and 180 nA. Structural evolution caused by ion irradiation in Si, GaAs, nanocrystal Ag was observed in situ. The in situ observation showed that the critical implantation dose for amorphization of Si is 10 14 cm -2 . The nuclear material C276 samples implanted with 115 keV Ar + was also studied, and dislocation loops sized at 3-12 nm were clearly observed after implantation to doses of over 1 x 10 15 cm -2 . The density of the loops increased with the dose. Evolution to polycrystalline and amorphous structures were observed at 5 x l0 15 cm -2 and 3 x 10 16 cm -2 , respectively. An in situ RBS/C chamber was installed on the transport line of the accelerator-TEM interface system. This enables in situ measurement of composition and location of the implanted species in lattice of the samples. In addition, a 50 kV low-energy gaseous ion generator was installed close to the TEM chamber, which facilitates in situ TEM observation of helium bubbles formed in helium-implanted materials. (authors)

  15. Standardized Polyalthia longifolia leaf extract (PLME) inhibits cell proliferation and promotes apoptosis: The anti-cancer study with various microscopy methods.

    Science.gov (United States)

    Vijayarathna, Soundararajan; Chen, Yeng; Kanwar, Jagat R; Sasidharan, Sreenivasan

    2017-07-01

    Over the years a number of microscopy methods have been developed to assess the changes in cells. Some non-invasive techniques such as holographic digital microscopy (HDM), which although does not destroy the cells, but helps to monitor the events that leads to initiation of apoptotic cell death. In this study, the apoptogenic property and the cytotoxic effect of P. longifolia leaf methanolic extract (PLME) against the human cervical carcinoma cells (HeLa) was studied using light microscope (LM), holographic digital microscopy (HDM), scanning electron microscope (SEM) and transmission electron microscope (TEM). The average IC 50 value of PLME against HeLa cells obtained by MTT and CyQuant assay was 22.00μg/mL at 24h. However, noncancerous Vero cells tested with PLME exhibited no cytotoxicity with the IC 50 value of 51.07μg/mL at 24h by using MTT assay. Cytological observations showed nuclear condensation, cell shrinkage, multinucleation, abnormalities of mitochondrial cristae, membrane blebbing, disappearance of microvilli and filopodia, narrowing of lamellipodia, holes, formation of numerous smaller vacuoles, cytoplasmic extrusions and formation of apoptotic bodies as confirmed collectively by HDM, LM, SEM and TEM. In conclusion, PLME was able to produce distinctive morphological features of HeLa cell death that corresponds to apoptosis. Copyright © 2017 Elsevier Masson SAS. All rights reserved.

  16. Electron microscopy study of antioxidant interaction with bacterial cells

    Science.gov (United States)

    Plotnikov, Oleg P.; Novikova, Olga V.; Konnov, Nikolai P.; Korsukov, Vladimir N.; Gunkin, Ivan F.; Volkov, Uryi P.

    2000-10-01

    To maintain native microorganisms genotype and phenotype features a lyophylization technique is widely used. However in this case cells are affected by influences of vacuum and low temperature that cause a part of the cells population to be destruction. Another factor reduced microorganisms vitality is formation of reactive oxygen forms that damage certain biological targets (such as DNA, membranes etc.) Recently to raise microorganism's resistance against adverse condition natural and synthetic antioxidants are used. Antioxidant- are antagonists of free radicals. Introduction of antioxidants in protective medium for lyophylization increase bacteria storage life about 2,0-4,8 fold in comparison with reference samples. In the article the main results of our investigation of antioxidants interaction with microorganism cells is described. As bacteria cells we use vaccine strain yersinia pestis EV, that were grown for 48 h at 28 degree(s)C on the Hottinger agar (pH 7,2). Antioxidants are inserted on the agar surface in specimen under test. To investigate a localization of antioxidants for electron microscopy investigation, thallium organic antioxidants were used. The thallium organic compounds have an antioxidant features if thallium is in low concentration (about 1(mu) g/ml). The localization of the thallium organic antioxidants on bacteria Y. pestis EV is visible in electron microscopy images, thallium being heavy metal with high electron density. The negatively stained bacteria and bacteria thin sections with thallium organic compounds were investigated by means of transmission electron microscopy. The localization of the thallium organic compounds is clearly visible in electron micrographs as small dark spots with size about 10-80nm. Probably mechanisms of interaction of antioxidants with bacteria cells are discussed.

  17. Confocal laser scanning microscopy in study of bone calcification

    Energy Technology Data Exchange (ETDEWEB)

    Nishikawa, Tetsunari, E-mail: tetsu-n@cc.osaka-dent.ac.jp [Department of Oral Pathology, Osaka Dental University, Osaka (Japan); Kokubu, Mayu; Kato, Hirohito [Department of Oral Pathology, Osaka Dental University, Osaka (Japan); Imai, Koichi [Department of Biomaterials, Osaka Dental University, Osaka (Japan); Tanaka, Akio [Department of Oral Pathology, Osaka Dental University, Osaka (Japan)

    2012-12-01

    Highlights: Black-Right-Pointing-Pointer High-magnification images with depth selection, and thin sections were observed using CLSM. Black-Right-Pointing-Pointer The direction and velocity of calcification of the bone was observed by administration of 2 fluorescent dyes. Black-Right-Pointing-Pointer In dog femora grafted with coral blocks, newly-formed bone was observed in the coral block space with a rough surface. Black-Right-Pointing-Pointer Twelve weeks after dental implant was grafted in dog femora, the space between screws was filled with newly-formed bones. - Abstract: Bone regeneration in mandible and maxillae after extraction of teeth or tumor resection and the use of rough surface implants in bone induction must be investigated to elucidate the mechanism of calcification. The calcified tissues are subjected to chemical decalcification or physical grinding to observe their microscopic features with light microscopy and transmission electron microscopy where the microscopic tissue morphology is significantly altered. We investigated the usefulness of confocal laser scanning microscopy (CLSM) for this purpose. After staggering the time of administration of calcein and alizarin red to experimental rats and dogs, rat alveolar bone and dog femur grafted with coral as scaffold or dental implants were observed with CLSM. In rat alveolar bone, the calcification of newly-formed bone and net-like canaliculi was observed at the mesial bone from the roots progressed at the rate of 15 {mu}m/day. In dog femur grafted with coral, newly-formed bones along the space of coral were observed in an orderly manner. In dog femur with dental implants, after 8 weeks, newly-formed bone proceeded along the rough surface of the implants. CLSM produced high-magnification images of newly-formed bone and thin sections were not needed.

  18. Confocal laser scanning microscopy in study of bone calcification

    International Nuclear Information System (INIS)

    Nishikawa, Tetsunari; Kokubu, Mayu; Kato, Hirohito; Imai, Koichi; Tanaka, Akio

    2012-01-01

    Highlights: ► High-magnification images with depth selection, and thin sections were observed using CLSM. ► The direction and velocity of calcification of the bone was observed by administration of 2 fluorescent dyes. ► In dog femora grafted with coral blocks, newly-formed bone was observed in the coral block space with a rough surface. ► Twelve weeks after dental implant was grafted in dog femora, the space between screws was filled with newly-formed bones. - Abstract: Bone regeneration in mandible and maxillae after extraction of teeth or tumor resection and the use of rough surface implants in bone induction must be investigated to elucidate the mechanism of calcification. The calcified tissues are subjected to chemical decalcification or physical grinding to observe their microscopic features with light microscopy and transmission electron microscopy where the microscopic tissue morphology is significantly altered. We investigated the usefulness of confocal laser scanning microscopy (CLSM) for this purpose. After staggering the time of administration of calcein and alizarin red to experimental rats and dogs, rat alveolar bone and dog femur grafted with coral as scaffold or dental implants were observed with CLSM. In rat alveolar bone, the calcification of newly-formed bone and net-like canaliculi was observed at the mesial bone from the roots progressed at the rate of 15 μm/day. In dog femur grafted with coral, newly-formed bones along the space of coral were observed in an orderly manner. In dog femur with dental implants, after 8 weeks, newly-formed bone proceeded along the rough surface of the implants. CLSM produced high-magnification images of newly-formed bone and thin sections were not needed.

  19. Local adhesive surface properties studied by force microscopy

    International Nuclear Information System (INIS)

    Lekka, M.; Lekki, J.; Marszalek, M.; Stachura, Z.; Cleff, B.

    1998-01-01

    Scanning force microscopy was used in the contact mode to determine the adhesion force between a mica surface and a silicon nitride tip. The measurements were performed in an aqueous solution of sodium and calcium chlorides. The adhesion force according to the Derjaguin-Landau-Verwey-Overbeek theory depends on the competition between two kinds of forces: van der Waals and electrostatic 'double layer'. Two different curves of adhesion force versus salt concentration were obtained from the experiment with monovalent and divalent ions. The tip-surface adhesion force was determined from a statistical analysis of data obtained from the force vs. distance retracting curves. (author)

  20. In situ transmission electron microscopy and scanning transmission electron microscopy studies of sintering of Ag and Pt nanoparticles

    International Nuclear Information System (INIS)

    Asoro, M.A.; Ferreira, P.J.; Kovar, D.

    2014-01-01

    Transmission electron microscopy and scanning transmission electron microscopy studies were conducted in situ on 2–5 nm Pt and 10–40 nm Ag nanoparticles to study mechanisms for sintering and to measure relevant sintering kinetics in nanoscale particles. Sintering between two separated particles was observed to initiate by either (1) diffusion of the particles on the sample support or (2) diffusion of atoms or small clusters of atoms to the neck region between the two particles. After particle contact, the rate of sintering was controlled by atomic surface diffusivity. The surface diffusivity was determined as a function of particle size and temperature from experimental measurements of the rate of neck growth of the particles. The surface diffusivities did not show a strong size effect for the range of particle sizes that were studied. The surface diffusivity for Pt nanoparticles exhibited the expected Arrhenius temperature dependence and did not appear to be sensitive to the presence of surface contaminants. In contrast, the surface diffusivity for Ag nanoparticles was affected by the presence of impurities such as carbon. The diffusivities for Ag nanoparticles were consistent with previous measurements of bulk surface diffusivities for Ag in the presence of C, but were significantly slower than those obtained from pristine Ag

  1. Observation of Pt-{100}-p(2×2-O reconstruction by an environmental TEM

    Directory of Open Access Journals (Sweden)

    Hengbo Li

    2016-06-01

    Full Text Available The surface structure of noble metal nanoparticles usually plays a crucial role during the catalytic process in the fields of energy and environment. It has been studied extensively by surface analytic methods, such as scanning tunneling microscopy. However, it is still challenging to secure a direct observation of the structural evolution of surfaces of nanocatalysts in reaction (gas and heating conditions at the atomic scale. Here we report an in-situ observation of atomic reconstruction on Pt {100} surfaces exposed to oxygen in an environmental transmission electron microscope (TEM. Our high-resolution TEM images revealed that Pt-{100}-p(2×2-O reconstruction occurs during the reaction between oxygen atoms and {100} facets. A reconstruction model was proposed, and TEM images simulated according to this model with different defocus values match the experimental results well.

  2. Scanning Ion Conductance Microscopy for Studying Biological Samples

    Directory of Open Access Journals (Sweden)

    Irmgard D. Dietzel

    2012-11-01

    Full Text Available Scanning ion conductance microscopy (SICM is a scanning probe technique that utilizes the increase in access resistance that occurs if an electrolyte filled glass micro-pipette is approached towards a poorly conducting surface. Since an increase in resistance can be monitored before the physical contact between scanning probe tip and sample, this technique is particularly useful to investigate the topography of delicate samples such as living cells. SICM has shown its potential in various applications such as high resolution and long-time imaging of living cells or the determination of local changes in cellular volume. Furthermore, SICM has been combined with various techniques such as fluorescence microscopy or patch clamping to reveal localized information about proteins or protein functions. This review details the various advantages and pitfalls of SICM and provides an overview of the recent developments and applications of SICM in biological imaging. Furthermore, we show that in principle, a combination of SICM and ion selective micro-electrodes enables one to monitor the local ion activity surrounding a living cell.

  3. Graphene-based sample supports for in situ high-resolution TEM electrical investigations

    International Nuclear Information System (INIS)

    Westenfelder, B; Scholz, F; Meyer, J C; Biskupek, J; Algara-Siller, G; Lechner, L G; Kaiser, U; Kusterer, J; Kohn, E; Krill, C E III

    2011-01-01

    Specially designed transmission electron microscopy (TEM) sample carriers have been developed to enable atomically resolved studies of the heat-induced evolution of adsorbates on graphene and their influence on electrical conductivity. Here, we present a strategy for graphene-based carrier realization, evaluating its design with respect to fabrication effort and applications potential. We demonstrate that electrical current can lead to very high temperatures in suspended graphene membranes, and we determine that current-induced cleaning of graphene results from Joule heating.

  4. TEM turbulence optimisation in stellarators

    Science.gov (United States)

    Proll, J. H. E.; Mynick, H. E.; Xanthopoulos, P.; Lazerson, S. A.; Faber, B. J.

    2016-01-01

    With the advent of neoclassically optimised stellarators, optimising stellarators for turbulent transport is an important next step. The reduction of ion-temperature-gradient-driven turbulence has been achieved via shaping of the magnetic field, and the reduction of trapped-electron mode (TEM) turbulence is addressed in the present paper. Recent analytical and numerical findings suggest TEMs are stabilised when a large fraction of trapped particles experiences favourable bounce-averaged curvature. This is the case for example in Wendelstein 7-X (Beidler et al 1990 Fusion Technol. 17 148) and other Helias-type stellarators. Using this knowledge, a proxy function was designed to estimate the TEM dynamics, allowing optimal configurations for TEM stability to be determined with the STELLOPT (Spong et al 2001 Nucl. Fusion 41 711) code without extensive turbulence simulations. A first proof-of-principle optimised equilibrium stemming from the TEM-dominated stellarator experiment HSX (Anderson et al 1995 Fusion Technol. 27 273) is presented for which a reduction of the linear growth rates is achieved over a broad range of the operational parameter space. As an important consequence of this property, the turbulent heat flux levels are reduced compared with the initial configuration.

  5. Electron microscopy study of red mud after seawater neutralisation

    International Nuclear Information System (INIS)

    Toledo, S.P.; Kiyohara, P.K.; Antunes, M.L.P.; Frost, Ray

    2012-01-01

    Red Mud, residue of Bayer process for extracting alumina from bauxite, is produced in large quantity. This residue is very alkaline and can cause damage to health and the environment. One way to minimize the environmental impact of this residue is neutralization by sea water. The Brazilian Red Mud was treated with sea water. It appears that the initial pH of the samples is reduced to 8. The analysis by x-ray diffraction allows to identify the formation of hydrotalcite and aragonite. The transmission electron microscopy images show that this consists of particles with dimensions between 0.02 to 2 μm. It was possible to identify by EDS/MET particles of magnesium, confirming the formation of hydrotalcite. (author)

  6. Molecules on vicinal Au surfaces studied by scanning tunnelling microscopy

    International Nuclear Information System (INIS)

    Kroeger, J; Neel, N; Jensen, H; Berndt, R; Rurali, R; Lorente, N

    2006-01-01

    Using low-temperature scanning tunnelling microscopy and spectroscopy we investigated the adsorption characteristics of 3,4,9,10-perylenetetracarboxylic-dianhydride and fullerenes on Au(788), Au(433), and Au(778). On Au(788) and Au(778), 3,4,9,10-perylenetetracarboxylic-dianhydride exhibits three coexisting superstructures, which do not reflect the periodicity of the hosting substrate. The adsorption on Au(433) leads to the formation of molecule chains along the step edges after annealing the sample. Fullerene molecules on Au(788) arrange in a mesh of islands, which extends over several hundreds of nanometres with an extraordinarily high periodicity. A combination of fullerene adsorption and annealing leads to facetting of Au(433) and the formation of extraordinarily long fullerene stripes

  7. Nanoscale electrical property studies of individual GeSi quantum rings by conductive scanning probe microscopy.

    Science.gov (United States)

    Lv, Yi; Cui, Jian; Jiang, Zuimin M; Yang, Xinju

    2012-11-29

    The nanoscale electrical properties of individual self-assembled GeSi quantum rings (QRs) were studied by scanning probe microscopy-based techniques. The surface potential distributions of individual GeSi QRs are obtained by scanning Kelvin microscopy (SKM). Ring-shaped work function distributions are observed, presenting that the QRs' rim has a larger work function than the QRs' central hole. By combining the SKM results with those obtained by conductive atomic force microscopy and scanning capacitance microscopy, the correlations between the surface potential, conductance, and carrier density distributions are revealed, and a possible interpretation for the QRs' conductance distributions is suggested.

  8. Study of Perylenetetracarboxylic Acid Dimethylimide Films by Cyclic Thermal Desorption and Scanning Probe Microscopy

    Science.gov (United States)

    Pochtennyi, A. E.; Lappo, A. N.; Il'yushonok, I. P.

    2018-02-01

    Some results of studying the direct-current (DC) conductivity of perylenetetracarboxylic acid dimethylimide films by cyclic oxygen thermal desorption are presented. The microscopic parameters of hopping electron transport over localized impurity and intrinsic states were determined. The bandgap width and the sign of major current carriers were determined by scanning probe microscopy methods (atomic force microscopy, scanning probe spectroscopy, and photoassisted Kelvin probe force microscopy). The possibility of the application of photoassisted scanning tunneling microscopy for the nanoscale phase analysis of photoconductive films is discussed.

  9. Hydration of magnesia cubes: a helium ion microscopy study

    Directory of Open Access Journals (Sweden)

    Ruth Schwaiger

    2016-02-01

    Full Text Available Physisorbed water originating from exposure to the ambient can have a strong impact on the structure and chemistry of oxide nanomaterials. The effect can be particularly pronounced when these oxides are in physical contact with a solid substrate such as the ones used for immobilization to perform electron or ion microscopy imaging. We used helium ion microscopy (HIM and investigated morphological changes of vapor-phase-grown MgO cubes after vacuum annealing and pressing into foils of soft and high purity indium. The indium foils were either used as obtained or, for reference, subjected to vacuum drying. After four days of storage in the vacuum chamber of the microscope and at a base pressure of p −7 mbar, we observed on these cubic particles the attack of residual physisorbed water molecules from the indium substrate. As a result, thin magnesium hydroxide layers spontaneously grew, giving rise to characteristic volume expansion effects, which depended on the size of the particles. Rounding of the originally sharp cube edges leads to a significant loss of the morphological definition specific to the MgO cubes. Comparison of different regions within one sample before and after exposure to liquid water reveals different transformation processes, such as the formation of Mg(OH2 shells that act as diffusion barriers for MgO dissolution or the evolution of brucite nanosheets organized in characteristic flower-like microstructures. The findings underline the significant metastability of nanomaterials under both ambient and high-vacuum conditions and show the dramatic effect of ubiquitous water films during storage and characterization of oxide nanomaterials.

  10. Electron microscopy and EXAFS studies on oxide-supported gold-silver nanoparticles prepared by flame spray pyrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Hannemann, Stefan [Institute of Chemical and Bioengineering, Swiss Federal Institute of Technology, ETH Hoenggerberg, CH-8093 Zurich (Switzerland); Grunwaldt, Jan-Dierk [Institute of Chemical and Bioengineering, Swiss Federal Institute of Technology, ETH Hoenggerberg, CH-8093 Zurich (Switzerland)]. E-mail: grunwaldt@chem.ethz.ch; Krumeich, Frank [Laboratory of Inorganic Chemistry, Swiss Federal Institute of Technology, ETH Hoenggerberg, CH-8093 Zurich (Switzerland); Kappen, Peter [Department of Physics, La Trobe University, Victoria 3086 (Australia); Baiker, Alfons [Institute of Chemical and Bioengineering, Swiss Federal Institute of Technology, ETH Hoenggerberg, CH-8093 Zurich (Switzerland)

    2006-09-15

    Gold and gold-silver nanoparticles prepared by flame spray pyrolysis (FSP) were characterized by electron microscopy, in situ X-ray absorption spectroscopy (XANES and EXAFS), X-ray diffraction (XRD) and their catalytic activity in CO oxidation. Within this one-step flame-synthesis procedure, precursor solutions of dimethyl gold(III) acetylacetonate and silver(I) benzoate together with the corresponding precursor of the silica, iron oxide or titania support, were sprayed and combusted. In order to prepare small metal particles, a low noble metal loading was required. A loading of 0.1-1 wt.% of Au and Ag resulted in 1-6 nm particles. The size of the noble metal particles increased with higher loadings of gold and particularly silver. Both scanning transmission electron microscopy (STEM) combined with energy dispersive X-ray spectroscopy (EDXS) and X-ray absorption spectroscopy (XAS) studies proved the formation of mixed Au-Ag particles. In case of 1% Au-1% Ag/SiO{sub 2}, TEM combined with electron spectroscopic imaging (ESI) using an imaging filter could be used in addition to prove the presence of silver and gold in the same noble metal particle. CO oxidation in the presence of hydrogen was chosen as a test reaction sensitive to small gold particles. Both the influence of the particle size and the alloying of gold and silver were reflected in the CO oxidation activity.

  11. Electron microscopy and EXAFS studies on oxide-supported gold-silver nanoparticles prepared by flame spray pyrolysis

    International Nuclear Information System (INIS)

    Hannemann, Stefan; Grunwaldt, Jan-Dierk; Krumeich, Frank; Kappen, Peter; Baiker, Alfons

    2006-01-01

    Gold and gold-silver nanoparticles prepared by flame spray pyrolysis (FSP) were characterized by electron microscopy, in situ X-ray absorption spectroscopy (XANES and EXAFS), X-ray diffraction (XRD) and their catalytic activity in CO oxidation. Within this one-step flame-synthesis procedure, precursor solutions of dimethyl gold(III) acetylacetonate and silver(I) benzoate together with the corresponding precursor of the silica, iron oxide or titania support, were sprayed and combusted. In order to prepare small metal particles, a low noble metal loading was required. A loading of 0.1-1 wt.% of Au and Ag resulted in 1-6 nm particles. The size of the noble metal particles increased with higher loadings of gold and particularly silver. Both scanning transmission electron microscopy (STEM) combined with energy dispersive X-ray spectroscopy (EDXS) and X-ray absorption spectroscopy (XAS) studies proved the formation of mixed Au-Ag particles. In case of 1% Au-1% Ag/SiO 2 , TEM combined with electron spectroscopic imaging (ESI) using an imaging filter could be used in addition to prove the presence of silver and gold in the same noble metal particle. CO oxidation in the presence of hydrogen was chosen as a test reaction sensitive to small gold particles. Both the influence of the particle size and the alloying of gold and silver were reflected in the CO oxidation activity

  12. Friction force microscopy study of annealed diamond-like carbon film

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Won Seok; Joung, Yeun-Ho [School of Electrical Engineering, Hanbat National University, Daejeon 305-719 (Korea, Republic of); Heo, Jinhee [Materials Safety Evaluation Group, Korea Institute of Materials Science, Changwon 641-831 (Korea, Republic of); Hong, Byungyou, E-mail: byhong@skku.edu [School of Information and Communication Engineering, Sungkyunkwan University, Suwon 440-746 (Korea, Republic of)

    2012-10-15

    In this paper we introduce mechanical and structural characteristics of diamond-like carbon (DLC) films which were prepared on silicon substrates by radio frequency (RF) plasma enhanced chemical vapor deposition (PECVD) method using methane (CH{sub 4}) and hydrogen (H{sub 2}) gas. The films were annealed at various temperatures ranging from 300 to 900 °C in steps of 200 °C using rapid thermal processor (RTP) in nitrogen ambient. Tribological properties of the DLC films were investigated by atomic force microscopy (AFM) in friction force microscopy (FFM) mode. The structural properties of the films were obtained by high resolution transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The wettability of the films was obtained using contact angle measurement. XPS analysis showed that the sp{sup 3} content is decreased from 75.2% to 24.1% while the sp{sup 2} content is increased from 24.8% to 75.9% when the temperature is changed from 300 to 900 °C. The contact angles of DLC films were higher than 70°. The FFM measurement results show that the highest friction coefficient value was achieved at 900 °C annealing temperature.

  13. Friction force microscopy study of annealed diamond-like carbon film

    International Nuclear Information System (INIS)

    Choi, Won Seok; Joung, Yeun-Ho; Heo, Jinhee; Hong, Byungyou

    2012-01-01

    In this paper we introduce mechanical and structural characteristics of diamond-like carbon (DLC) films which were prepared on silicon substrates by radio frequency (RF) plasma enhanced chemical vapor deposition (PECVD) method using methane (CH 4 ) and hydrogen (H 2 ) gas. The films were annealed at various temperatures ranging from 300 to 900 °C in steps of 200 °C using rapid thermal processor (RTP) in nitrogen ambient. Tribological properties of the DLC films were investigated by atomic force microscopy (AFM) in friction force microscopy (FFM) mode. The structural properties of the films were obtained by high resolution transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The wettability of the films was obtained using contact angle measurement. XPS analysis showed that the sp 3 content is decreased from 75.2% to 24.1% while the sp 2 content is increased from 24.8% to 75.9% when the temperature is changed from 300 to 900 °C. The contact angles of DLC films were higher than 70°. The FFM measurement results show that the highest friction coefficient value was achieved at 900 °C annealing temperature.

  14. Correlated Fluorescence-Atomic Force Microscopy Studies of the Clathrin Mediated Endocytosis in SKMEL Cells

    Science.gov (United States)

    Smith, Steve; Hor, Amy; Luu, Anh; Kang, Lin; Scott, Brandon; Bailey, Elizabeth; Hoppe, Adam

    Clathrin-mediated endocytosis is one of the central pathways for cargo transport into cells, and plays a major role in the maintenance of cellular functions, such as intercellular signaling, nutrient intake, and turnover of plasma membrane in cells. The clathrin-mediated endocytosis process involves invagination and formation of clathrin-coated vesicles. However, the biophysical mechanisms of vesicle formation are still debated. We investigate clathrin vesicle formation mechanisms through the utilization of tapping-mode atomic force microscopy for high resolution topographical imaging in neutral buffer solution of unroofed cells exposing the inner membrane, combined with fluorescence imaging to definitively label intracellular constituents with specific fluorescent fusion proteins (actin filaments labeled with green phalloidin-antibody and clathrin coated vesicles with the fusion protein Tq2) in SKMEL (Human Melanoma) cells. Results from our work are compared against dynamical polarized total internal fluorescence (TIRF), super-resolution photo-activated localization microscopy (PALM) and transmission electron microscopy (TEM) to draw conclusions regarding the prominent model of vesicle formation in clathrin-mediated endocytosis. Funding provided by NSF MPS/DMR/BMAT award # 1206908.

  15. Structural TEM study of nonpolar a-plane gallium nitride grown on(112_0) 4H-SiC by organometallic vapor phase epitaxy

    Energy Technology Data Exchange (ETDEWEB)

    Zakharov, Dmitri N.; Liliental-Weber, Zuzanna; Wagner, Brian; Reitmeier,Zachary J.; Preble, Edward A.; Davis, Robert F.

    2005-04-05

    Conventional and high resolution electron microscopy havebeen applied for studying lattice defects in nonpolar a-plane GaN grownon a 4H-SiC substrate with an AlN buffer layer. Samples in plan-view andcross-section configurations have been investigated. Basal and prismaticstacking faults together with Frank and Shockley partial dislocationswere found to be the main defects in the GaN layers. High resolutionelectron microscopy in combination with image simulation supported Drum smodel for the prismatic stacking faults. The density of basal stackingfaults was measured to be ~;1.6_106cm-1. The densities of partialdislocations terminating I1 and I2 types of intrinsic basal stackingfaults were ~;4.0_1010cm-2 and ~;0.4_1010cm-2, respectively. The energyof the I2 stacking fault in GaN was estimated to be (40+-4) erg/cm2 basedon the separation of Shockley partial dislocations. To the best of ourknowledge, the theoretically predicted I3 basal stacking fault in GaN wasobserved experimentally for the first time.

  16. Study of temperature and radiation induced microstructural changes in Xe-implanted UO2 by TEM, STEM, SIMS and positron spectroscopy

    International Nuclear Information System (INIS)

    Djourelov, Nikolay; Marchand, Benoît; Marinov, Hristo; Moncoffre, Nathalie; Pipon, Yves; Bérerd, Nicolas; Nédélec, Patrick; Raimbault, Louis; Epicier, Thierry

    2013-01-01

    Doppler broadening of annihilation gamma-line combined with a slow positron beam (SPB) was used to measure the momentum density distribution of annihilating pairs in a set of sintered UO 2 samples implantated with 800-keV 136 Xe 2+ at fluences of 1 × 10 15 and 1 × 10 16 Xe cm −2 . The effect of prolonged post-implantation annealing at 1673 and 1873 K, grain size, and 152-MeV Iodine irradiation were studied by analysis of S(E) profiles and S-W maps and discussed versus secondary ion mass spectroscopy (SIMS), scanning transmission electron microscopy results. Spectroscopy with SPB and SIMS is an excellent combination of complementary techniques for studying the formation and evolution of Xe-bubbles, and Xe retention

  17. Comparison of ultramicrotomy and focused-ion-beam for the preparation of TEM and STEM cross section of organic solar cells

    DEFF Research Database (Denmark)

    Corazza, Michael; Simonsen, Søren Bredmose; Gnaegi, Helmut

    2016-01-01

    The challenge of preparing cross sections of organic photovoltaics (OPV) suitable for transmission electron microscopy (TEM) and scanning TEM (STEM) is addressed. The samples were polymer solar cells fabricated using roll-to-roll (R2R) processing methods on a flexible polyethylene terephthalate...... resolution, enabling further studies of phase separation of P3HT:PCBM by means of energy filtered TEM (EFTEM). The sample prepared by FIB shows good structure preservation, but reduced resolution due to non-optimal thicknesses achieved after treatment. Degradation studies of samples prepared...

  18. Atomic Force Microscopy Application in Biological Research: A Review Study

    Directory of Open Access Journals (Sweden)

    Surena Vahabi

    2013-06-01

    Full Text Available Atomic force microscopy (AFM is a three-dimensional topographic technique with a high atomic resolution to measure surface roughness. AFM is a kind of scanning probe microscope, and its near-field technique is based on the interaction between a sharp tip and the atoms of the sample surface. There are several methods and many ways to modify the tip of the AFM to investigate surface properties, including measuring friction, adhesion forces and viscoelastic properties as well as determining the Young modulus and imaging magnetic or electrostatic properties. The AFM technique can analyze any kind of samples such as polymers, adsorbed molecules, films or fibers, and powders in the air whether in a controlled atmosphere or in a liquid medium. In the past decade, the AFM has emerged as a powerful tool to obtain the nanostructural details and biomechanical properties of biological samples, including biomolecules and cells. The AFM applications, techniques, and -in particular- its ability to measure forces, are not still familiar to most clinicians. This paper reviews the literature on the main principles of the AFM modality and highlights the advantages of this technique in biology, medicine, and- especially- dentistry. This literature review was performed through E-resources, including Science Direct, PubMed, Blackwell Synergy, Embase, Elsevier, and Scholar Google for the references published between 1985 and 2010.

  19. Scanning electron microscopy and roughness study of dental composite degradation.

    Science.gov (United States)

    Soares, Luís Eduardo Silva; Cortez, Louise Ribeiro; Zarur, Raquel de Oliveira; Martin, Airton Abrahão

    2012-04-01

    Our aim was to test the hypothesis that the use of mouthwashes, consumption of soft drinks, as well as the type of light curing unit (LCU), would change the surface roughness (Ra) and morphology of a nanofilled composite resin (Z350® 3M ESPE). Samples (80) were divided into eight groups: Halogen LCU, group 1, saliva (control); group 2, Pepsi Twist®; group 3, Listerine®; group 4, Colgate Plax®; LED LCU, group 5, saliva; group 6, Pepsi Twist®; group 7, Listerine®; group 8, Colgate Plax®. Ra values were measured at baseline, and after 7 and 14 days. One specimen of each group was prepared for scanning electron microscopy analysis after 14 days. The data were subjected to multifactor analysis of variance at a 95% confidence followed by Tukey's honestly significant difference post-hoc test. All the treatments resulted in morphological changes in composite resin surface, and the most significant change was in Pepsi Twist® groups. The samples of G6 had the greatest increase in Ra. The immersion of nanofilled resin in mouthwashes with alcohol and soft drink increases the surface roughness. Polymerization by halogen LCU (reduced light intensity) associated with alcohol contained mouthwash resulted in significant roughness on the composite.

  20. Electron microscopy study of radiation effects in boron carbide

    International Nuclear Information System (INIS)

    Stoto, T.

    1987-03-01

    Boron carbide is a disordered non-stoechiometric material with a strongly microtwinned polycristallyne microstructure. This ceramic is among the candidate materials for the first wall coating in fusion reactor and is used as a neutron absorber in the control rods of fast breeder reactors. The present work deals with the nature of radiation damage in this solid. Because of helium internal production, neutron irradiated boron carbide is affected by swelling and by a strong microcracking which can break up a pellet in fine powder. These processes are rather intensitive to the irradiation parameters (temperature, flux and even neutron spectrum). Transmission electron microscopy of samples irradiated by the fast neutrons of a reactor, the electrons of a high voltage electron microscope and of samples implanted with helium ions was used to understand the respective roles of helium and point defects in the processes of swelling and microcracking. The design of an irradiation chamber for helium implantation at controlled temperature from 600 to 1700 0 C was an important technical part of this work [fr

  1. Characterization of carbonated serpentine using XPS and TEM

    International Nuclear Information System (INIS)

    Schulze, Roland K.; Hill, Mary Ann; Field, Robert D.; Papin, Pallas A.; Hanrahan, Robert J.; Byler, Darrin D.

    2004-01-01

    With the increasing concentration volume of carbon dioxide in the atmosphere, there has been an increasing interest in carbon dioxide sequestration. One method is to store the carbon dioxide in mineral form, reacting solution dissolved CO 2 to precipitate carbonates. In order to understand whether or not such an endeavor is feasible, the carbonation reaction must first be understood. In this study, the surface of ground serpentine, untreated, heat treated and following a carbonation experiment, has been characterized using X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). The results indicate that the mechanism for the reaction involves dissolution of the serpentine through the formation of an amorphous phase and subsequent precipitation of magnesite. The rate limiting step appears to be the diffusion of Mg out of the amorphous phase

  2. LM and TEM study of the orthokeratinized and parakeratinized epithelium of the tongue in the domestic duck (Anas platyrhynchos f. domestica).

    Science.gov (United States)

    Skieresz-Szewczyk, Kinga; Jackowiak, Hanna; Ratajczak, Marlena

    2014-12-01

    The previous histological studies of the lingual mucosa in birds characterized two types of keratinized epithelium, i.e. orthokeratinized and parakeratinized. These epithelia are composed of three layers: basal, intermediate and keratinized. The present study showed detailed ultrastructural features of cells in particular layers of two types of keratinized epithelia on the tongue in the domestic duck and defined structural differences. TEM observations showed a gradual reduction in cell organelles in the following layers, at increasing amounts of keratin fibers. The characteristic feature of the ortho- and parakeratinized epithelium is the presence of sub-layers in the intermediate layer, i.e. the upper and lower part, which results from the different shape of cell nuclei and dye affinity of the cytoplasm. The keratinized layer of ortho- and parakeratinized epithelium is built of two types of cells such as electron dark and light cells, which undergo exfoliation. The basic difference between the keratinized epithelia is the presence of flattened cell nuclei in the keratinized layer of the parakeratinized epithelium. The differentiating feature is also an arrangement of keratin fibers in the cell cytoplasm of the keratinized layer. The analysis of the thickness of the epithelium and the keratinized layer, indicated differences between keratinized epithelia, which result from two variants of performing protective functions, either through a thick keratinized layer or by a higher epithelium. Differences in the ultrastructure of the ortho- and parakeratinized epithelium are associated with mechanical functions of the epithelium resulting from different forces acting on the tongue during feeding activities. Copyright © 2014 Elsevier Ltd. All rights reserved.

  3. Concurrent treatment of metamict and crystalline fergusonite by U, Th and Pb-rich fluids:an EMPA and TEM study

    Czech Academy of Sciences Publication Activity Database

    Škoda, R.; Čopkajová, R.; Klementová, Mariana

    2011-01-01

    Roč. 14, č. 1 (2011), s. 197-199 ISSN 0328-2767 R&D Projects: GA AV ČR KJB301630801 Institutional research plan: CEZ:AV0Z40320502 Keywords : fergusonite * metamict state * experimental alteration * EMPA * TEM Subject RIV: DB - Geology ; Mineralogy

  4. Destructive interference of TEM and ITG turbulence

    International Nuclear Information System (INIS)

    Merz, F.; Jenko, F.

    2009-01-01

    Full text: Turbulence driven by ion temperature gradient (ITG) modes and trapped electron modes (TEMs) is generally considered the key mechanism for anomalous transport in fusion devices on ion scales. But while pure ITG and, to a lesser extent, also pure TEM turbulence have been studied in detail over the last years, not much is presently known about nonlinear interactions between ITG modes and TEMs, which are often present simultaneously in experimentally relevant situations. This important issue is addressed by means of linear and nonlinear gyrokinetic simulations with the GENE code. To examine the properties of the (linear) TEM and ITG instabilities in the (realistic) transitional regime, the GENE code is run as eigenvalue solver, which allows for a systematic study of dominant and subdominant modes. Corresponding nonlinear initial value computations show that the particle transport of the turbulent system can be completely suppressed if the two driving instabilities are active simultaneously. The direct comparison of the linear modes and the corresponding turbulent system reveals a coexistence of the two microinstabilities in a transitional regime even at the same wave number. The consequences of this dual turbulence drive for transport modeling is discussed. (author)

  5. Study of deformation and fracture micro mechanisms of titanium alloy Ti-6Al-4V using electron microscopy and and X-ray diffraction techniques

    International Nuclear Information System (INIS)

    Morcelli, Aparecido Edilson

    2009-01-01

    This present work allowed the study of deformation and fracture micro mechanisms of titanium alloy Ti-6Al-4V, used commercially for the manufacture of metallic biomaterials. The techniques employed for the analysis of the material under study were: scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). The study of the influence and behavior of the phases present in titanium alloys is important to evaluate the behavior of cracks in titanium alloys with high mechanical strength, which have fine alpha (α), beta (β) and (α±β) microstructure, linking the presence of the phases with the strength of the material. The evaluation in situ of deformation and fracture micro mechanisms were performed by TEM and was also a study of phase transformations during cooling in titanium alloys, using the techniques of bright field, dark field and diffraction of electrons in the selected area. After heat treatment differences were observed between the amount of in relation to the original microstructure of the β and α phases material for different conditions used in heat treatment applied to the alloy. The presence of lamellar microstructure formed during cooling in the β field was observed, promoting the conversion of part of the secondary alpha structure in β phase, which was trapped between the lamellar of alpha. (author)

  6. High resolution transmission electron microscopy studies of {sigma} phase in Ni-based single crystal superalloys

    Energy Technology Data Exchange (ETDEWEB)

    Sun Fei [Key Laboratory of Liquid Structure and Heredity of Materials, Ministry of Education, Shandong University, Jinan 250061 (China); Zhang Jianxin, E-mail: jianxin@sdu.edu.cn [Key Laboratory of Liquid Structure and Heredity of Materials, Ministry of Education, Shandong University, Jinan 250061 (China); Liu Pan [Institute of Microstructure and Property of Advanced Materials, Beijing University of Technology, Beijing 100124 (China); Feng Qiang [National Center for Materials Service Safety, University of Science and Technology Beijing, Beijing 100083 (China); State Key Laboratory for Advanced Metals and Materials, University of Science and Technology Beijing, Beijing 100083 (China); Han Xiaodong; Mao Shengcheng [Institute of Microstructure and Property of Advanced Materials, Beijing University of Technology, Beijing 100124 (China)

    2012-09-25

    Graphical abstract: (a) TEM micrograph of {sigma} phase; (b) HRTEM image of {sigma}/{gamma} interface corresponding to the area of the white frame in (a); (c) an enlarged image of area from the white frame in (b). The combination of {sigma}/{gamma} interface appears very well, and a two-atomic-layer step is shown on the {sigma}/{gamma} interface. In addition, {sigma} phase has the orientation relationship of [0 0 1]{sub {gamma}}//[1 1 2{sup Macron }]{sub {sigma}}, (2{sup Macron} 2 0){sub {gamma}}//(1{sup Macron} 1 0){sub {sigma}}, (2{sup Macron }2{sup Macron} 0){sub {gamma}}//(1 1 1){sub {sigma}}; [0 1 1]{sub {gamma}}//[1 1 0]{sub {sigma}}, (1 1{sup Macron} 1){sub {gamma}}//(0 0 1{sup Macron }){sub {sigma}} with the {gamma} phase. Highlights: Black-Right-Pointing-Pointer Elemental characteristic of {sigma} phase is studied by HAADF techniques and EDS analysis. Black-Right-Pointing-Pointer Interfacial characteristics of {sigma}/{gamma} interface are revealed by HRTEM. Black-Right-Pointing-Pointer An atomic structural {sigma}/{gamma} interface with a two-atomic-layer step has been proposed. - Abstract: By means of high resolution transmission electron microscopy (HRTEM) and high-angle annular dark-field image technique (HAADF), morphological of plate-shaped {sigma} phase and interfacial characteristics between plate-shaped {sigma} phase and {gamma} phase in Ni-based single crystal superalloys have been studied. On the basis of HRTEM observations, an atomic structural interface between {sigma} phase and {gamma} phase with a step has been proposed. {sigma} Phase has the relationship of [0 0 1]{sub {gamma}}//[1 1 2{sup Macron }]{sub {sigma}}, (2{sup Macron} 2 0){sub {gamma}}//(1{sup Macron} 1 0){sub {sigma},} (2{sup Macron }2{sup Macron} 0){sub {gamma}}//(1 1 1){sub {sigma}}; [0 1 1]{sub {gamma}}//[1 1 0]{sub {sigma}}, (1 1{sup Macron} 1){sub {gamma}}//(0 0 1{sup Macron }){sub {sigma}} with the {gamma} phase. The compositional characteristics of the {sigma} phase which

  7. Atomic force microscopy studies of native photosynthetic membranes.

    Science.gov (United States)

    Sturgis, James N; Tucker, Jaimey D; Olsen, John D; Hunter, C Neil; Niederman, Robert A

    2009-05-05

    In addition to providing the earliest surface images of a native photosynthetic membrane at submolecular resolution, examination of the intracytoplasmic membrane (ICM) of purple bacteria by atomic force microscopy (AFM) has revealed a wide diversity of species-dependent arrangements of closely packed light-harvesting (LH) antennae, capable of fulfilling the basic requirements for efficient collection, transmission, and trapping of radiant energy. A highly organized architecture was observed with fused preparations of the pseudocrystalline ICM of Blastochloris viridis, consiting of hexagonally packed monomeric reaction center light-harvesting 1 (RC-LH1) core complexes. Among strains which also form a peripheral LH2 antenna, images of ICM patches from Rhodobacter sphaeroides exhibited well-ordered, interconnected networks of dimeric RC-LH1 core complexes intercalated by rows of LH2, coexisting with LH2-only domains. Other peripheral antenna-containing species, notably Rhodospirillum photometricum and Rhodopseudomonas palustris, showed a less regular organization, with mixed regions of LH2 and RC-LH1 cores, intermingled with large, paracrystalline domains. The ATP synthase and cytochrome bc(1) complex were not observed in any of these topographs and are thought to be localized in the adjacent cytoplasmic membrane or in inaccessible ICM regions separated from the flat regions imaged by AFM. The AFM images have served as a basis for atomic-resolution modeling of the ICM vesicle surface, as well as forces driving segregation of photosynthetic complexes into distinct domains. Docking of atomic-resolution molecular structures into AFM topographs of Rsp. photometricum membranes generated precise in situ structural models of the core complex surrounded by LH2 rings and a region of tightly packed LH2 complexes. A similar approach has generated a model of the highly curved LH2-only membranes of Rba. sphaeroides which predicts that sufficient space exists between LH2 complexes

  8. Annealing of hydrogen-induced defects in RF-plasma-treated Si wafers: ex situ and in situ transmission electron microscopy studies

    International Nuclear Information System (INIS)

    Ghica, C; Nistor, L C; Vizireanu, S; Dinescu, G

    2011-01-01

    The smart-cut(TM) process is based on inducing and processing structural defects below the free surface of semiconductor wafers. The necessary defects are currently induced by implantation of light elements such as hydrogen or helium. An alternative softer way to induce shallow subsurface defects is by RF-plasma hydrogenation. To facilitate the smart-cut process, the wafers containing the induced defects need to be subjected to an appropriate thermal treatment. In our experiments, (0 0 1) Si wafers are submitted to 200 and 50 W hydrogen RF-plasma and are subsequently annealed. The samples are studied by transmission electron microscopy (TEM), before and after annealing. The plasma-introduced defects are {1 1 1} and {1 0 0} planar-like defects and nanocavities, all of them involving hydrogen. Many nanocavities are aligned into strings almost parallel to the wafer surface. The annealing is performed either by furnace thermal treatment at 550 deg. C, or by in situ heating in the electron microscope at 450, 650 and 800 deg. C during the TEM observations. The TEM microstructural studies indicate a partial healing of the planar defects and a size increase of the nanometric cavities by a coalescence process of the small neighbouring nanocavities. By annealing, the lined up nanometric voids forming chains in the as-hydrogenated sample coalesced into well-defined cracks, mostly parallel to the wafer surface.

  9. Study of surface reaction of spinel Li4Ti5O12 during the first lithium insertion and extraction processes using atomic force microscopy and analytical transmission electron microscopy.

    Science.gov (United States)

    Kitta, Mitsunori; Akita, Tomoki; Maeda, Yasushi; Kohyama, Masanori

    2012-08-21

    Spinel lithium titanate (Li(4)Ti(5)O(12), LTO) is a promising anode material for a lithium ion battery because of its excellent properties such as high rate charge-discharge capability and life cycle stability, which were understood from the viewpoint of bulk properties such as small lattice volume changes by lithium insertion. However, the detailed surface reaction of lithium insertion and extraction has not yet been studied despite its importance to understand the mechanism of an electrochemical reaction. In this paper, we apply both atomic force microscopy (AFM) and transmission electron microscopy (TEM) to investigate the changes in the atomic and electronic structures of the Li(4)Ti(5)O(12) surface during the charge-discharged (lithium insertion and extraction) processes. The AFM observation revealed that irreversible structural changes of an atomically flat Li(4)Ti(5)O(12) surface occurs at the early stage of the first lithium insertion process, which induces the reduction of charge transfer resistance at the electrolyte/Li(4)Ti(5)O(12) interface. The TEM observation clarified that cubic rock-salt crystal layers with a half lattice size of the original spinel structure are epitaxially formed after the first charge-discharge cycle. Electron energy loss spectroscopy (EELS) observation revealed that the formed surface layer should be α-Li(2)TiO(3). Although the transformation of Li(4)Ti(5)O(12) to Li(7)Ti(5)O(12) is well-known as the lithium insertion reaction of the bulk phase, the generation of surface product layers should be inevitable in real charge-discharge processes and may play an effective role in the stable electrode performance as a solid-electrolyte interphase (SEI).

  10. A simple algorithm for measuring particle size distributions on an uneven background from TEM images

    DEFF Research Database (Denmark)

    Gontard, Lionel Cervera; Ozkaya, Dogan; Dunin-Borkowski, Rafal E.

    2011-01-01

    Nanoparticles have a wide range of applications in science and technology. Their sizes are often measured using transmission electron microscopy (TEM) or X-ray diffraction. Here, we describe a simple computer algorithm for measuring particle size distributions from TEM images in the presence of a...... application to images of heterogeneous catalysts is presented.......Nanoparticles have a wide range of applications in science and technology. Their sizes are often measured using transmission electron microscopy (TEM) or X-ray diffraction. Here, we describe a simple computer algorithm for measuring particle size distributions from TEM images in the presence...

  11. Raman and fluorescence microscopy to study the internalization and dissolution of photosensitizer nanoparticles into living cells

    Science.gov (United States)

    Scalfi-Happ, Claudia; Steiner, Rudolf; Wittig, Rainer; Graefe, Susanna; Ryabova, Anastasia; Loschenov, Victor

    2015-07-01

    In this present study we applied Raman and fluorescence microscopy to investigate the internalisation, cellular distribution and effects on cell metabolism of photosensitizer nanoparticles for photodynamic therapy in fibroblasts and macrophages.

  12. Study of planar defects associated to martensite transformation in copper alloys by transmission electron microscopy

    International Nuclear Information System (INIS)

    Condo, A.M.

    1997-01-01

    In this work the planar faults in non-compact planes (non-basal faults) in the 2H and 18R martensitic phases in Cu-Zn-Al alloys are analyzed. The study was carried out using transmission electron microscopy (TEM) combining the two-beam condition technique, high resolution transmission electron microscopy (HRTEM) and computer simulated images. The displacement vectors of the faults were determined. It was found that these vectors were different from those of the basal faults, even though the faults are connected. One single class of non-basal faults, named F 1 , was observed in the 2H phase, whereas two different classes were found in the 18R phase, named F o and F x . In the latter phase non-basal faults made up of different segments of F o and F x faults were observed (composed faults). The Burgers vectors of the partial dislocations at the edges of the non-basal faults were determined in both phases. Additionally, the Burgers vectors of the intermediate dislocations found between the different segments of the composed faults in the 18R phase were determined. It was verified that there exist two types of dislocations with Burgers vectors that differ in approximately 1/3 [100]. It was found that the presence of a particular dislocation type depends on the arrangement between the non-basal fault and the basal fault that originates the dislocation. The internal structure of the non-basal faults in the 18R phase was studied with HRTEM. It was observed that the shift of the crystal planes due to the presence of the faults occurs in a region of a finite extension of about 1.5 nm. It was also observed that in this region the crystal planes appear rotated and lose the characteristic corrugation they have in the 18R structure. As a consequence of this, new translation vectors appear in the defect; this fact could be reflected in new plastic deformation systems. The rotation of the crystal planes in the non-basal faulted area of the 18R phase was compared with the rotation

  13. On the annealing behaviour of dysprosium ion implanted nickel: a combined study using Rutherford backscattering, transmission electron microscopy, and total current spectroscopy

    International Nuclear Information System (INIS)

    Chadderton, L.T.; Johnson, E.

    1977-01-01

    Despite continuing improvements in applications of the analytical method of Rutherford backscattering (RBS) to solid state physics it is recognized that more complete information can be obtained if other techniques - for example transmission electron microscopy (TEM) - are employed simultaneously. Experiments are described in which a combined RBS and TEM study of the annealing of nickel, rendered amorphous by implantation of 20 keV dysprosium ions is supplemented with a completely new technique - total current spectroscopy (TCS). In TCS low energy electrons (0-15 eV) are used to probe the damaged nickel. Observations have been made during annealing of both the reappearance of the bulk band structure of the metal and of a 'surface peak' which is highly sensitive to the recovery process. Changes in the height of the surface peak reveal three sharp annealing stages, the first two being preceded by reverse annealing which correlates well with RBS and TEM results. The first annealing stage - following the amorphous to crystalline transition - may be associated with electronic effects in the vicinity of the Curie point. Changes in the position of the surface peak allow one to trace the diffusion of dysprosium to the surface. Quantum mechanical resonances at the damage/crystal interface have also been followed throughout annealing. The initially amorphous layer (approximately 2.2nm) increases in thickness slightly during recovery. (Auth.)

  14. Quantitative in situ magnetization reversal studies in Lorentz microscopy and electron holography

    International Nuclear Information System (INIS)

    Rodríguez, L.A.; Magén, C.; Snoeck, E.; Gatel, C.; Marín, L.; Serrano-Ramón, L.

    2013-01-01

    A generalized procedure for the in situ application of magnetic fields by means of the excitation of the objective lens for magnetic imaging experiments in Lorentz microscopy and electron holography is quantitatively described. A protocol for applying magnetic fields with arbitrary in-plane magnitude and orientation is presented, and a freeware script for Digital Micrograph ™ is provided to assist the operation of the microscope. Moreover, a method to accurately reconstruct hysteresis loops is detailed. We show that the out-of-plane component of the magnetic field cannot be always neglected when performing quantitative measurements of the local magnetization. Several examples are shown to demonstrate the accuracy and functionality of the methods. - Highlights: • Generalized procedure for application of magnetic fields with the TEM objective lens. • Arbitrary in-plane magnetic field magnitude and orientation can be applied. • Method to accurately reconstruct hysteresis loops by electron holography. • Out-of-plane field component should be considered in quantitative measurements. • Examples to illustrate the method in Lorentz microscopy and electron holography

  15. Analysis of incomplete excisions of basal-cell carcinomas after breadloaf microscopy compared with 3D-microscopy: a prospective randomized and blinded study.

    Science.gov (United States)

    Boehringer, Alexandra; Adam, Patrick; Schnabl, Saskia; Häfner, Hans-Martin; Breuninger, Helmut

    2015-08-01

    Basal-cell carcinomas may show irregular, asymmetric subclinical growth. This study analyzed the efficacy of 'breadloaf' microscopy (serial sectioning) and three-dimensional (3D) microscopy in detecting positive tumor margins. Two hundred eighty-three (283) tumors (51.2%) were put into the breadloaf microscopy group; 270 tumors (48.8%) into the 3D microscopy group. The position of any detected tumor outgrowths was identified in clock face fashion. The time required for cutting and embedding the specimens and the examination of the microscopic slides was measured. Patient/tumor characteristics and surgical margins did not differ significantly. Tumor outgrowths at the excision margin were found in 62 of 283 cases (21.9%) in the breadloaf microscopy group and in 115 of 270 cases (42.6%) in the 3D microscopy group, constituting a highly significant difference (p < 0.001). This difference held true with incomplete excision of fibrosing (infiltrative/sclerosing/morpheaform) tumors [32.9% in the breadloaf microscopy group and 57.5% in the 3D microscopy group (p = 0.003)] and also with solid (nodular) tumors [16.1 and 34.2%, respectively (p < 0.001)]. The mean overall examination time required showed no important difference. In summary, for detection of tumor outgrowths, 3D microscopy has almost twice the sensitivity of breadloaf microscopy, particularly in the situation of aggressive/infiltrative carcinomas. © 2015 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

  16. A high-resolution analytical scanning transmission electron microscopy study of the early stages of spinodal decomposition in binary Fe–Cr

    International Nuclear Information System (INIS)

    Westraadt, J.E.; Olivier, E.J.; Neethling, J.H.; Hedström, P.; Odqvist, J.; Xu, X.; Steuwer, A.

    2015-01-01

    Spinodal decomposition (SD) is an important phenomenon in materials science and engineering. For example, it is considered to be responsible for the 475 °C embrittlement of stainless steels comprising the bcc (ferrite) or bct (martensite) phases. Structural characterization of the evolving minute nano-scale concentration fluctuations during SD in the Fe–Cr system is, however, a notable challenge, and has mainly been considered accessible via atom probe tomography (APT) and small-angle neutron scattering. The standard tool for nanostructure characterization, viz. transmission electron microscopy (TEM), has only been successfully applied to late stages of SD when embrittlement is already severe. However, we here demonstrate that the structural evolution in the early stages of SD in binary Fe–Cr, and alloys based on the binary, are accessible via analytical scanning TEM. An Fe–36 wt% Cr alloy aged at 500 °C for 1, 10 and 100 h is investigated using an aberration-corrected microscope and it is found that highly coherent and interconnected Cr-rich regions develop. The wavelength of decomposition is rather insensitive to the sample thickness and it is quantified to 2, 3 and 6 nm after ageing for 1, 10 and 100 h, which is in reasonable agreement with prior APT analysis. The concentration amplitude is more sensitive to the sample thickness and acquisition parameters but the TEM analysis is in good agreement with APT analysis for the longest ageing time. These findings open up for combinatorial TEM studies where both local crystallography and chemistry is required. - Highlights: • STEM-EELS analysis was successfully applied to resolve early stage SD in Fe–Cr. • Compositional wavelength measured with STEM-EELS compares well to previous ATP studies. • Compositional amplitude measured with STEM-EELS is a function of experimental parameters. • STEM-EELS allows for combinatorial studies of SD using complementary techniques.

  17. A high-resolution analytical scanning transmission electron microscopy study of the early stages of spinodal decomposition in binary Fe–Cr

    Energy Technology Data Exchange (ETDEWEB)

    Westraadt, J.E., E-mail: johan.westraadt@nmmu.ac.za [Centre for High Resolution TEM, Nelson Mandela Metropolitan University, University Way, Port Elizabeth 6031 (South Africa); Olivier, E.J.; Neethling, J.H. [Centre for High Resolution TEM, Nelson Mandela Metropolitan University, University Way, Port Elizabeth 6031 (South Africa); Hedström, P.; Odqvist, J.; Xu, X. [Dept. Materials Science and Engineering, KTH Royal Institute of Technology, Brinellvägen 23, 10044 Stockholm (Sweden); Steuwer, A. [Nelson Mandela Metropolitan University, Gardham Av., Port Elizabeth 6031 (South Africa)

    2015-11-15

    Spinodal decomposition (SD) is an important phenomenon in materials science and engineering. For example, it is considered to be responsible for the 475 °C embrittlement of stainless steels comprising the bcc (ferrite) or bct (martensite) phases. Structural characterization of the evolving minute nano-scale concentration fluctuations during SD in the Fe–Cr system is, however, a notable challenge, and has mainly been considered accessible via atom probe tomography (APT) and small-angle neutron scattering. The standard tool for nanostructure characterization, viz. transmission electron microscopy (TEM), has only been successfully applied to late stages of SD when embrittlement is already severe. However, we here demonstrate that the structural evolution in the early stages of SD in binary Fe–Cr, and alloys based on the binary, are accessible via analytical scanning TEM. An Fe–36 wt% Cr alloy aged at 500 °C for 1, 10 and 100 h is investigated using an aberration-corrected microscope and it is found that highly coherent and interconnected Cr-rich regions develop. The wavelength of decomposition is rather insensitive to the sample thickness and it is quantified to 2, 3 and 6 nm after ageing for 1, 10 and 100 h, which is in reasonable agreement with prior APT analysis. The concentration amplitude is more sensitive to the sample thickness and acquisition parameters but the TEM analysis is in good agreement with APT analysis for the longest ageing time. These findings open up for combinatorial TEM studies where both local crystallography and chemistry is required. - Highlights: • STEM-EELS analysis was successfully applied to resolve early stage SD in Fe–Cr. • Compositional wavelength measured with STEM-EELS compares well to previous ATP studies. • Compositional amplitude measured with STEM-EELS is a function of experimental parameters. • STEM-EELS allows for combinatorial studies of SD using complementary techniques.

  18. Analysis of Fractured Teeth Utilizing Digital Microscopy: A Pilot Study

    Science.gov (United States)

    2016-06-01

    pathology (8). Artifacts such as beam hardening, streaking and cupping may limit the clinician’s ability to detect fractures (9). Metallic structures...visualization of a pathologic condition in the area of diagnostic interest (9). There have been multiple studies published which measure the size of...Heimel P, Metscher B. Volume analysis of heat-induced cracks in human molars: A preliminary study. J Forensic Dent Sci 2014;6:139-44. 13. Hunter J

  19. Transmission Electron Microscopy of Single Wall Carbon Nanotube/Polymer Nanocomposites: A First-Principles Study

    Science.gov (United States)

    Sola, Francisco; Xia, Zhenhai; Lebrion-Colon, Marisabel; Meador, Michael A.

    2012-01-01

    The physics of HRTEM image formation and electron diffraction of SWCNT in a polymer matrix were investigated theoretically on the basis of the multislice method, and the optics of a FEG Super TWIN Philips CM 200 TEM operated at 80 kV. The effect of nanocomposite thickness on both image contrast and typical electron diffraction reflections of nanofillers were explored. The implications of the results on the experimental applicability to study dispersion, chirality and diameter of nanofillers are discussed.

  20. Scanning electron microscopy and transmission electron microscopy study of hot-deformed gamma-TiAl-based alloy microstructure.

    Science.gov (United States)

    Chrapoński, J; Rodak, K

    2006-09-01

    The aim of this work was to assess the changes in the microstructure of hot-deformed specimens made of alloys containing 46-50 at.% Al, 2 at.% Cr and 2 at.% Nb (and alloying additions such as carbon and boron) with the aid of scanning electron microscopy and transmission electron microscopy techniques. After homogenization and heat treatment performed in order to make diverse lamellae thickness, the specimens were compressed at 1000 degrees C. Transmission electron microscopy examinations of specimens after the compression test revealed the presence of heavily deformed areas with a high density of dislocation. Deformation twins were also observed. Dynamically recrystallized grains were revealed. For alloys no. 2 and no. 3, the recovery and recrystallization processes were more extensive than for alloy no. 1.

  1. Annealing temperature and environment effects on ZnO nanocrystals embedded in SiO2: a photoluminescence and TEM study.

    Science.gov (United States)

    Pita, Kantisara; Baudin, Pierre; Vu, Quang Vinh; Aad, Roy; Couteau, Christophe; Lérondel, Gilles

    2013-12-06

    We report on efficient ZnO nanocrystal (ZnO-NC) emission in the near-UV region. We show that luminescence from ZnO nanocrystals embedded in a SiO2 matrix can vary significantly as a function of the annealing temperature from 450°C to 700°C. We manage to correlate the emission of the ZnO nanocrystals embedded in SiO2 thin films with transmission electron microscopy images in order to optimize the fabrication process. Emission can be explained using two main contributions, near-band-edge emission (UV range) and defect-related emissions (visible). Both contributions over 500°C are found to be size dependent in intensity due to a decrease of the absorption cross section. For the smallest-size nanocrystals, UV emission can only be accounted for using a blueshifted UV contribution as compared to the ZnO band gap. In order to further optimize the emission properties, we have studied different annealing atmospheres under oxygen and under argon gas. We conclude that a softer annealing temperature at 450°C but with longer annealing time under oxygen is the most preferable scenario in order to improve near-UV emission of the ZnO nanocrystals embedded in an SiO2 matrix.

  2. Cellulose fibril aggregation studies of eucalyptus dissolving pulps using atomic force microscopy

    CSIR Research Space (South Africa)

    Chunilall, Viren

    2006-11-01

    Full Text Available STUDIES OF Eucalyptus DISSOLVING PULPS USING ATOMIC FORCE MICROSCOPY V. Chunilall1, J.Wesley-Smith2, T. Bush1 1CSIR, Forestry and Forest Product Research Centre, P.O. Box 17001, Congella, 4013, South Africa. 2Electron Microscope Unit, University of Kwa... pulp using atomic force microscopy (AFM) have reported increased cellulose fibril aggregation during processing, and a concomitant decrease in surface area available for chemical reaction1,2. These findings were subsequently confirmed...

  3. The endolymphatic sac: a scanning and transmission electron microscopy study

    DEFF Research Database (Denmark)

    Qvortrup, Klaus; Bretlau, Poul

    2002-01-01

    A recent investigation has suggested that the chief cells of the endolymphatic sac produce an endogenous inhibitor of sodium resorption in the kidneys, tentatively named saccin. In the current study, the ultrastructure of the endolymphatic sac and in particular the chief cells are described...... to demonstrate that this organ fulfils the morphological criteria of a potential endocrine gland. Accordingly, the chief cells are shown to exhibit all the organelles and characteristics of cells that simultaneously synthesize, secrete, absorb and digest proteins....

  4. Study of Adhesion Interaction Using Atomic Force Microscopy

    Science.gov (United States)

    Grybos, J.; Pyka-Fosciak, G.; Lebed, K.; Lekka, M.; Stachura, Z.; Styczeñ, J.

    2003-05-01

    An atomic force microscope is a useful tool to study the interaction forces at molecular level. In particular the atomic force microscope can measure an unbinding force needed to separate the two single molecule complexes. Recent studies have shown that such unbinding force depends linearly on the logarithm of the applied loading rate, defined as a product of scanning velocity and the spring constant characterizing the investigated system (cantilever vs. surface). This dependence can be used to study the energy landscape shape of a molecular complex by the estimation of energy barrier locations and the related dissociation rates. In the present work the complex consisting of ethylene(di)aminetetraacetic acid and the bovine serum albumin was measured. The dependence between the unbinding force and the logarithm of the loading rate was linear. Using the Bell model describing the dissociation of the above molecules caused by the action of the external bond breaking force, two parameters were estimated: the dissociation rate and the position of the energy barrier needed to overcome during a transition from a bound to unbound state. The obtained results are similar to those obtained for a typical ligand--receptor interaction.

  5. Characterization of the system MoS{sub 2} + C, HAADF vs Tem conventional; Cracterizacion del sistema MoS{sub 2} + C, HAADF vs TEM convencional

    Energy Technology Data Exchange (ETDEWEB)

    Reza, C; Cruz, G [ININ, 52045 Ocoyoacac, Estado de Mexico (Mexico); Santiago, P; Rendon, L [IFUNAM, A.P. 20-364, 04510 Mexico D.F. (Mexico)

    2004-07-01

    A study is presented about the synthesis and characterization of unidimensional nano systems composed of MoS{sub 2} and C with potential use as solid lubricant. The synthesis process was developed for the mold method, via thermal decomposition, which uses a film of nano porous aluminium oxide. Such systems were characterized by two analysis methods that involve Transmission Electron Microscopy, HRTEM (Conventional TEM) and HAADF (Z Contrast). The results obtained in the structural and morphological characterization were supplemented to determine the structure type obtained in the unidimensional systems. (Author)

  6. Study of single-electron excitations by electron microscopy

    International Nuclear Information System (INIS)

    Craven, A.J.; Gibson, J.M.; Howie, A.; Spalding, D.R.

    1978-01-01

    The inelastic scattering of fast electrons by the excitation of L-shell electrons at a stacking fault in silicon has been studied with a scanning transmission electron microscope. It was found that the bright-field stacking fault contrast is preserved in the filtered L-shell-loss signal at 100 eV. This result is discussed in terms of the delocalization of the excitation mechanism. It is concluded that localization effects will typically become significant only for energy transfers greater than 1 keV from a fast electron of energy 80 keV. (author)

  7. Simulation study of secondary electron images in scanning ion microscopy

    CERN Document Server

    Ohya, K

    2003-01-01

    The target atomic number, Z sub 2 , dependence of secondary electron yield is simulated by applying a Monte Carlo code for 17 species of metals bombarded by Ga ions and electrons in order to study the contrast difference between scanning ion microscopes (SIM) and scanning electron microscopes (SEM). In addition to the remarkable reversal of the Z sub 2 dependence between the Ga ion and electron bombardment, a fine structure, which is correlated to the density of the conduction band electrons in the metal, is calculated for both. The brightness changes of the secondary electron images in SIM and SEM are simulated using Au and Al surfaces adjacent to each other. The results indicate that the image contrast in SIM is much more sensitive to the material species and is clearer than that for SEM. The origin of the difference between SIM and SEM comes from the difference in the lateral distribution of secondary electrons excited within the escape depth.

  8. Contribution of scanning Auger microscopy to electron beam damage study

    International Nuclear Information System (INIS)

    Fontaine, J.M.

    1983-04-01

    Electron bombardment can produce surface modifications of the analysed sample. The electron beam effects on solid surfaces which have been discussed in the published literature can be classified into the following four categories: (1) heating and its consequent effects, (2) charge accumulation in insulators and its consequent effects, (3) electron stimulated adsorption (ESA), and (4) electron stimulated desorption and/or decomposition (ESD). In order to understand the physico-chemical processes which take place under electron irradiation in an Al-O system, we have carried out experiments in which, effects, such as heating, charging and gas contamination, were absent. Our results point out the role of an enhanced surface diffusion of oxygen during electron bombardment of an Al (111) sample. The importance of this phenomenon and the contribution of near-elastic scattering of the primary electrons (5 keV) to the increase of the oxidation degree observed on Al (111) are discussed, compared to the generally studied effects

  9. Electron microscopy studies of activation mechanisms in hydrotreating catalysis

    DEFF Research Database (Denmark)

    Dahl-Petersen, Christian

    The aim of this work is to remedy the limited fundamental insight that exists in terms of the activation and formation of hydrotreating catalysts utilized in industrial oil refining of crude oil. This is done through numerous studies of the conversion of industrially relevant molybdenum oxide...... larger amount of formed MoS2. MoS2 forms in one of two conformations of the two-dimensional atomic structure that is either in an orientation parallel or perpendicular to the nanoparticle surface. Both the initial growth of MoS2 and the subsequent formation of multi-layered structures is addressed....... This shows that initial growth tends to form an apparent bond between the MoO2 surface and the MoS2 edge and that the layer size increases through coalescence. For multi-layered structures, it is found that MoS2 layers grow through a layer-under-layer mechanism, where defects in the outer layers enable...

  10. Application of transmission electron microscopy for microstructural characterization of perfluoropentacene thin films

    International Nuclear Information System (INIS)

    Haas, Benedikt; Beyer, Andreas; Witte, Wiebke; Breuer, Tobias; Witte, Gregor; Volz, Kerstin

    2011-01-01

    The crystalline structure and orientation of perfluoropentacene (C 22 F 14 , PFP) fibers formed upon thin-film deposition onto SiO 2 substrates have been studied by means of transmission electron microscopy (TEM), atomic force microscopy (AFM), and x-ray diffraction. The synopsis of TEM micrographs and diffraction patterns enhances the understanding of local crystal orientation on small length scales. The relationship of the PFP fiber morphology with the crystalline arrangement of PFP molecules within single fibers was established using this technique. Radiation damage, which is a critical problem for TEM investigations of organic materials, is described and the sample morphology after TEM investigations is correlated with AFM measurements of samples previously examined by TEM.

  11. GISAXS modelling of helium-induced nano-bubble formation in tungsten and comparison with TEM

    International Nuclear Information System (INIS)

    Thompson, Matt; Sakamoto, Ryuichi; Bernard, Elodie; Kirby, Nigel; Kluth, Patrick; Riley, Daniel; Corr, Cormac

    2016-01-01

    Grazing-incidence small angle x-ray scattering (GISAXS) is a powerful non-destructive technique for the measurement of nano-bubble formation in tungsten under helium plasma exposure. Here, we present a comparative study between transmission electron microscopy (TEM) and GISAXS measurements of nano-bubble formation in tungsten exposed to helium plasma in the Large Helical Device (LHD) fusion experiment. Both techniques are in excellent agreement, suggesting that nano-bubbles range from spheroidal to ellipsoidal, displaying exponential diameter distributions with mean diameters μ=0.68 ± 0.04 nm and μ=0.6 ± 0.1 nm measured by TEM and GISAXS respectively. Depth distributions were also computed, with calculated exponential depth distributions with mean depths of 8.4 ± 0.5 nm and 9.1 ± 0.4 nm for TEM and GISAXS. In GISAXS modelling, spheroidal particles were fitted with an aspect ratio ε=0.7 ± 0.1. The GISAXS model used is described in detail. - Highlights: • GISAXS and TEM were used to measure nano-bubble formation in W exposed to He plasma in the large helical device. • Nano-bubbles had an exponential diameter distributions with averages 0.6 ± 0.1 nm and 0.68 ± 0.04 nm measured by GISAXS and TEM. • Nano-bubbles had an exponential depth distributions with average depths of 9.1 ± 0.4 nm and 8.4 ± 0.5 nm for GISAXS and TEM. • The GISAXS model used to analyse diffraction patterns is explained in detail.

  12. GISAXS modelling of helium-induced nano-bubble formation in tungsten and comparison with TEM

    Energy Technology Data Exchange (ETDEWEB)

    Thompson, Matt, E-mail: matt.a.thompson@anu.edu.au [Research School of Physics and Engineering, Australian National University, Mills Road, Acton, ACT 2601 (Australia); Sakamoto, Ryuichi [National Institute for Fusion Science, Toki, Gifu 509-5292 (Japan); Bernard, Elodie [Aix-Marseille University, Marseille 13288 (France); Kirby, Nigel [SAXS/WAXS Beamline, Australian Synchrotron, 800 Blackburn Rd, Clayton, VIC, 3168 (Australia); Kluth, Patrick [Research School of Physics and Engineering, Australian National University, Mills Road, Acton, ACT 2601 (Australia); Riley, Daniel [Australian Nuclear Science and Technology Organisation, Locked Bag 2001, Kirrawee DC, NSW, 2232 (Australia); Corr, Cormac [Research School of Physics and Engineering, Australian National University, Mills Road, Acton, ACT 2601 (Australia)

    2016-05-15

    Grazing-incidence small angle x-ray scattering (GISAXS) is a powerful non-destructive technique for the measurement of nano-bubble formation in tungsten under helium plasma exposure. Here, we present a comparative study between transmission electron microscopy (TEM) and GISAXS measurements of nano-bubble formation in tungsten exposed to helium plasma in the Large Helical Device (LHD) fusion experiment. Both techniques are in excellent agreement, suggesting that nano-bubbles range from spheroidal to ellipsoidal, displaying exponential diameter distributions with mean diameters μ=0.68 ± 0.04 nm and μ=0.6 ± 0.1 nm measured by TEM and GISAXS respectively. Depth distributions were also computed, with calculated exponential depth distributions with mean depths of 8.4 ± 0.5 nm and 9.1 ± 0.4 nm for TEM and GISAXS. In GISAXS modelling, spheroidal particles were fitted with an aspect ratio ε=0.7 ± 0.1. The GISAXS model used is described in detail. - Highlights: • GISAXS and TEM were used to measure nano-bubble formation in W exposed to He plasma in the large helical device. • Nano-bubbles had an exponential diameter distributions with averages 0.6 ± 0.1 nm and 0.68 ± 0.04 nm measured by GISAXS and TEM. • Nano-bubbles had an exponential depth distributions with average depths of 9.1 ± 0.4 nm and 8.4 ± 0.5 nm for GISAXS and TEM. • The GISAXS model used to analyse diffraction patterns is explained in detail.

  13. Illuminating Electron Microscopy of Photocatalysts

    DEFF Research Database (Denmark)

    Cavalca, Filippo

    .1% of the surface of the planet with a device that converts solar energy into a useable form at 10% efficiency would give more than the present worldwide consumption of fossil energy. Photocatalysts are of fundamental interest for sustainable energy research because they provide a viable route for converting solar...... energy into chemical bonds. By means of Transmission Electron Microscopy (TEM) it is possible to gain insight in the fundamentals of their reaction mechanisms, chemical behaviour, structure and morphology before, during and after reaction using in situ investigations. In particular, the environmental TEM...... the microscope that allows electron microscopy under nonconventional TEM conditions and new kinds of in situ spectroscopy....

  14. Three dimensional transient electromagnetic model study for fracture prediction from tunnel face; Sanjigen model keisan ni yoru TEM ho no tunnel zenpo tansa eno tekiyosei no kento

    Energy Technology Data Exchange (ETDEWEB)

    Wada, K; Tsutsui, T; Saito, A [Mitsui Mineral Development Engineering Co. Ltd., Tokyo (Japan); Hara, T [Toda Corp., Tokyo, (Japan); Zhdanov, M [University of Utah, UT (United States)

    1996-10-01

    In order to apply TEM model to fracture prediction at tunnel face, 3-D TEM model computation by FEM was conducted by installing a transmission loop on a tunnel face. MT field responses diffusing into the 3-D model were computed by time-domain difference calculus, and analytical precision was improved by introducing a staggered grid method. In the case where a low resistive zone exists before a tunnel face, time variance in diffused eddy current and induction current in the low resistive zone could be obtained. The difference in tunnel-axial transient curve (transient phenomenon curve in magnetic field) between uniform medium and low resistive zone models was based on the absorption process of diffused eddy current into the low resistive zone, and the expanding process of it toward the outside. Change in background condition could be predicted from the background and the ratio of transient curves every measurement. The detection limit of the low resistive zone was dependent on resistivity contrast, distance and geometry. Fluctuation in measurement due to noises and S/N ratio were also essential. 3 refs., 10 figs.

  15. TEM study of structural and microstructural characteristics of a precipitate phase in Ni-rich Ni–Ti–Hf and Ni–Ti–Zr shape memory alloys

    International Nuclear Information System (INIS)

    Santamarta, R.; Arróyave, R.; Pons, J.; Evirgen, A.; Karaman, I.; Karaca, H.E.; Noebe, R.D.

    2013-01-01

    The precipitates formed after suitable thermal treatments in seven Ni-rich Ni–Ti–Hf and Ni–Ti–Zr high-temperature shape memory alloys have been investigated by conventional and high-resolution transmission electron microscopy. In both ternary systems, the precipitate coarsening kinetics become faster as the Ni and ternary element contents (Hf or Zr) of the bulk alloy are increased, in agreement with the precipitate composition measured by energy-dispersive X-ray microanalysis. The precipitate structure has been found to be the same in both Hf- and Zr-containing ternary alloys, and determined to be a superstructure of the B2 austenite phase, which arises from a recombination of the Hf/Zr and Ti atoms in their sublattice. Two different structural models for the precipitate phase were optimized using density functional theory methods. These calculations indicate that the energetics of the structure are not very sensitive to the atomic configuration of the Ti–Hf/Zr planes, thus significant configurational disorder due to entropic effects can be envisaged at high temperatures. The precipitates are fully coherent with the austenite B2 matrix; however, upon martensitic transformation, they lose some coherency with the B19′ matrix as a result of the transformation shear process in the surrounding matrix. The strain accommodation around the particles is much easier in the Ni–Ti–Zr-containing alloys than in the Ni–Ti–Hf system, which correlates well with the lower transformation strain and stiffness predicted for the Ni–Ti–Zr alloys. The B19′ martensite twinning modes observed in the studied Ni-rich ternary alloys are not changed by the new precipitated phase, being equivalent to those previously reported in Ni-poor ternary alloys

  16. Transmission electron microscopy study of precipitates in an artificially aged Al–12.7Si–0.7Mg alloy

    International Nuclear Information System (INIS)

    Liu, Fang; Yu, Fuxiao; Zhao, Dazhi; Zuo, Liang

    2015-01-01

    An investigation of Al–12.7Si–0.7Mg alloy aged at 160 °C, 180 °C and 200 °C for 3 h was carried out in order to identify the precipitating phases. Regular transmission and high resolution electron microscopy (TEM and HREM) were employed for this purpose. The studies were focused on the dark spots and needle-shaped precipitates lying in (001) Al plane. Based on the HREM observations, dark spots and needle-shaped precipitates have different characteristics. The results revealed that the ellipsoidal and needle-shaped precipitates along <100> direction of the matrix coexist in the alloy by tilting experiments at given aging condition. The ellipsoidal dark spot precipitates viewing along [001] Al is not cross-sectional image of needle-shaped precipitates along <001> Al . Needle-shaped precipitate is coherent with the matrix. The diffraction pattern associated with the ellipsoidal precipitates is consistent with β″ reported in literature. - Highlights: • Wrought Al–Si–Mg alloy has been investigated to identify the precipitating phases. • The ellipsoidal and needle-shaped precipitates coexist in wrought Al–Si–Mg alloy. • The needle-shaped and ellipsoidal precipitates exhibit different characteristics

  17. Oxidation in ceria infiltrated metal supported SOFCs – A TEM investigation

    DEFF Research Database (Denmark)

    Knibbe, Ruth; Wang, Hsiang-Jen; Blennow Tullmar, Peter

    2013-01-01

    electron microscopy (TEM) techniques including energy-dispersive X-ray spectroscopy and electron energy-loss spectroscopy of focus ion beamed TEM samples. The infiltrated CGO is predominately converted into CeFeO3 after high temperature processing, protecting the alloy. A thin layer of Cr-oxide is observed...

  18. A flexible multi-stimuli in situ (S)TEM: Concept, optical performance, and outlook

    International Nuclear Information System (INIS)

    Börrnert, Felix; Müller, Heiko; Riedel, Thomas; Linck, Martin; Kirkland, Angus I.; Haider, Max.; Büchner, Bernd; Lichte, Hannes

    2015-01-01

    The progress in (scanning) transmission electron microscopy development had led to an unprecedented knowledge of the microscopic structure of functional materials at the atomic level. Additionally, although not widely used yet, electron holography is capable to map the electric and magnetic potential distributions at the sub-nanometer scale. Nevertheless, in situ studies inside a (scanning) transmission electron microscope ((S)TEM) are extremely challenging because of the much restricted size and accessibility of the sample space. Here, we introduce a concept for a dedicated in situ (S)TEM with a large sample chamber for flexible multi-stimuli experimental setups and report about the electron optical performance of the instrument. We demonstrate a maximum resolving power of about 1 nm in conventional imaging mode and substantially better than 5 nm in scanning mode while providing an effectively usable “pole piece gap” of 70 mm. - Highlights: • A concept for a (S)TEM with a large sample chamber is outlined. • An actual microscope is modified and has now a 70 mm high sample space. • The resolving power is about 1 nm in TEM and better than 5 nm in STEM mode. • Possible dedicated in situ microscopes with present technology are discussed

  19. Soft nanomaterials analysed by in situ liquid TEM: Towards high resolution characterisation of nanoparticles in motion

    Directory of Open Access Journals (Sweden)

    Joseph P. Patterson

    2015-12-01

    Full Text Available In this article we present in situ transmission electron microscopy (TEM of soft, synthetic nanoparticles with a comparative analysis using conventional TEM methods. This comparison is made with the simple aim of describing what is an unprecedented example of in situ imaging by TEM. However, we contend the technique will quickly become essential in the characterisation of analogous systems, especially where dynamics are of interest in the solvated state. In this case, particles were studied which were obtained from the direct polymerisation of an oxaliplatin analogue, designed for an ongoing programme in novel chemotherapeutic delivery systems. The resulting nanoparticles provided sufficient contrast for facile imaging in situ, and point towards key design parameters that enable this new characterisation approach for organic nanomaterials. We describe the preparation of the synthetic nanoparticles together with their characterisation in liquid water. Finally, we provide a future perspective of this technique for the analysis of soft and dynamic nanomaterials and discussion the progress which needs to be made in order to bring in situ liquid TEM to its full potential.

  20. A flexible multi-stimuli in situ (S)TEM: Concept, optical performance, and outlook

    Energy Technology Data Exchange (ETDEWEB)

    Börrnert, Felix, E-mail: felix.boerrnert@triebenberg.de [Speziallabor Triebenberg, Technische Universität Dresden, 01062 Dresden (Germany); IFW Dresden, PF 27 01 16, 01171 Dresden (Germany); Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH (United Kingdom); Müller, Heiko; Riedel, Thomas; Linck, Martin [CEOS GmbH, Englerstraße 28, 69126 Heidelberg (Germany); Kirkland, Angus I. [Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH (United Kingdom); Haider, Max. [CEOS GmbH, Englerstraße 28, 69126 Heidelberg (Germany); Büchner, Bernd [IFW Dresden, PF 27 01 16, 01171 Dresden (Germany); Lichte, Hannes [Speziallabor Triebenberg, Technische Universität Dresden, 01062 Dresden (Germany)

    2015-04-15

    The progress in (scanning) transmission electron microscopy development had led to an unprecedented knowledge of the microscopic structure of functional materials at the atomic level. Additionally, although not widely used yet, electron holography is capable to map the electric and magnetic potential distributions at the sub-nanometer scale. Nevertheless, in situ studies inside a (scanning) transmission electron microscope ((S)TEM) are extremely challenging because of the much restricted size and accessibility of the sample space. Here, we introduce a concept for a dedicated in situ (S)TEM with a large sample chamber for flexible multi-stimuli experimental setups and report about the electron optical performance of the instrument. We demonstrate a maximum resolving power of about 1 nm in conventional imaging mode and substantially better than 5 nm in scanning mode while providing an effectively usable “pole piece gap” of 70 mm. - Highlights: • A concept for a (S)TEM with a large sample chamber is outlined. • An actual microscope is modified and has now a 70 mm high sample space. • The resolving power is about 1 nm in TEM and better than 5 nm in STEM mode. • Possible dedicated in situ microscopes with present technology are discussed.

  1. Electron microscopy of nanostructured semiconductor materials

    International Nuclear Information System (INIS)

    Neumann, Wolfgang

    2003-01-01

    For various material systems of low dimensions, including multilayers, islands, and quantum dots, the potential applicability of transmission electron microscopy (TEM) is demonstrated. Conventional TEM is applied to elucidate size, shape, and arrangement of nanostructures, whereas high-resolution imaging is used for visualizing their atomic structure. In addition, microchemical peculiarities of the nanoscopic objects are investigated by analytical TEM techniques (energy-filtered TEM, energy-dispersive X-ray spectroscopy)

  2. Gallium Nitride: A Nano scale Study using Electron Microscopy and Associated Techniques

    International Nuclear Information System (INIS)

    Mohammed Benaissa; Vennegues, Philippe

    2008-01-01

    A complete nano scale study on GaN thin films doped with Mg. This study was carried out using TEM and associated techniques such as HREM, CBED, EDX and EELS. It was found that the presence of triangular defects (of few nanometers in size) within GaN:Mg films were at the origin of unexpected electrical and optical behaviors, such as a decrease in the free hole density at high Mg doping. It is shown that these defects are inversion domains limited with inversion-domains boundaries. (author)

  3. Application of TEM to highly reactive metals

    International Nuclear Information System (INIS)

    Sherry, W.M.; Prinz, F.

    1982-01-01

    In the following a method for the preparation and observation of sodium TEM specimens and the first TEM micrograph ever to be published on the dislocation microstructure of sodium are reported. (orig./IHOE) [de

  4. Determining oxygen relaxations at an interface: A comparative study between transmission electron microscopy techniques.

    Science.gov (United States)

    Gauquelin, N; van den Bos, K H W; Béché, A; Krause, F F; Lobato, I; Lazar, S; Rosenauer, A; Van Aert, S; Verbeeck, J

    2017-10-01

    Nowadays, aberration corrected transmission electron microscopy (TEM) is a popular method to characterise nanomaterials at the atomic scale. Here, atomically resolved images of nanomaterials are acquired, where the contrast depends on the illumination, imaging and detector conditions of the microscope. Visualization of light elements is possible when using low angle annular dark field (LAADF) STEM, annular bright field (ABF) STEM, integrated differential phase contrast (iDPC) STEM, negative spherical aberration imaging (NCSI) and imaging STEM (ISTEM). In this work, images of a NdGaO 3 -La 0.67 Sr 0.33 MnO 3 (NGO-LSMO) interface are quantitatively evaluated by using statistical parameter estimation theory. For imaging light elements, all techniques are providing reliable results, while the techniques based on interference contrast, NCSI and ISTEM, are less robust in terms of accuracy for extracting heavy column locations. In term of precision, sample drift and scan distortions mainly limits the STEM based techniques as compared to NCSI. Post processing techniques can, however, partially compensate for this. In order to provide an outlook to the future, simulated images of NGO, in which the unavoidable presence of Poisson noise is taken into account, are used to determine the ultimate precision. In this future counting noise limited scenario, NCSI and ISTEM imaging will provide more precise values as compared to the other techniques, which can be related to the mechanisms behind the image recording. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Magnetic force microscopy and simulation studies on Co 50 Fe 50 ...

    Indian Academy of Sciences (India)

    We studied the magnetization reversal mechanism of single-layered Co50Fe50 nanomagnets by measuring the magnetization reversal and using the micromagnetic simulations. The magnetization reversal strongly depends on the thickness of the nanomagnets. In the remanent state, the magnetic force microscopy studies ...

  6. Studies on the mechanism of replication of adenovirus DNA. III. Electron microscopy of replicating DNA

    NARCIS (Netherlands)

    Ellens, D.J.; Sussenbach, J.S.; Jansz, H.S.

    1974-01-01

    Replicating Ad5 DNA was isolated from nuclei of infected KB cells and studied by electron microscopy. Branched as well as unbranched linear intermediates were observed containing extended regions of single-stranded DNA. The relationship between the branched and unbranched structures was studied

  7. A study on microstructures and extended defects in Ni- and Co-base superalloys. Development and application of advanced TEM techniques

    Energy Technology Data Exchange (ETDEWEB)

    Mueller, Julian

    2016-04-21

    To improve the efficiency of stationary gas turbines and air craft jet engines, it is crucial to increase the maximum temperature capabilities of single crystalline superalloys by appropriate alloy design and microstructure tuning. The mechanical properties of superalloys are largely influenced by the physical constitution of the microstructure. To develop a better understanding of fundamental aspects of creep deformation, like the stress states, defect structures and other degradation processes, it is necessary to employ scale-bridging characterization. In the present work, Ni- and Co-based superalloys are investigated by a series of advanced transmission electron microscopy techniques and by the application of specifically developed characterization methods to identify dominating processes on atomic scale and hence to make a direct correlation to the macroscopic creep behavior. For instance, the misfit between γ and γ' in the initial microstructure is of great importance, since it strongly influences the rafting process and the interfacial dislocation network. To address the stress state, on the one hand misfit measurements in undeformed samples are conducted and are directly compared to finite-element simulations. On the other hand, deformed samples are investigated to assess the influence of an initial rafting process and the formation of an interface dislocation network. For this, characterization methods are used which are based on the evaluation of atomically resolved images and on electron diffraction. Moreover, the temperature dependency of the misfit and of the microstructure stability is specifically investigated for different Co-base alloys in in situ heating experiments. The characterization of defect structures in Ni-base superalloys after creep deformation builds the second pillar of this work. Specific cutting processes of superdislocations are studied to elucidate which atomic processes take place. A series of left angle 100 right angle and

  8. An identical-location transmission electron microscopy study on the degradation of Pt/C nanoparticles under oxidizing, reducing and neutral atmosphere

    International Nuclear Information System (INIS)

    Dubau, L.; Castanheira, L.; Berthomé, G.; Maillard, F.

    2013-01-01

    This study shows that the predominant degradation mechanism of Pt/Vulcan XC72 electrocatalysts strongly depends on the nature of the gas atmosphere and of the upper potential limit used in accelerated stress tests (ASTs). The morphological changes of Pt/Vulcan XC72 nanoparticles were studied by identical location transmission electron microscopy (IL-TEM), following accelerated stress tests in different potential ranges and under various gas atmospheres. X-ray photoelectron spectroscopy was used to probe changes in carbon surface chemistry. Whereas minor changes were detected under neutral atmosphere (Ar) and low potential limit conditions (0.05 2 ). With an increase of the upper potential limit to 1.23 V vs. RHE, the trends observed previously were maintained but 3D Ostwald ripening strongly overlapped with the three other degradation mechanisms, precluding any identification of the dominant mechanism

  9. Vacancy ordered γ-Fe{sub 2}O{sub 3} nanoparticles functionalized with nanohydroxyapatite: XRD, FTIR, TEM, XPS and Mössbauer studies

    Energy Technology Data Exchange (ETDEWEB)

    Ramos Guivar, Juan A., E-mail: juan.ramos5@unmsm.edu.pe [Faculty of Physical Sciences, National University of San Marcos, P. O. Box 14- 0149, Lima 14 (Peru); Sanches, Edgar A., E-mail: sanches.ufam@gmail.com [Federal University of Amazonas, Department of Physics, Manaus/AM (Brazil); Bruns, Florian, E-mail: f.bruns@tu-braunschweig.de [Institut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38110 Braunschweig (Germany); Sadrollahi, Elaheh, E-mail: elahe.sadrollahi@gmail.com [Institut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38110 Braunschweig (Germany); Morales, M.A., E-mail: marco.moralestorres@gmail.com [Department of Theoretical and Experimental Physics, UFRN, Natal, RN 59078- 970 (Brazil); López, Elvis O., E-mail: lopmezel@gmail.com [Brazilian Center for Research in Physics (CBPF), Rio de Janeiro, RJ 22290-180 (Brazil); Litterst, F. Jochen, E-mail: litterst@cbpf.br [Institut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38110 Braunschweig (Germany); Brazilian Center for Research in Physics (CBPF), Rio de Janeiro, RJ 22290-180 (Brazil)

    2016-12-15

    Graphical abstract: Possible bonding configuration in the γ-Fe{sub 2}O{sub 3} nanoparticles functionalized with nanoHAp. - Highlights: • Coprecipitation in alkaline medium for the synthesis of vacancy ordered γ-Fe{sub 2}O{sub 3}@HAp nanocomposite. • Samples were characterized by XRD, FTIR, XPS, TEM, VSM and Mössbauer spectroscopy. • The functionalization is explained with the binding of two oxygens of chemisorbed H{sub 2}O molecules at the common interface of HAp/C{sub 6}H{sub 8}O{sub 7}/γ-Fe{sub 2}O{sub 3}. - Abstract: Vacancy ordered maghemite (γ-Fe{sub 2}O{sub 3}) nanoparticles functionalized with nanohydroxyapatite (HAp – Ca{sub 10}(PO{sub 4}) {sub 6}(OH){sub 2}) have been successfully synthesized using an inexpensive co-precipitation chemical route. Evidence for the presence of vacancy order in maghemite was shown by the superstructure lines observed in X-ray diffraction. The adsorption of carboxyl groups of citric acid (C{sub 6}H{sub 8}O{sub 7}) onto γ-Fe{sub 2}O{sub 3} nanoparticles was investigated by FTIR, XPS and Mössbauer spectroscopy. From XPS surface analysis, two binding energies related to oxygen were attributed to bindings between C{sub 6}H{sub 8}O{sub 7}/γ- Fe{sub 2}O{sub 3} and C{sub 6}H{sub 8}O{sub 7}/HAp from an interfacial reaction promoted by strongly adsorbed H{sub 2}O molecules at the surface of these nanomaterials. Le Bail refinement of the XRD patterns showed the formation of well-crystallized pure tetragonal maghemite before and after functionalization with nanoHAp. The temperature dependence of hyperfine parameters of pure and functionalized γ-Fe{sub 2}O{sub 3} nanoparticles was investigated via Mössbauer spectroscopy. TEM revealed the formation of quasi-spherical γ- Fe{sub 2}O{sub 3} nanoparticles with an average diameter of ca. 12 nm and 16 nm before and after functionalization with nanoHAp in agreement with Le Bail refinement. Magnetometry measurements showed a saturation magnetization of 12 emu/g and a blocking

  10. Electron microscopy study of Nb-rich nanoprecipitates in Ni–Ti–Nb and their influence on the martensitic transformation

    International Nuclear Information System (INIS)

    Shi, H.; Pourbabak, S.; Van Humbeeck, J.; Schryvers, D.

    2012-01-01

    Graphical abstract: -- Nb-rich nanoprecipitates in the matrix of an annealed commercial Ni–Ti–Nb alloy are investigated by scanning and transmission electron microscopy, including slice-and-view and chemical analysis. The precipitates have a diameter of around 100 nm, are faceted and have a cube-on-cube relation with the B2 matrix. In situ TEM cooling shows that the martensitic transformation is hampered by the presence of these precipitates. The latter could explain the increase in hysteresis when compared with the binary system.

  11. TEM and EELS study of deuterated carbon: application to the fuel retention in tokamaks; Etude couplee MET-EELS du carbone deutere: application a la retention du combustible dans les tokamaks

    Energy Technology Data Exchange (ETDEWEB)

    Bernier, N

    2007-12-15

    We developed a methodology, based on the combination of TEM and EELS techniques, for a structural and chemical characterization, at a high spatial resolution, of a wide range of carbon materials. We i) optimized, in the framework of theoretical models, the sp2 fraction quantification from pure carbons by EELS ii) transferred this quantification to deuterated amorphous carbon layers iii) showed, from graphitized carbons, how the TEM-EELS combination allows to detect low concentrations of implanted D. Due to the accomplishment of these developments, we applied our approach to the study of D retention in composites C/C, which are the plasma-facing materials in TS. We showed that specific localized retention sites correspond to relatively large ({approx} 3 mm.) cracks between fibres and matrix; such cracks offer a simple and direct path for deuterated amorphous carbon. The particle balance performed in TS is discussed in the light of this trapping mechanism. (author)

  12. A Combined TEM/STEM and Micromagnetic Study of the Anisotropic Nature of Grain Boundaries and Coercivity in Nd-Fe-B Magnets

    Directory of Open Access Journals (Sweden)

    Gregor A. Zickler

    2017-01-01

    Full Text Available The nanoanalytical high resolution TEM/STEM investigation of the intergranular grain boundary phase of anisotropic sintered and rapidly quenched heavy rare earth-free Nd-Fe-B magnet materials revealed a difference in composition for grain boundaries parallel (large Fe-content and perpendicular (low Fe content to the alignment direction. This behaviour vanishes in magnets with a high degree of misorientation. The numerical finite element micromagnetic simulations are based on the anisotropic compositional behaviour of GBs and show a decrease of the coercive field with an increasing thickness of the grain boundary layer. The magnetization reversal and expansion of reversed magnetic domains primarily start as Bloch domain wall at grain boundaries parallel to the c-axis and secondly as Néel domain wall perpendicular to the c-axis into the adjacent hard magnetic grains. The increasing misalignment of grains leads to the loss of the anisotropic compositional behaviour and therefore to an averaged value of the grain boundary composition. In this case the simulations show an increase of the coercive field compared to the anisotropic magnet. The calculated coercive field values of the investigated magnet samples are in the order of μ0HcJ=1.8 T–2.1 T for a mean grain boundary thickness of 4 nm, which agrees perfectly with the experimental data.

  13. Study of the phase transformation of single particles of Ga2O3 by UV-Raman spectroscopy and high-resolution TEM.

    Science.gov (United States)

    Wang, Xiang; Xu, Qian; Fan, Fengtao; Wang, Xiuli; Li, Mingrun; Feng, Zhaochi; Li, Can

    2013-09-01

    By taking advantage of UV-Raman spectroscopy and high-resolution TEM (HRTEM), combined with the focused ion beam (FIB) technique, the transformation from GaOOH into α-Ga2O3 and then into β-Ga2O3 was followed. We found that the stepwise transformations took place from the surface region before developing into the bulk of single particles without particle agglomeration and growth. During the transformation from GaOOH into α-Ga2O3, the elimination of water vapor through the dehydroxylation of GaOOH resulted in the formation of micropores in the single particles, whilst maintaining their particle size. For the phase transformation from α-Ga2O3 into β-Ga2O3, the nucleation of β-Ga2O3 was found to occur at the surface defects and this process could be retarded by occupying these defects with a small amount of La2O3. By finely controlling the process of the phase transformation, the β-Ga2O3 domains gradually developed from the surface into the bulk of the single particles without particle agglomeration. Therefore, the surface structure of the α-Ga2O3 single particles can be easily tuned and a particle with an α@β core-shell phase structure has been obtained. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Characterization of the system MoS2 + C, HAADF vs Tem conventional

    International Nuclear Information System (INIS)

    Reza, C.; Cruz, G.; Santiago, P.; Rendon, L.

    2004-01-01

    A study is presented about the synthesis and characterization of unidimensional nano systems composed of MoS 2 and C with potential use as solid lubricant. The synthesis process was developed for the mold method, via thermal decomposition, which uses a film of nano porous aluminium oxide. Such systems were characterized by two analysis methods that involve Transmission Electron Microscopy, HRTEM (Conventional TEM) and HAADF (Z Contrast). The results obtained in the structural and morphological characterization were supplemented to determine the structure type obtained in the unidimensional systems. (Author)

  15. Adsorption of Cu phthalocyanine on Pt modified Ge(001): A scanning tunneling microscopy study

    NARCIS (Netherlands)

    Saedi, A.; Berkelaar, Robin P.; Kumar, Avijit; Poelsema, Bene; Zandvliet, Henricus J.W.

    2010-01-01

    The adsorption configurations of copper phthalocyanine (CuPc) molecules on platinum-modified Ge(001) have been studied using scanning tunneling microscopy. After deposition at room temperature and cooling down to 77 K the CuPc molecules are still dynamic. However, after annealing at 550±50 K, the

  16. Studying the Adhesion Force and Glass Transition of Thin Polystyrene Films by Atomic Force Microscopy

    DEFF Research Database (Denmark)

    Kang, Hua; Qian, Xiaoqin; Guan, Li

    2018-01-01

    microscopy (AFM)-based forcedistance curve to study the relaxation dynamics and the film thickness dependence of glass transition temperature (T-g) for normal thin polystyrene (PS) films supported on silicon substrate. The adhesion force (F-ad) between AFM tip and normal thin PS film surfaces...

  17. Transmission Electron Microscopy Studies of Electron-Selective Titanium Oxide Contacts in Silicon Solar Cells

    KAUST Repository

    Ali, Haider; Yang, Xinbo; Weber, Klaus; Schoenfeld, Winston V.; Davis, Kristopher O.

    2017-01-01

    In this study, the cross-section of electron-selective titanium oxide (TiO2) contacts for n-type crystalline silicon solar cells were investigated by transmission electron microscopy. It was revealed that the excellent cell efficiency of 21

  18. Photolithographic Polymerization of Diacetylene-Containing Phospholipid Bilayers Studied by Multimode Atomic Force Microscopy

    NARCIS (Netherlands)

    Morigaki, Kenichi; Schönherr, Holger; Frank, Curtis W.; Knoll, Wolfgang

    2003-01-01

    Photopolymerization of the diacetylene-containing phospholipid 1,2-bis(10,12-tricosadiynoyl)-sn-glycero-3-phosphocholine (1) in substrate-supported planar lipid bilayers (SPBs) has been studied by using multimode atomic force microscopy (AFM). Monolayers and bilayers of 1 have been transferred onto

  19. Transient gels in colloid-polymer mixtures studied with fluorescence confocal scanning laser microscopy

    NARCIS (Netherlands)

    Verhaegh, N.A.M.; Asnaghi, D.; Lekkerkerker, H.N.W.

    1999-01-01

    We study the structure and the time evolution of transient gels formed in colloid-polymer mixtures, by means of uorescence Confocal Scanning Laser Microscopy (CSLM). This technique is used in conjunction with novel colloidal silica particles containing a uorescent core. The confocal micrographs

  20. Accessibility, Structure and Reactivity of Individual Catalyst Particles Studied by Fluorescence Microscopy

    NARCIS (Netherlands)

    Hendriks, F.C.|info:eu-repo/dai/nl/412642697

    2017-01-01

    This PhD thesis is aimed at using fluorescence microscopy to study accessibility, structure and reactivity of two types of systems. The first part of this thesis is focused on model zeolite crystals. Fundamental insights into the accessibility and internal structure of zeolite powders and crystals

  1. Defect imaging and channeling studies using channeling scanning transmission ion microscopy

    NARCIS (Netherlands)

    King, PJC; Breese, MBH; Smulders, PJM; Wilshaw, PR; Grime, GW

    The technique of channeling scanning transmission ion microscopy (CSTIM) can be used to produce images of individual crystal defects (such as dislocations and stacking faults) using the scanned, focused ion beam from a nuclear microprobe. As well as offering a new method for studies of crystal

  2. Quantitative optical microscopy and micromanipulation studies on the lipid bilayer membranes of giant unilamellar vesicles

    DEFF Research Database (Denmark)

    Bagatolli, Luis; Needham, David

    2014-01-01

    to study composition-structure-property materials relationships of free-standing lipid bilayer membranes. Because their size (~5 to 100 m diameter) that is well above the resolution limit of regular light microscopes, GUVs are suitable membrane models for optical microscopy and micromanipulation...

  3. A structural study of solid electrolyte interface on negative electrode of lithium-Ion battery by electron microscopy.

    Science.gov (United States)

    Matsushita, Tadashi; Watanabe, Jiro; Nakao, Tatsuya; Yamashita, Seiichi

    2014-11-01

    For the last decades, the performance of the lithium-ion battery (LIB) has been significantly improved and its applications have been expanding rapidly. However, its performance has yet to be enhanced.In the lithium-ion battery development, it is important to elucidate the electrode structure change in detail during the charge and discharge cycling. In particular, solid electrolyte interface (SEI) formed by decomposition of the electrolytes on the graphite negative electrode surface should play an important role for battery properties. Therefore, it is essential to control the structure and composition of SEI to improve the battery performance. Here, we conducted a scanning electron microscope (SEM) and transmission electron microscope (TEM) study to elucidate the structures of the SEI during the charge and discharge process using LiNi1/3Co1/3Mn1/3O2 [1] cathode and graphite anode. [2] Since SEI is a lithium-containing compound with high activity, it was observed without being exposed to the atmosphere. The electrodes including SEI were sampled after dismantling batteries with cutoff voltages of 3V and 4.2V for the charge process and 3V for the discharge process. Fig.1 shows SEM images of the graphite electrode surface during the charge and discharge process. The change of the SEI structure during the process was clearly observed. Further, TEM images showed that the SEI grew thicker during the charge process and becomes thinner when discharged. These results with regard to the reversible SEI structure could give a new insight for the battery development.jmicro;63/suppl_1/i21/DFU056F1F1DFU056F1Fig. 1.SEM images of the graphite electrode surface:(a) before charge process;(b) with charge-cutoff voltage of 3.0V; (c) with charge-cutoff voltage of 4.2V; (d) with discharge-cutoff voltage of 3.0V. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  4. The development of optical microscopy techniques for the advancement of single-particle studies

    Science.gov (United States)

    Marchuk, Kyle

    Single particle orientation and rotational tracking (SPORT) has recently become a powerful optical microscopy tool that can expose many molecular motions. Unfortunately, there is not yet a single microscopy technique that can decipher all particle motions in all environmental conditions, thus there are limitations to current technologies. Within, the two powerful microscopy tools of total internal reflection and interferometry are advanced to determine the position, orientation, and optical properties of metallic nanoparticles in a variety of environments. Total internal reflection is an optical phenomenon that has been applied to microscopy to produce either fluorescent or scattered light. The non-invasive far-field imaging technique is coupled with a near-field illumination scheme that allows for better axial resolution than confocal microscopy and epi-fluorescence microscopy. By controlling the incident illumination angle using total internal reflection fluorescence (TIRF) microscopy, a new type of imaging probe called "non-blinking" quantum dots (NBQDs) were super-localized in the axial direction to sub-10-nm precision. These particles were also used to study the rotational motion of microtubules being propelled by the motor protein kinesin across the substrate surface. The same instrument was modified to function under total internal reflection scattering (TIRS) microscopy to study metallic anisotropic nanoparticles and their dynamic interactions with synthetic lipid bilayers. Utilizing two illumination lasers with opposite polarization directions at wavelengths corresponding to the short and long axis surface plasmon resonance (SPR) of the nanoparticles, both the in-plane and out-of-plane movements of many particles could be tracked simultaneously. When combined with Gaussian point spread function (PSF) fitting for particle super-localization, the binding status and rotational movement could be resolved without degeneracy. TIRS microscopy was also used to

  5. The development of optical microscopy techniques for the advancement of single-particle studies

    Energy Technology Data Exchange (ETDEWEB)

    Marchuk, Kyle [Iowa State Univ., Ames, IA (United States)

    2013-05-15

    Single particle orientation and rotational tracking (SPORT) has recently become a powerful optical microscopy tool that can expose many molecular motions. Unfortunately, there is not yet a single microscopy technique that can decipher all particle motions in all environmental conditions, thus there are limitations to current technologies. Within, the two powerful microscopy tools of total internal reflection and interferometry are advanced to determine the position, orientation, and optical properties of metallic nanoparticles in a variety of environments. Total internal reflection is an optical phenomenon that has been applied to microscopy to produce either fluorescent or scattered light. The non-invasive far-field imaging technique is coupled with a near-field illumination scheme that allows for better axial resolution than confocal microscopy and epi-fluorescence microscopy. By controlling the incident illumination angle using total internal reflection fluorescence (TIRF) microscopy, a new type of imaging probe called “non-blinking” quantum dots (NBQDs) were super-localized in the axial direction to sub-10-nm precision. These particles were also used to study the rotational motion of microtubules being propelled by the motor protein kinesin across the substrate surface. The same instrument was modified to function under total internal reflection scattering (TIRS) microscopy to study metallic anisotropic nanoparticles and their dynamic interactions with synthetic lipid bilayers. Utilizing two illumination lasers with opposite polarization directions at wavelengths corresponding to the short and long axis surface plasmon resonance (SPR) of the nanoparticles, both the in-plane and out-of-plane movements of many particles could be tracked simultaneously. When combined with Gaussian point spread function (PSF) fitting for particle super-localization, the binding status and rotational movement could be resolved without degeneracy. TIRS microscopy was also used to

  6. Transmission electron microscopy and image simulation study of CuAu domains in CuInS{sub 2} epitaxial layers

    Energy Technology Data Exchange (ETDEWEB)

    Barcones, B.; Romano-Rodriguez, A.; Arbiol, J.; Alvarez-Garcia, J.; Perez-Rodriguez, A.; Morante, J.R.; Scheer, R

    2003-05-01

    In this work the occurrence of two polytypic structures, chalcopyrite (CH) and cationic fcc CuAu-ordering (CA), in epitaxial CuInS{sub 2} samples on Si (1 1 1) oriented substrates has been studied. Samples with different Cu-to-In ratios and grown at 500 and 575 deg. C, respectively, have been analysed. Cross-section Transmission electron microscopy (TEM) samples have been prepared and studied in two directions normal to the growth direction [2 2 1]{sub CH}, namely, [1-1 0]{sub CH}, which is parallel to [1 0 0]{sub CA}, and [1 1-1]{sub CH} that is parallel to [0 1-1]{sub CA}. Electron diffraction and high resolution TEM images corroborate the existence of both polytypes and give the orientation relationship between them, namely, [1-1 0]{sub CH} parallel [1 0 0]{sub CA} and (1 1 2){sub CH} parallel (0 1 1){sub CA}. Cu-rich samples have good crystalline quality with large grains and sharp interfaces between both polytypes, the most important being between the (1 1 2){sub CH} and (0 1 1){sub CA} planes. On the contrary, the crystalline quality of Cu-poor samples is minor, no clear interfaces can be observed, and a high density of twins in the (0 1-1){sub CA} planes can be observed. The results on the crystalline quality are in agreement with previous results on polycrystalline CuInS{sub 2} films.

  7. In situ transmission electron microscopy studies of microstructure evolution in Ba(Zr0.2Ti0.8)O3-x(Ba0.7Ca0.3)TiO3 piezoceramic

    International Nuclear Information System (INIS)

    Zakhozheva, Marina

    2016-01-01

    The purpose of this work is to understand the microstructural features which contribute to the strong electromechanical properties of the lead-free Ba (Zr 0.2 Ti 0.8 )O 3 -x(Ba 0.7 Ca 0.3 )TiO 3 (BZT-xBCT) piezoelectric ceramic. Detailed conventional transmission electron microscopy (TEM) studies on a broad variety of BZT - xBCT were performed in order to demonstrate the composition dependent structural changes. Moreover, several in situ TEM techniques, including in situ hot- and cold-stage, in situ electric field and in situ electric field with simultaneous cooling, were successfully applied in order to monitor the domain morphology evolution in real time. By means of in situ temperature dependent TEM experiments it was shown that during rhombohedral → orthorhombic → tetragonal phase transition the domain morphology changed according to the crystal structure present. During in situ electric field investigations the displacement of the domain walls and changes in the domain configuration during electrical poling were observed, which indicates a high extrinsic contribution to the piezoelectric response in all BZT - xBCT compositions studied. From the results of in situ electric field TEM experiments with simultaneous cooling, we obtained experimental evidence that the further the composition deviates from the polymorphic phase boundary, the higher the electric field required to fully pole the material.

  8. Characterization of isolated polyamide thin films of RO and NF membranes using novel TEM techniques

    KAUST Repository

    Pacheco, Federico A.; Pinnau, Ingo; Reinhard, Martin; Leckie, James O.

    2010-01-01

    Achieving a better understanding of transport and rejection mechanisms in RO and NF membranes requires more detailed information of the nanostructure of polyamide thin films. This study reports on two novel transmission electron microscopy (TEM) techniques for characterizing polyamide nanostructure. The first technique produces cross-sectional images of isolated polyamide thin films by removing the polysulfone support from regular TEM cross-sections. In the second technique called " projected area" TEM (PA-TEM), isolated polyamide thin films are placed with their surface perpendicular to the electron beam. The resulting images capture the thickness, morphology and mass density of the entire thin film. In combination, these new techniques provide information on polyamide nanostructure that is not evident using conventional methods. For the commercial RO membrane ESPA3, the cross-sectional view of the isolated polyamide thin film shows a 30-60. nm thick base of nodular polyamide (presumably the separation barrier) that forms a relatively smooth interface with the polysulfone support. Above this, a more open structure of loose polyamide extends outward giving rise to the ridge-and-valley surface structure. In PA-TEM images, the ridges and valleys correspond to the dark and bright regions, respectively; the polyamide nodular base appears as round features forming an irregular honeycomb pattern throughout the images. Membrane cross-sections were prepared with a simple resin embedding protocol using the acrylic resin LR White. The protocol did not require dehydration steps, and was applicable to both dry and wet membrane samples. Artifacts that may be produced during sample preparation were also documented. © 2010 Elsevier B.V.

  9. Characterization of isolated polyamide thin films of RO and NF membranes using novel TEM techniques

    KAUST Repository

    Pacheco, Federico A.

    2010-08-15

    Achieving a better understanding of transport and rejection mechanisms in RO and NF membranes requires more detailed information of the nanostructure of polyamide thin films. This study reports on two novel transmission electron microscopy (TEM) techniques for characterizing polyamide nanostructure. The first technique produces cross-sectional images of isolated polyamide thin films by removing the polysulfone support from regular TEM cross-sections. In the second technique called " projected area" TEM (PA-TEM), isolated polyamide thin films are placed with their surface perpendicular to the electron beam. The resulting images capture the thickness, morphology and mass density of the entire thin film. In combination, these new techniques provide information on polyamide nanostructure that is not evident using conventional methods. For the commercial RO membrane ESPA3, the cross-sectional view of the isolated polyamide thin film shows a 30-60. nm thick base of nodular polyamide (presumably the separation barrier) that forms a relatively smooth interface with the polysulfone support. Above this, a more open structure of loose polyamide extends outward giving rise to the ridge-and-valley surface structure. In PA-TEM images, the ridges and valleys correspond to the dark and bright regions, respectively; the polyamide nodular base appears as round features forming an irregular honeycomb pattern throughout the images. Membrane cross-sections were prepared with a simple resin embedding protocol using the acrylic resin LR White. The protocol did not require dehydration steps, and was applicable to both dry and wet membrane samples. Artifacts that may be produced during sample preparation were also documented. © 2010 Elsevier B.V.

  10. Study of the developed precipitates in Al-0.63Mg-0.37Si-0.5Cu (wt.%) alloy by using DSC and TEM techniques

    Energy Technology Data Exchange (ETDEWEB)

    Gaber, A. [Physics Department, Faculty of Science, Assiut University (Egypt)]. E-mail: gaberaf@acc.aun.edu.eg; Ali, A. Mossad [Physics Department, Faculty of Science, Assiut University (Egypt); Matsuda, K. [Faculty of Engineering, University of Toyama (Japan); Kawabata, T. [Faculty of Engineering, University of Toyama (Japan); Yamazaki, T. [Faculty of Engineering, University of Toyama (Japan); Ikeno, S. [Faculty of Engineering, University of Toyama (Japan)

    2007-04-25

    Heat treatable Al-Mg-Si containing Cu alloys can be strengthened by the precipitation of the nano-scale metastable precipitates. In order to follow the precipitation sequence in balanced Al-1 mass%Mg{sub 2}Si containing 0.5 mass%Cu during continuous heating, differential scanning calorimetry (DSC) was performed. Analysis of non-isothermal DSC scans at various heating rates were carried out to evaluate the overall activation energies associated with the precipitation processes and, therefore, the mechanism of the developed precipitates has been characterized. The most important developed precipitates that assist the strength of the alloy are random, Q' and {beta}' precipitates. According to the obtained activation energies, the kinetics of the evolved Q'-precipitates could be controlled by the diffusion of Mg, Si and Cu in the crystal lattice of the alloy. Both conventional and high resolution transmission electron microscopy (HRTEM) were utilized to confirm the obtained results.

  11. Electron Microscopy of Ebola Virus-Infected Cells.

    Science.gov (United States)

    Noda, Takeshi

    2017-01-01

    Ebola virus (EBOV) replicates in host cells, where both viral and cellular components show morphological changes during the process of viral replication from entry to budding. These steps in the replication cycle can be studied using electron microscopy (EM), including transmission electron microscopy (TEM) and scanning electron microscopy (SEM), which is one of the most useful methods for visualizing EBOV particles and EBOV-infected cells at the ultrastructural level. This chapter describes conventional methods for EM sample preparation of cultured cells infected with EBOV.

  12. Nature of the Ag-Si interface in screen-printed contacts. A detailed transmission electron microscopy study of cross-sectional structures

    Energy Technology Data Exchange (ETDEWEB)

    Ballif, C. [Fraunhofer ISE, Laboratory and Service Center Gelsenkirchen (Germany); Huljic, D.M.; Willeke, G. [Fraunhofer-Institut fuer Solare Energiesysteme (ISE), Freiburg im Breisgau (Germany); Hessler-Wyser, A. [Swiss Federal Inst. of Technology, CIME, Lausanne (Switzerland)

    2002-07-01

    As screen printed contacts are the predominant metallisation technique in industrial production of Si solar cells, a better understanding of their properties is necessary. In this work, we show that high-quality cross-sectional samples can be prepared, whose study by transmission electron microscopy (TEM) reveals precisely the structure of the contact between the silver fingers and the Si. On diffused [100] Si wafers, direct firing of an Ag paste results in interfaces which are mainly composed of shaped Ag crystallites penetrating the emitter up to 120 nm. These crystallites are in epitaxial relation with the Sl substrate. When firing the contacts through a SiN{sub x} layer, larger Ag crystallites are present at the interface with Si and the orientation relation is lost. In both cases, high resolution TEM imaging and EDX analyses reveal a crystalline Ag/Si interface, where neither oxide nor glass frit can be detected. The presence of a significant glass frit layer between the Ag crystallites contacting the Si and the large Ag grains forming the bulk of the fingers can partly explain why lowly doped emitters are difficult to contact by screen-printing. (orig.)

  13. Quantitative phase imaging and differential interference contrast imaging for biological TEM

    International Nuclear Information System (INIS)

    Allman, B.E.; McMahon, P.J.; Barone-Nugent, E.D.; Nugent, E.D.

    2002-01-01

    Full text: Phase microscopy is a central technique in science. An experienced microscopist uses this effect to visualise (edge) structure within transparent samples by slightly defocusing the microscope. Although widespread in optical microscopy, phase contrast transmission electron microscopy (TEM) has not been widely adopted. TEM for biological specimens has largely relied on staining techniques to yield sufficient contrast. We show here a simple method for quantitative TEM phase microscopy that quantifies this phase contrast effect. Starting with conventional, digital, bright field images of the sample, our algorithm provides quantitative phase information independent of the sample's bright field intensity image. We present TEM phase images of a range of stained and unstained, biological and material science specimens. This independent phase and intensity information is then used to emulate a range of phase visualisation images familiar to optical microscopy, e.g. differential interference contrast. The phase images contain features not visible with the other imaging modalities. Further, if the TEM samples have been prepared on a microtome to a uniform thickness, the phase information can be converted into refractive index structure of the specimen. Copyright (2002) Australian Society for Electron Microscopy Inc

  14. [Contribution of confocal microscopy and anterior chamber OCT to the study of corneal endothelial pathologies].

    Science.gov (United States)

    Fayol, N; Labbé, A; Dupont-Monod, S; Dupas, B; Baudouin, C

    2007-04-01

    To describe the appearance of various endothelial diseases with in vivo confocal microscopy and anterior chamber optical coherence tomography (AC OCT). In this study, ten patients with five different corneal endothelial pathologies were evaluated. Three patients had cornea guttata, three had corneal endothelial precipitates, two had irido-corneo-endothelial (ICE) syndrome, one had endothelial folds, and one had breaks in the Descemet membrane. All patients had bilateral ophthalmologic examinations, in vivo confocal microscopy, and AC OCT analysis. In cases of cornea guttata, AC OCT showed a finely embossed line corresponding to the empty intercellular cavities found with in vivo confocal microscopy. Corneal endothelium precipitates had the aspect of round formations suspended with the endothelium. Iris atrophy and irido-corneal synechiae resulting from ICE syndrome were precisely visualized with the AC OCT. High-resolution images of the anterior segment could be obtained using the AC OCT. Associated with in vivo confocal microscopy, these two new imaging techniques provide a precise evaluation of endothelial pathologies.

  15. Studies of the structure of insulin fibrils by Fourier transform infrared (FTIR) spectroscopy and electron microscopy.

    Science.gov (United States)

    Nielsen, L; Frokjaer, S; Carpenter, J F; Brange, J

    2001-01-01

    Fibril formation (aggregation) of insulin was investigated in acid media by visual inspection, transmission electron microscopy (TEM), and Fourier transform infrared (FTIR) spectroscopy. Insulin fibrillated faster in hydrochloric acid than in acetic acid at elevated temperatures, whereas the fibrillation tendencies were reversed at ambient temperatures. Electron micrographs showed that bovine insulin fibrils consisted of long fibers with a diameter of 5 to 10 nm and lengths of several microns. The fibrils appeared either as helical filaments (in hydrochloric acid) or arranged laterally in bundles (in acetic acid, NaCl). Freeze-thawing cycles broke the fibrils into shorter segments. FTIR spectroscopy showed that the native secondary structure of insulin was identical in hydrochloric acid and acetic acid, whereas the secondary structure of fibrils formed in hydrochloric acid was different from that formed in acetic acid. Fibrils of bovine insulin prepared by heating or agitating an acid solution of insulin showed an increased content of beta-sheet (mostly intermolecular) and a decrease in the intensity of the alpha-helix band. In hydrochloric acid, the frequencies of the beta-sheet bands depended on whether the fibrillation was induced by heating or agitation. This difference was not seen in acetic acid. Freeze-thawing cycles of the fibrils in hydrochloric acid caused an increase in the intensity of the band at 1635 cm(-1) concomitant with reduction of the band at 1622 cm(-1). The results showed that the structure of insulin fibrils is highly dependent on the composition of the acid media and on the treatment. Copyright 2001 Wiley-Liss Inc. and the American Pharmaceutical Association J Pharm Sci 90: 29-37, 2001

  16. Energy-filtered TEM imaging and EELS study of ODS particles and argon-filled cavities in ferritic-martensitic steels.

    Science.gov (United States)

    Klimiankou, M; Lindau, R; Möslang, A

    2005-01-01

    Oxide-dispersion-strengthened (ODS) ferritic-martensitic steels with yttrium oxide (Y(2)O(3)) have been produced by mechanical alloying and hot isostatic pressing for use as advanced material in fusion power reactors. Argon gas, usually widely used as inert gas during mechanical alloying, was surprisingly detected in the nanodispersion-strengthened materials. Energy-filtered transmission electron microscopy (EFTEM) and electron energy loss spectroscopy (EELS) led to the following results: (i) chemical composition of ODS particles, (ii) voids with typical diameters of 1-6 nm are formed in the matrix, (iii) these voids are filled with Ar gas, and (iv) the high-density nanosized ODS particles serve as trapping centers for the Ar bubbles. The Ar L(3,2) energy loss edge at 245 eV as well as the absorption features of the ODS particle elements were identified in the EELS spectrum. The energy resolution in the EEL spectrum of about 1.0 eV allows to identify the electronic structure of the ODS particles.

  17. In situ TEM electromechanical testing of nanowires and nanotubes.

    Science.gov (United States)

    Espinosa, Horacio D; Bernal, Rodrigo A; Filleter, Tobin

    2012-11-05

    The emergence of one-dimensional nanostructures as fundamental constituents of advanced materials and next-generation electronic and electromechanical devices has increased the need for their atomic-scale characterization. Given its spatial and temporal resolution, coupled with analytical capabilities, transmission electron microscopy (TEM) has been the technique of choice in performing atomic structure and defect characterization. A number of approaches have been recently developed to combine these capabilities with in-situ mechanical deformation and electrical characterization in the emerging field of in-situ TEM electromechanical testing. This has enabled researchers to establish unambiguous synthesis-structure-property relations for one-dimensional nanostructures. In this article, the development and latest advances of several in-situ TEM techniques to carry out mechanical and electromechanical testing of nanowires and nanotubes are reviewed. Through discussion of specific examples, it is shown how the merging of several microsystems and TEM has led to significant insights into the behavior of nanowires and nanotubes, underscoring the significant role in-situ techniques play in the development of novel nanoscale systems and materials. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Correlation of simulated TEM images with irradiation induced damage

    International Nuclear Information System (INIS)

    Schaeublin, R.; Almeida, P. de; Almazouzi, A.; Victoria, M.

    2000-01-01

    Crystal damage induced by irradiation is investigated using transmission electron microscopy (TEM) coupled to molecular dynamics (MD) calculations. The displacement cascades are simulated for energies ranging from 10 to 50 keV in Al, Ni and Cu and for times of up to a few tens of picoseconds. Samples are then used to perform simulations of the TEM images that one could observe experimentally. Diffraction contrast is simulated using a method based on the multislice technique. It appears that the cascade induced damage in Al imaged in weak beam exhibits little contrast, which is too low to be experimentally visible, while in Ni and Cu a good contrast is observed. The number of visible clusters is always lower than the actual one. Conversely, high resolution TEM (HRTEM) imaging allows most of the defects contained in the sample to be observed, although experimental difficulties arise due to the low contrast intensity of the smallest defects. Single point defects give rise in HTREM to a contrast that is similar to that of cavities. TEM imaging of the defects is discussed in relation to the actual size of the defects and to the number of clusters deduced from MD simulations

  19. TEM specimen preparation of semiconductor-PMMA-metal interfaces

    International Nuclear Information System (INIS)

    Thangadurai, P.; Lumelsky, Yulia; Silverstein, Michael S.; Kaplan, Wayne D.

    2008-01-01

    Transmission electron microscopy (TEM) cross-section specimens of PMMA in contact with gold and Si were prepared by focused ion beam (FIB) and compared with plan-view PMMA specimens prepared by a dip-coating technique. The specimens were characterized by TEM and electron energy loss spectroscopy (EELS). In the cross-section specimens, the thin films of PMMA were located in a Si-PMMA-Au multilayer. Different thicknesses of PMMA films were spin-coated on the Si substrates. The thickness of the TEM specimens prepared by FIB was estimated using EELS to be 0.65 of the plasmon mean-free-path. Along the PMMA-Au interface, Au particle diffusion into the PMMA was observed, and the size of the Au particles was in the range of 2-4 nm. Dip-coating of PMMA directly on Cu TEM grids resulted in thin specimens with a granular morphology, with a thickness of 0.58 of the plasmon mean-free-path. The dip-coated specimens were free from ion milling induced artifacts, and thus serve as control specimens for comparison with the cross-sectioned specimens prepared by FIB

  20. TEM sample preparation by femtosecond laser machining and ion milling for high-rate TEM straining experiments

    Energy Technology Data Exchange (ETDEWEB)

    Voisin, Thomas; Grapes, Michael D. [Dept. of Materials Science and Engineering, Johns Hopkins University, Baltimore, MD 21218 (United States); Zhang, Yong [Dept. of Mechanical Engineering, Johns Hopkins University, Baltimore, MD 21218 (United States); Lorenzo, Nicholas; Ligda, Jonathan; Schuster, Brian [US Army Research Laboratory, Aberdeen Proving Ground, Aberdeen, MD 21005 (United States); Weihs, Timothy P. [Dept. of Materials Science and Engineering, Johns Hopkins University, Baltimore, MD 21218 (United States)

    2017-04-15

    To model mechanical properties of metals at high strain rates, it is important to visualize and understand their deformation at the nanoscale. Unlike post mortem Transmission Electron Microscopy (TEM), which allows one to analyze defects within samples before or after deformation, in situ TEM is a powerful tool that enables imaging and recording of deformation and the associated defect motion during mechanical loading. Unfortunately, all current in situ TEM mechanical testing techniques are limited to quasi-static strain rates. In this context, we are developing a new test technique that utilizes a rapid straining stage and the Dynamic TEM (DTEM) at the Lawrence Livermore National Laboratory (LLNL). The new straining stage can load samples in tension at strain rates as high as 4×10{sup 3}/s using two piezoelectric actuators operating in bending while the DTEM at LLNL can image in movie mode with a time resolution as short as 70 ns. Given the piezoelectric actuators are limited in force, speed, and displacement, we have developed a method for fabricating TEM samples with small cross-sectional areas to increase the applied stresses and short gage lengths to raise the applied strain rates and to limit the areas of deformation. In this paper, we present our effort to fabricate such samples from bulk materials. The new sample preparation procedure combines femtosecond laser machining and ion milling to obtain 300 µm wide samples with control of both the size and location of the electron transparent area, as well as the gage cross-section and length. - Highlights: • Tensile straining TEM specimens made by femtosecond laser machining and ion milling. • Accurate positioning of the electron transparent area within a controlled gauge region. • Optimization of femtosecond laser and ion milling parameters. • Fast production of numerous samples with a highly repeatable geometry.

  1. 3D TEM reconstruction and segmentation process of laminar bio-nanocomposites

    International Nuclear Information System (INIS)

    Iturrondobeitia, M.; Okariz, A.; Fernandez-Martinez, R.; Jimbert, P.; Guraya, T.; Ibarretxe, J.

    2015-01-01

    The microstructure of laminar bio-nanocomposites (Poly (lactic acid)(PLA)/clay) depends on the amount of clay platelet opening after integration with the polymer matrix and determines the final properties of the material. Transmission electron microscopy (TEM) technique is the only one that can provide a direct observation of the layer dispersion and the degree of exfoliation. However, the orientation of the clay platelets, which affects the final properties, is practically immeasurable from a single 2D TEM image. This issue can be overcome using transmission electron tomography (ET), a technique that allows the complete 3D characterization of the structure, including the measurement of the orientation of clay platelets, their morphology and their 3D distribution. ET involves a 3D reconstruction of the study volume and a subsequent segmentation of the study object. Currently, accurate segmentation is performed manually, which is inefficient and tedious. The aim of this work is to propose an objective/automated segmentation methodology process of a 3D TEM tomography reconstruction. In this method the segmentation threshold is optimized by minimizing the variation of the dimensions of the segmented objects and matching the segmented V clay (%) and the actual one. The method is first validated using a fictitious set of objects, and then applied on a nanocomposite

  2. Memory properties and charge effect study in Si nanocrystals by scanning capacitance microscopy and spectroscopy

    Directory of Open Access Journals (Sweden)

    Bassani Franck

    2011-01-01

    Full Text Available Abstract In this letter, isolated Si nanocrystal has been formed by dewetting process with a thin silicon dioxide layer on top. Scanning capacitance microscopy and spectroscopy were used to study the memory properties and charge effect in the Si nanocrystal in ambient temperature. The retention time of trapped charges injected by different direct current (DC bias were evaluated and compared. By ramp process, strong hysteresis window was observed. The DC spectra curve shift direction and distance was observed differently for quantitative measurements. Holes or electrons can be separately injected into these Si-ncs and the capacitance changes caused by these trapped charges can be easily detected by scanning capacitance microscopy/spectroscopy at the nanometer scale. This study is very useful for nanocrystal charge trap memory application.

  3. Tetrairon(III) Single Molecule Magnet Studied by Scanning Tunneling Microscopy and Spectroscopy

    Science.gov (United States)

    Oh, Youngtek; Jeong, Hogyun; Lee, Minjun; Kwon, Jeonghoon; Yu, Jaejun; Mamun, Shariful Islam; Gupta, Gajendra; Kim, Jinkwon; Kuk, Young

    2011-03-01

    Tetrairon(III) single-molecule magnet (SMM) on a clean Au(111) has studied using scanning tunneling microscopy (STM) and spectroscopy (STS) to understand quantum mechanical tunneling of magnetization and hysteresis of pure molecular origin. Before the STM studies, elemental analysis, proton nuclear magnetic resonance (NMR) measurement and Energy Dispersive X- ray Spectroscopy (EDS) were carried out to check the robustness of the sample. The STM image of this molecule shows a hexagonal shape, with a phenyl ring at the center and surrounding six dipivaloylmethane ligands. Two peaks are observed at 0.5 eV, 1.5 eV in the STS results, agreeing well with the first principles calculations. Spin-polarized scanning tunneling microscopy (SPSTM) measurements have been performed with a magnetic tip to get the magnetization image of the SMM. We could observe the antiferromagnetic coupling and a centered- triangular topology with six alkoxo bridges inside the molecule while applying external magnetic fields.

  4. In vivo studies of transdermal nanoparticle delivery with microneedles using photoacoustic microscopy

    Science.gov (United States)

    Moothanchery, Mohesh; Seeni, Razina Z.; Xu, Chenjie; Pramanik, Manojit

    2017-01-01

    Microneedle technology allows micron-sized conduits to be formed within the outermost skin layers for both localized and systemic delivery of therapeutics including nanoparticles. Histological methods are often employed for characterization, and unfortunately do not allow for the in vivo visualization of the delivery process. This study presents the utilization of optical resolution-photoacoustic microscopy to characterize the transdermal delivery of nanoparticles using microneedles. Specifically, we observe the in vivo transdermal delivery of gold nanoparticles using microneedles in mice ear and study the penetration, diffusion, and spatial distribution of the nanoparticles in the tissue. The promising results reveal that photoacoustic microscopy can be used as a potential imaging modality for the in vivo characterization of microneedles based drug delivery. PMID:29296482

  5. Oxidation study by Moessbauer and optic microscopy of steels from boiler tubes used in sugar industry

    International Nuclear Information System (INIS)

    Fajardo, M.; Perez Alcazar, G.A.; Aguilar, Y.

    1998-01-01

    Optic microscopy and Moessbauer spectroscopy were used to study the fail and the inner rusted surface of two boiler tubes used in the sugar industry, respectively. The studied tubes, of the type ASTM A 192, were found to have cracks. By optic microscopy it was observed that the failure begins in the inner surface with circumferential cracking. Also, inside and around the surface close to the cracks a rusted layer was detected. Powder from these layers was collected for Moessbauer spectroscopy analysis. By this method the presence of two or three types of Fe oxides such as wuestite, magnetite and hematite, was proved. These results permit to conclude that the failure mechanism was the thermal fatigue due to a hot work in an O 2 -rich vapor atmosphere. The rusted products are stable at high temperatures

  6. Optical coherent tomography and fluorescent microscopy for the study of meningeal lymphatic systems

    Science.gov (United States)

    Semyachkina-Glushkovskaya, O.; Abdurashitov, A.; Namykin, A.; Fedosov, I.; Pavlov, A.; Karavaev, A.; Sindeeva, O.; Shirokov, A.; Ulanova, M.; Shushunova, N.; Khorovodov, A.; Agranovich, I.; Bodrova, A.; Sagatova, M.; Shareef, Ali Esmat; Saranceva, E.; Dvoryatkina, M.; Tuchin, V.

    2018-04-01

    The development of novel technologies for the imaging of meningeal lymphatic vessels is one of the amazing trends of biophotonics thanks to discovery of brain lymphatics over several years ago. However, there is the limited technologies exist for the study of lymphatics in vivo because lymphatic vessels are transparent with a low speed flow of lymph. Here we demonstrate the successful application of fluorescent microscopy for the imaging of lymphatic system in the mouse brain in vivo.

  7. Studying the dynamics of colloidal particles with digital holographic microscopy and electromagnetic scattering solutions

    Directory of Open Access Journals (Sweden)

    V. N. Manoharan

    2011-09-01

    Full Text Available Digital holographic microscopy (DHM can measure the 3D positions as well as the scattering properties of colloidal particles in a single 2D image. We describe DHM and our analysis of recorded holograms with exact scattering solutions, which permit the measurement of 3D particle positions with ∼10 nm precision and millisecond time resolution, and discuss studies of the Brownian dynamics of clusters of spheres with DHM.

  8. SCANNING ELECTRON MICROSCOPY STUDY OF THE DORSAL SURFACE OF THE TONGUE IN Chaetophractus vellerosus (MAMMALIA, DASYPODIDAE)

    OpenAIRE

    Estecondo, Silvia; Codón, Stella Maris; Casanave, Emma Beatriz

    2001-01-01

    The characteristics of the dorsal surface of Chaetophractus vellerosus tongue were studied by scanning electron microscopy. Simple or branched filiform, fungiform and vallate papillae are described. Simple conical filiform papillae appear in the apex, lateral edges and posterior third, caudally to the circumvallated ones. The branched papillae are densely distributed all over the dorsal surface of the lingual body. Fungiform ones are scattered among the branched filiform papillae. In the post...

  9. Bulk microstructure and local elastic properties of carbon nanocomposites studied by impulse acoustic microscopy technique

    Science.gov (United States)

    Levin, V.; Petronyuk, Yu.; Morokov, E.; Chernozatonskii, L.; Kuzhir, P.; Fierro, V.; Celzard, A.; Bellucci, S.; Bistarelli, S.; Mastrucci, M.; Tabacchioni, I.

    2016-05-01

    Bulk microstructure and elastic properties of epoxy-nanocarbon nanocomposites for diverse types and different content of carbon nanofiller has been studied by using impulse acoustic microscopy technique. It has been shown occurrence of various types of mesoscopic structure formed by nanoparticles inside the bulk of nanocomposite materials, including nanoparticle conglomerates and nanoparticle aerogel systems. In spite of the bulk microstructure, nanocarbon composites demonstrate elastic uniformity and negligible influence of nanofiller on elastic properties of carbon nanocomposite materials.

  10. Evolution and change of He bubbles in He-containing Ti films upon thermal treatment studied by small-angle X-ray scattering and transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Guangai [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); College of Nuclear Science and Technology, University of Science and Technology of China, Hefei, 230029 (China); Wu, Erdong, E-mail: ewu@imr.ac.cn [National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China); Huang, Chaoqiang [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); College of Nuclear Science and Technology, University of Science and Technology of China, Hefei, 230029 (China); Cheng, Chun [National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China); Yan, Guanyun [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); Wang, Xiaolin [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); College of Nuclear Science and Technology, University of Science and Technology of China, Hefei, 230029 (China); Liu, Shi [National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China); Tian, Qiang; Chen, Bo [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); Wu, Zhonghua [Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China); Liu, Yi; Wang, Jie [Institute of Shanghai Apply Physics, Chinese Academy of Sciences, Shanghai 201800 (China)

    2014-05-02

    Evolution and change of He bubbles in magnetron sputtering prepared He-containing Ti films under thermal treatment are studied by small-angle X-ray scattering (SAXS), transmission electron microscopy (TEM) and X-ray diffraction. Incorporation of He introduces a large number of He-vacancy clusters and some voids in the films, and significantly increases SAXS intensity and causes anisotropic scattering. The change of He induced defects during annealing is affected by thermal diffusion and migration of trapped He to the surface and between interfaces of He induced defects within the films. Annealing at 200 and 400 °C reduces intensity and anisotropy of SAXS, in accord with observed shrinking and disappearance of the voids. The simultaneous growth of non-uniformly distributed He bubbles to the sizes of 1–2 nm and a population level of 10{sup 5}/μm{sup 3} are detected in the temperature range. The changes are explained by migration and coalescence mechanisms, which requires low apparent activation energy. Inconsistence between TEM and SAXS observations is noted and attributed to thinning induced internal stress relaxation of TEM specimen. Remarkable enlargement of He bubbles, associated with increased SAXS intensity and fractal dimension, is observed after 600 °C annealing, indicating involvement of Ostwald Ripening (OR) mechanism. The OR process dominates at 800 °C, where the high temperature provides activation energy for accelerated He dissociation from small bubbles into larger ones, and generating textured microstructure and agglomerated bubble clusters. The inhomogeneous bubble size distribution observed at this temperature covers a broad range of about 10–50 nm and possessing a population density level of 10{sup 3}/μm{sup 3}. - Highlights: • Change of He bubbles in thermally treated Ti–He films is studied by SAXS and TEM. • SAXS reveals size distribution and fractional population of He bubbles in films. • He-vacancy clusters in Ti–He film

  11. Denaturing of single electrospun fibrinogen fibers studied by deep ultraviolet fluorescence microscopy.

    Science.gov (United States)

    Kim, Jeongyong; Song, Hugeun; Park, Inho; Carlisle, Christine R; Bonin, Keith; Guthold, Martin

    2011-03-01

    Deep ultraviolet (DUV) microscopy is a fluorescence microscopy technique to image unlabeled proteins via the native fluorescence of some of their amino acids. We constructed a DUV fluorescence microscope, capable of 280 nm wavelength excitation by modifying an inverted optical microscope. Moreover, we integrated a nanomanipulator-controlled micropipette into this instrument for precise delivery of picoliter amounts of fluid to selected regions of the sample. In proof-of-principle experiments, we used this instrument to study, in situ, the effect of a denaturing agent on the autofluorescence intensity of single, unlabeled, electrospun fibrinogen nanofibers. Autofluorescence emission from the nanofibers was excited at 280 nm and detected at ∼350 nm. A denaturant solution was discretely applied to small, select sections of the nanofibers and a clear local reduction in autofluorescence intensity was observed. This reduction is attributed to the dissolution of the fibers and the unfolding of proteins in the fibers. Copyright © 2010 Wiley-Liss, Inc.

  12. Mammosomatotroph adenoma of the pituitary associated with gigantism and hyperprolactinemia. A morphological study including immunoelectron microscopy.

    Science.gov (United States)

    Felix, I A; Horvath, E; Kovacs, K; Smyth, H S; Killinger, D W; Vale, J

    1986-01-01

    A 29-year old giantess with growth hormone excess and hyperprolactinemia underwent transsphenoidal surgery to remove her pituitary tumor. Electron microscopy revealed a mammosomatotroph adenoma composed of one cell type. Immunoelectron microscopy, using the immunogold technique, demonstrated predominantly growth hormone or prolactin or a varying mixture of both growth hormone and prolactin in the adenoma cells. The presence of growth hormone and prolactin was found not only in the cytoplasm of the same adenoma cells but also in the same secretory granules. In the nontumorous adenohypophysis, somatotrophs and lactotrophs showed ultrastructural signs of hyperactivity. This finding is in contrast with the presence of suppressed somatotrophs and lactotrophs seen in nontumorous portions of adult pituitaries harboring growth hormone or prolactin-secreting adenomas. Our morphological study reinforces the view that growth hormone-producing pituitary tumors, originating in childhood, are different from those of the adult gland.

  13. Transfer doping of single isolated nanodiamonds, studied by scanning probe microscopy techniques.

    Science.gov (United States)

    Bolker, Asaf; Saguy, Cecile; Kalish, Rafi

    2014-09-26

    The transfer doping of diamond surfaces has been applied in various novel two-dimensional electronic devices. Its extension to nanodiamonds (ND) is essential for ND-based applications in many fields. In particular, understanding the influence of the crystallite size on transfer doping is desirable. Here, we report the results of a detailed study of the electronic energetic band structure of single, isolated transfer-doped nanodiamonds with nanometric resolution using a combination of scanning tunneling spectroscopy and Kelvin force microscopy measurements. The results show how the band gap, the valence band maximum, the electron affinity and the work function all depend on the ND's size and nanoparticle surface properties. The present analysis, which combines information from both scanning tunneling spectroscopy and Kelvin force microscopy, should be applicable to any nanoparticle or surface that can be measured with scanning probe techniques.

  14. Transfer doping of single isolated nanodiamonds, studied by scanning probe microscopy techniques

    Science.gov (United States)

    Bolker, Asaf; Saguy, Cecile; Kalish, Rafi

    2014-09-01

    The transfer doping of diamond surfaces has been applied in various novel two-dimensional electronic devices. Its extension to nanodiamonds (ND) is essential for ND-based applications in many fields. In particular, understanding the influence of the crystallite size on transfer doping is desirable. Here, we report the results of a detailed study of the electronic energetic band structure of single, isolated transfer-doped nanodiamonds with nanometric resolution using a combination of scanning tunneling spectroscopy and Kelvin force microscopy measurements. The results show how the band gap, the valence band maximum, the electron affinity and the work function all depend on the ND’s size and nanoparticle surface properties. The present analysis, which combines information from both scanning tunneling spectroscopy and Kelvin force microscopy, should be applicable to any nanoparticle or surface that can be measured with scanning probe techniques.

  15. Transfer doping of single isolated nanodiamonds, studied by scanning probe microscopy techniques

    International Nuclear Information System (INIS)

    Bolker, Asaf; Kalish, Rafi; Saguy, Cecile

    2014-01-01

    The transfer doping of diamond surfaces has been applied in various novel two-dimensional electronic devices. Its extension to nanodiamonds (ND) is essential for ND-based applications in many fields. In particular, understanding the influence of the crystallite size on transfer doping is desirable. Here, we report the results of a detailed study of the electronic energetic band structure of single, isolated transfer-doped nanodiamonds with nanometric resolution using a combination of scanning tunneling spectroscopy and Kelvin force microscopy measurements. The results show how the band gap, the valence band maximum, the electron affinity and the work function all depend on the ND’s size and nanoparticle surface properties. The present analysis, which combines information from both scanning tunneling spectroscopy and Kelvin force microscopy, should be applicable to any nanoparticle or surface that can be measured with scanning probe techniques. (paper)

  16. Microscopy studies on pronton exchange membrane fuel cell electrodes with different ionomer contents

    DEFF Research Database (Denmark)

    Ma, Shuang; Solterbeck, Claus Henning; Odgaard, Madeleine

    2009-01-01

    of the electrode was well displayed in the topography and phase images. The particle and pore size (Z) distributions showed the most frequent values at 30-40 nm and 20-30 nm, respectively. The particle size corresponds to the size of the carbon support for the platinum catalyst. Catalyst agglomeration was observed......Proton Exchange Membrane (PEM) fuel cell electrodes with different ionomer contents were studied with various microscopic techniques. The morphology and surface potential were examined by Atomic Force Microscopy (AFM) and Kelvin Probe Microscopy (KPM), respectively. The particulate nature...... in high ionomer content electrodes. The surface potential images showed distinct difference to the topography images. The overall grain size was seen to increase, the pore volume to decrease, the surface roughness to decrease, and the surface potential variation to increase with the increase of ionomer...

  17. Experimental transmission electron microscopy studies and phenomenological model of bismuth-based superconducting compounds

    International Nuclear Information System (INIS)

    Elboussiri, Khalid

    1991-01-01

    The main part of this thesis is devoted to an experimental study by transmission electron microscopy of the different phases of the superconducting bismuth cuprates Bi_2Sr_2Ca_n_-_1Cu_nO_2_n_+_4. In high resolution electron microscopy, the two types of incommensurate modulation realized in these compounds have been observed. A model of structure has been proposed from which the simulated images obtained are consistent with observations. The medium resolution images correlated with the electron diffraction data have revealed existence of a multi-soliton regime with latent lock in phases of commensurate periods between 4b and 10b. At last, a description of different phases of these compounds as a result of superstructures from a disordered perovskite type structure is proposed (author) [fr

  18. Application of SEM/EBSD and FEG-TEM/CBED to determine eutectic solidification mechanisms

    International Nuclear Information System (INIS)

    Nogita, K.; Dahle, A.K.; Drennan, J.

    2002-01-01

    Full text: This study shows the application of electron backscatter diffraction (EBSD) in SEM and convergent beam electron diffraction (CBED) in FEG-TEM to determine eutectic nucleation and growth in hypoeutectic Al-Si foundry alloys. Because the eutectic reaction is often the final stage of solidification it can be expected to have a significant impact on the formation of casting defects, particularly porosity. Previous EBSD work by Nogita and Dahle (2001), Dahle et al (2001), has shown that the eutectic nucleates on the primary phase in the unmodified alloy, and eutectic grains are nucleated in the intergranular liquid, instead of filling the dendrite envelopes, when Sr or Sb is added. However, the orientation relationship between silicon and aluminium in the eutectic has so far not been determined because of difficulties with sample preparation for EBSD and also detection limitations of Kikuchi refraction of silicon and aluminium, particularly in modified alloys with a refined eutectic. The combination of the EBSD technique in SEM and CBED in TEM analyses can provide crystallographic orientation relationships between primary aluminium dendrites, eutectic aluminium and silicon, which are important to explicitly define the solidification mode of the eutectic in hypoeutectic Al-Si alloys. These relationships are influenced, and altered, by the addition of certain elements. This paper also describes the sample preparation techniques for SEM and TEM for samples with different eutectic structures. The advantages the techniques are discussed. Copyright (2002) Australian Society for Electron Microscopy Inc

  19. "Rinse and trickle": a protocol for TEM preparation and investigation of inorganic fibers from biological material.

    Science.gov (United States)

    Vigliaturo, Ruggero; Capella, Silvana; Rinaudo, Caterina; Belluso, Elena

    2016-07-01

    The purpose of this work is to define a sample preparation protocol that allows inorganic fibers and particulate matter extracted from different biological samples to be characterized morphologically, crystallographically and chemically by transmission electron microscopy-energy dispersive spectroscopy (TEM-EDS). The method does not damage or create artifacts through chemical attacks of the target material. A fairly rapid specimen preparation is applied with the aim of performing as few steps as possible to transfer the withdrawn inorganic matter onto the TEM grid. The biological sample is previously digested chemically by NaClO. The salt is then removed through a series of centrifugation and rinse cycles in deionized water, thus drastically reducing the digestive power of the NaClO and concentrating the fibers for TEM analysis. The concept of equivalent hydrodynamic diameter is introduced to calculate the settling velocity during the centrifugation cycles. This technique is applicable to lung tissues and can be extended to a wide range of organic materials. The procedure does not appear to cause morphological damage to the fibers or modify their chemistry or degree of crystallinity. The extrapolated data can be used in interdisciplinary studies to understand the pathological effects caused by inorganic materials.

  20. GISAXS modelling of helium-induced nano-bubble formation in tungsten and comparison with TEM

    Science.gov (United States)

    Thompson, Matt; Sakamoto, Ryuichi; Bernard, Elodie; Kirby, Nigel; Kluth, Patrick; Riley, Daniel; Corr, Cormac

    2016-05-01

    Grazing-incidence small angle x-ray scattering (GISAXS) is a powerful non-destructive technique for the measurement of nano-bubble formation in tungsten under helium plasma exposure. Here, we present a comparative study between transmission electron microscopy (TEM) and GISAXS measurements of nano-bubble formation in tungsten exposed to helium plasma in the Large Helical Device (LHD) fusion experiment. Both techniques are in excellent agreement, suggesting that nano-bubbles range from spheroidal to ellipsoidal, displaying exponential diameter distributions with mean diameters μ=0.68 ± 0.04 nm and μ=0.6 ± 0.1 nm measured by TEM and GISAXS respectively. Depth distributions were also computed, with calculated exponential depth distributions with mean depths of 8.4 ± 0.5 nm and 9.1 ± 0.4 nm for TEM and GISAXS. In GISAXS modelling, spheroidal particles were fitted with an aspect ratio ε=0.7 ± 0.1. The GISAXS model used is described in detail.

  1. In Situ Environmental TEM in Imaging Gas and Liquid Phase Chemical Reactions for Materials Research.

    Science.gov (United States)

    Wu, Jianbo; Shan, Hao; Chen, Wenlong; Gu, Xin; Tao, Peng; Song, Chengyi; Shang, Wen; Deng, Tao

    2016-11-01

    Gas and liquid phase chemical reactions cover a broad range of research areas in materials science and engineering, including the synthesis of nanomaterials and application of nanomaterials, for example, in the areas of sensing, energy storage and conversion, catalysis, and bio-related applications. Environmental transmission electron microscopy (ETEM) provides a unique opportunity for monitoring gas and liquid phase reactions because it enables the observation of those reactions at the ultra-high spatial resolution, which is not achievable through other techniques. Here, the fundamental science and technology developments of gas and liquid phase TEM that facilitate the mechanistic study of the gas and liquid phase chemical reactions are discussed. Combined with other characterization tools integrated in TEM, unprecedented material behaviors and reaction mechanisms are observed through the use of the in situ gas and liquid phase TEM. These observations and also the recent applications in this emerging area are described. The current challenges in the imaging process are also discussed, including the imaging speed, imaging resolution, and data management. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Sinusoidal obstruction syndrome (SOS): A light and electron microscopy study in human liver.

    Science.gov (United States)

    Vreuls, C P H; Driessen, A; Olde Damink, S W M; Koek, G H; Duimel, H; van den Broek, M A J; Dejong, C H C; Braet, F; Wisse, E

    2016-05-01

    Oxaliplatin is an important chemotherapeutic agent, used in the treatment of hepatic colorectal metastases, and known to induce the sinusoidal obstruction syndrome (SOS). Pathophysiological knowledge concerning SOS is based on a rat model. Therefore, the aim was to perform a comprehensive study of the features of human SOS, using both light microscopy (LM) and electron microscopy (EM). Included were all patients of whom wedge liver biopsies were collected during a partial hepatectomy for colorectal liver metastases, in a 4-year period. The wedge biopsy were perfusion fixated and processed for LM and EM. The SOS lesions were selected by LM and details were studied using EM. Material was available of 30 patients, of whom 28 patients received neo-adjuvant oxaliplatin. Eighteen (64%) of the 28 patients showed SOS lesions, based on microscopy. The lesions consisted of sinusoidal endothelial cell detachment from the space of Disse on EM. In the enlarged space of Disse a variable amount of erythrocytes were located. Sinusoidal endothelial cell detachment was present in human SOS, accompanied by enlargement of the space of Disse and erythrocytes in this area. These findings, originally described in a rat model, were now for the first time confirmed in human livers under clinically relevant settings. Copyright © 2016 Elsevier Ltd. All rights reserved.

  3. [Does dark field microscopy according to Enderlein allow for cancer diagnosis? A prospective study].

    Science.gov (United States)

    El-Safadi, Samer; Tinneberg, Hans-Rudolf; von Georgi, Richard; Münstedt, Karsten; Brück, Friede

    2005-06-01

    Dark field microscopy according to Enderlin claims to be able to detect forthcoming or beginning cancer at an early stage through minute abnormalities in the blood. In Germany and the USA, this method is used by an increasing number of physicians and health practitioners (non-medically qualified complementary practitioners), because this easy test seems to give important information about patients' health status. Can dark field microscopy reliably detect cancer? In the course of a prospective study on iridology, blood samples were drawn for dark field microscopy in 110 patients. A health practitioner with several years of training in the field carried out the examination without prior information about the patients. Out of 12 patients with present tumor metastasis as confirmed by radiological methods (CT, MRI or ultra-sound) 3 were correctly identified. Analysis of sensitivity (0.25), specificity (0.64), positive (0.09) and negative (0.85) predictive values revealed unsatisfactory results. Dark field micoroscopy does not seem to reliably detect the presence of cancer. Clinical use of the method can therefore not be recommended until future studies are conducted.

  4. TEM investigations of microstructures of combustion aerosols

    International Nuclear Information System (INIS)

    Marquardt, A.; Hackfort, H.; Borchardt, J.; Schober, T.; Friedrich, J.

    1992-12-01

    In the incineration of organic material, apart from a series of gaseous pollutants, particulate pollutants or combustion aerosols also arise. The latter frequently consist of particles with a solid core of carbon to which a large number of inorganic and organic compounds are attached. These primarily include the polycyclic aromatic hydrocarbons (PAH) and their nitro-derivatives (NPAH), whose mutagenic or carcinogenic effect is known. The invisible particle sizes in the nanometer range, whose retention in the incineration off-gas is not state of the art, are of increasing significance for man and environment. On the one hand, they are deposited almost completely in the human lung. On the other hand, due to their fine dispersity they have along residence time in the atmosphere where they participate in chemical reactions and climatically significant processes. Important insights about the formation process of combustion aerosols are to be expected from the imaging of their microstructures in the transmission electron microscope (TEM). The present contribution describes the development and application of a representative sampling procedure for aerosols from a partial flow of flue gas from a fluidized-bed furnace. The method developed consists of electrically charging aerosol particles in situ and subsequently selectively precipitating them onto a microscope slide in an electric field. TEM studies of aerosol microstructures on the microscope slides revealed that in the combustion of petrol and heating oil under different combustion conditions in principle the same particle structures result, whereas in the incineration of used lubricating oil quite different particle structures were found. Results from the literature on aerosol microstructures in exhaust gases from petrol and diesel engines demonstrate agreement with the results of this study in the basic structure of the particles. (orig.) [de

  5. Environmental TEM Study of Electron Beam Induced Electrochemistry of Pr0.64Ca0.36MnO3 Catalysts for Oxygen Evolution

    DEFF Research Database (Denmark)

    Mildner, Stephanie; Beleggia, Marco; Mierwaldt, Daniel

    2015-01-01

    Environmental transmission electron microscopy (ETEVI) studies offer great potential for gathering atomic scale information on the electronic state of electrodes in contact with reactants. It also poses big challenges due to the impact of the high energy electron beam. In this article, we present...

  6. In Situ Transmission Electron Microscopy Studies of the Magnetization Reversal Mechanism in Information Storage Materials.

    Science.gov (United States)

    Petford-Long; Portier; Bayle-Guillemaud; Anthony; Brug

    1998-05-01

    : The Foucault and Fresnel modes of Lorentz microscopy, together with a quantitative magnetization mapping technique, summed image differential phase-contrast imaging, were used to study the magnetization reversal mechanism of the sense layer in spin-valve structures exhibiting the giant magnetoresistance effect. In addition to studies of sheet film, lithographically defined spin-valve elements were investigated. A current can be passed through the element during magnetizing so that the effect of the applied current on the giant magnetoresistance and magnetization reversal mechanism can be studied. Results are presented for a number of different spin-valve structures.

  7. Novel in-situ lamella fabrication technique for in-situ TEM.

    Science.gov (United States)

    Canavan, Megan; Daly, Dermot; Rummel, Andreas; McCarthy, Eoin K; McAuley, Cathal; Nicolosi, Valeria

    2018-03-29

    In-situ transmission electron microscopy is rapidly emerging as the premier technique for characterising materials in a dynamic state on the atomic scale. The most important aspect of in-situ studies is specimen preparation. Specimens must be electron transparent and representative of the material in its operational state, amongst others. Here, a novel fabrication technique for the facile preparation of lamellae for in-situ transmission electron microscopy experimentation using focused ion beam milling is developed. This method involves the use of rotating microgrippers during the lift-out procedure, as opposed to the traditional micromanipulator needle and platinum weld. Using rotating grippers, and a unique adhesive substance, lamellae are mounted onto a MEMS device for in-situ TEM annealing experiments. We demonstrate how this technique can be used to avoid platinum deposition as well as minimising damage to the MEMS device during the thinning process. Our technique is both a cost effective and readily implementable alternative to the current generation of preparation methods for in-situ liquid, electrical, mechanical and thermal experimentation within the TEM as well as traditional cross-sectional lamella preparation. Copyright © 2018 Elsevier B.V. All rights reserved.

  8. Characterization of mineral particles in winter fog of Beijing analyzed by TEM and SEM.

    Science.gov (United States)

    Li, Weijun; Shao, Longyi

    2010-02-01

    Aerosol samples were collected during winter fog and nonfog episodes in Beijing. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were applied to study morphologies, sizes, and compositions of aerosol particles. TEM observation indicates that most mineral particles collected in fog episode are scavenged in fog droplets. Number-size distributions of mineral particles collected in fog and nonfog episodes show two main peaks at the ranges of 0.1-0.3 and 1-2.5 microm, respectively. Based on their major compositions, mineral particles mainly include Si-rich, Ca-rich, and S-rich. Average S/Ca ratio of mineral particles collected in fog episode is 6.11, being eight times higher than that in nonfog episodes. Development mechanism of individual mineral particles in fog droplets is proposed. It is suggested that mineral particles with abundant alkaline components (e.g., "Ca-rich" particles) occurred in air should alleviate acidic degree of fog and contribute to complexity of fog droplets in Beijing.

  9. Transmission electron microscopy investigation of Bi-2223/Ag tapes

    DEFF Research Database (Denmark)

    Andersen, L.G.; Bals, S.; Tendeloo, G. Van

    2001-01-01

    during the tape processing, (3) a study of the grain boundaries on an atomic scale, including intergrowth investigations. Tapes with different process parameters have been compared with respect to the microstructure. A fully processed tape has on the average 50% thicker Bi-2223 grains than a tape after......The microstructure of (Bi,Pb)(2)Sr2Ca2CuOx (Bi-2223) tapes has been investigated by means of transmission electron microscopy (TEM) and high-resolution TEM. The emphasis has been placed on: (1) an examination of the grain morphology and size, (2) grain and colony boundary angles, which are formed...

  10. Electron microscopy studies of octa-calcium phosphate thin films obtained by pulsed laser deposition

    Energy Technology Data Exchange (ETDEWEB)

    Iliescu, Monica; Nelea, V.; Werckmann, J.; Mihailescu, I.N.; Socol, G.; Bigi, Adriana; Bracci, Barbara

    2004-04-01

    Octa-calcium phosphate (OCP), Ca{sub 8}(HPO{sub 4}){sub 2}(PO{sub 4}){sub 4}{center_dot}5H{sub 2}O, is present as transient compound in the precipitation of hydroxyapatite (HA) and biological apatites. Because of these characteristics, OCP plays a crucial role in the in-vivo mineralization of human bones and teeth. The use of OCP in developing new generations of bone prosthesis stands therefore for an innovative challenge. This paper reports studies of OCP structures grown in the form of thin films by pulsed laser deposition (PLD) with emphasis on electron microscopy investigations. OCP films were grown on etched Ti substrates, using an UV KrF* excimer laser source ({lambda}=248 nm, {tau}{>=}20 ns). Films were deposited in low-pressure (50 Pa) water vapors environment on substrates heated at 20-180 deg. C. We performed annealing treatments in water vapors and ambient pressure at substrate temperatures identical to those used during deposition. Comprehensive structural and morphological investigations were carried out with different based-electron microscopy procedures. Grazing incidence X-ray diffraction (GIXRD) and white light confocal microscopy were also applied to characterize the films. Ca/P atomic ratio of films was determined by energy dispersive X-ray spectrometry, electron energy loss spectroscopy and X-ray photoelectron spectroscopy. The obtained films generally exhibit an amorphous structure, as evidenced by GIXRD. Nevertheless, cross-section transmission electron microscopy investigations provide supplementary information about the film characteristics and material crystallization in small domains. OCP nanoparticles coalesce and grow perpendicular to the substrate in a tree-like structure, comparable to a coral reef.

  11. Microfabricated Nanofluidic cells for in situ liquid TEM

    DEFF Research Database (Denmark)

    Laganà, Simone

    Over the last decade, transmission electron microscopy (TEM) has been revolutionized not only by the introduction of new and very sophisticated hardware for improved resolution, such as aberration correctors and monochromators, but also by the improvement of new methods that have provided more than......, allowing quantitative and high-precision acquisition of liquid thickness maps, high resolution observations and meaningful information about synthesis of NPs from metal precursor solutions in confined space. Finally, a new concept device based on a Si3N4 membrane for plunge freezing fixation, which enables...

  12. Sample preparation methods for scanning electron microscopy of homogenized Al-Mg-Si billets: A comparative study

    International Nuclear Information System (INIS)

    Österreicher, Johannes Albert; Kumar, Manoj; Schiffl, Andreas; Schwarz, Sabine; Hillebrand, Daniel; Bourret, Gilles Remi

    2016-01-01

    Characterization of Mg-Si precipitates is crucial for optimizing the homogenization heat treatment of Al-Mg-Si alloys. Although sample preparation is key for high quality scanning electron microscopy imaging, most common methods lead to dealloying of Mg-Si precipitates. In this article we systematically evaluate different sample preparation methods: mechanical polishing, etching with various reagents, and electropolishing using different electrolytes. We demonstrate that the use of a nitric acid and methanol electrolyte for electropolishing a homogenized Al-Mg-Si alloy prevents the dissolution of Mg-Si precipitates, resulting in micrographs of higher quality. This preparation method is investigated in depth and the obtained scanning electron microscopy images are compared with transmission electron micrographs: the shape and size of Mg-Si precipitates appear very similar in either method. The scanning electron micrographs allow proper identification and measurement of the Mg-Si phases including needles with lengths of roughly 200 nm. These needles are β″ precipitates as confirmed by high resolution transmission electron microscopy. - Highlights: •Secondary precipitation in homogenized 6xxx Al alloys is crucial for extrudability. •Existing sample preparation methods for SEM are improvable. •Electropolishing with nitric acid/methanol yields superior quality in SEM. •The obtained micrographs are compared to TEM micrographs.

  13. Sample preparation methods for scanning electron microscopy of homogenized Al-Mg-Si billets: A comparative study

    Energy Technology Data Exchange (ETDEWEB)

    Österreicher, Johannes Albert; Kumar, Manoj [LKR Light Metals Technologies Ranshofen, Austrian Institute of Technology, Postfach 26, 5282 Ranshofen (Austria); Schiffl, Andreas [Hammerer Aluminium Industries Extrusion GmbH, Lamprechtshausener Straße 69, 5282 Ranshofen (Austria); Schwarz, Sabine [University Service Centre for Transmission Electron Microscopy, Vienna University of Technology, Wiedner Hauptstr. 8-10, 1040 Wien (Austria); Hillebrand, Daniel [Hammerer Aluminium Industries Extrusion GmbH, Lamprechtshausener Straße 69, 5282 Ranshofen (Austria); Bourret, Gilles Remi, E-mail: gilles.bourret@sbg.ac.at [Department of Materials Science and Physics, University of Salzburg, Hellbrunner Straße 34, 5020 Salzburg (Austria)

    2016-12-15

    Characterization of Mg-Si precipitates is crucial for optimizing the homogenization heat treatment of Al-Mg-Si alloys. Although sample preparation is key for high quality scanning electron microscopy imaging, most common methods lead to dealloying of Mg-Si precipitates. In this article we systematically evaluate different sample preparation methods: mechanical polishing, etching with various reagents, and electropolishing using different electrolytes. We demonstrate that the use of a nitric acid and methanol electrolyte for electropolishing a homogenized Al-Mg-Si alloy prevents the dissolution of Mg-Si precipitates, resulting in micrographs of higher quality. This preparation method is investigated in depth and the obtained scanning electron microscopy images are compared with transmission electron micrographs: the shape and size of Mg-Si precipitates appear very similar in either method. The scanning electron micrographs allow proper identification and measurement of the Mg-Si phases including needles with lengths of roughly 200 nm. These needles are β″ precipitates as confirmed by high resolution transmission electron microscopy. - Highlights: •Secondary precipitation in homogenized 6xxx Al alloys is crucial for extrudability. •Existing sample preparation methods for SEM are improvable. •Electropolishing with nitric acid/methanol yields superior quality in SEM. •The obtained micrographs are compared to TEM micrographs.

  14. TEMS: results of a specialist centre.

    Science.gov (United States)

    Flexer, S M; Durham-Hall, A C; Steward, M A; Robinson, J M

    2014-06-01

    Transanal endoscopic microsurgery (TEMS) is becoming more widespread due to the increasing body of evidence to support its role. Previous published data has reported recurrence rates in excess of 10% for benign polyps after TEMS. Bradford Royal Infirmary is a tertiary referral centre for TEMS and early rectal cancer in the UK. Data for all TEMS operations were entered into a prospective database over a 7-year period. Demographic data, complications and recurrence rates were recorded. Both benign adenomas and malignant lesions were included. A total of 164 patients (65% male), with a mean age of 68 years were included; 114 (70%) of the lesions resected were benign adenomas, and 50 (30%) were malignant lesions. Median polyp size was 4 (range 0.6-14.5) cm. Mean length of operation was 55 (range 10-120) min. There were no recurrences in any patients with a benign adenoma resected; two patients with malignant lesions developed recurrences. Three intra-operative complications were recorded, two rectal perforations (repaired primarily, one requiring defunctioning stoma), and a further patient suffered a blood loss of >300 ml requiring transfusion. Six patients developed strictures requiring dilation either endoscopically or under anaesthetic in the post-operative period. We have demonstrated that TEMS procedures performed in a specialist centre provide low rates of both recurrence and complication. Within a specialist centre, TEMS surgery should be offered to all patients for rectal lesions, both benign and malignant, that are amenable to TEMS.

  15. Study of Black Sand Particles from Sand Dunes in Badr, Saudi Arabia Using Electron Microscopy

    Directory of Open Access Journals (Sweden)

    Haider Abbas Khwaja

    2015-08-01

    Full Text Available Particulate air pollution is a health concern. This study determines the microscopic make-up of different varieties of sand particles collected at a sand dune site in Badr, Saudi Arabia in 2012. Three categories of sand were studied: black sand, white sand, and volcanic sand. The study used multiple high resolution electron microscopies to study the morphologies, emission source types, size, and elemental composition of the particles, and to evaluate the presence of surface “coatings or contaminants” deposited or transported by the black sand particles. White sand was comprised of natural coarse particles linked to wind-blown releases from crustal surfaces, weathering of igneous/metamorphic rock sources, and volcanic activities. Black sand particles exhibited different morphologies and microstructures (surface roughness compared with the white sand and volcanic sand. Morphological Scanning Electron Microscopy (SEM and Laser Scanning Microscopy (LSM analyses revealed that the black sand contained fine and ultrafine particles (50 to 500 nm ranges and was strongly magnetic, indicating the mineral magnetite or elemental iron. Aqueous extracts of black sands were acidic (pH = 5.0. Fe, C, O, Ti, Si, V, and S dominated the composition of black sand. Results suggest that carbon and other contaminant fine particles were produced by fossil-fuel combustion and industrial emissions in heavily industrialized areas of Haifa and Yanbu, and transported as cloud condensation nuclei to Douf Mountain. The suite of techniques used in this study has yielded an in-depth characterization of sand particles. Such information will be needed in future environmental, toxicological, epidemiological, and source apportionment studies.

  16. Transmission Electron Microscopy of Minerals and Rocks

    Science.gov (United States)

    McLaren, Alex C.

    1991-04-01

    Of the many techniques that have been applied to the study of crystal defects, none has contributed more to our understanding of their nature and influence on the physical and chemical properties of crystalline materials than transmission electron microscopy (TEM). TEM is now used extensively by an increasing number of earth scientists for direct observation of defect microstructures in minerals and rocks. Transmission Electron Microscopy of Rocks and Minerals is an introduction to the principles of the technique and is the only book to date on the subject written specifically for geologists and mineralogists. The first part of the book deals with the essential physics of the transmission electron microscope and presents the basic theoretical background required for the interpretation of images and electron diffraction patterns. The final chapters are concerned with specific applications of TEM in mineralogy and deal with such topics as planar defects, intergrowths, radiation-induced defects, dislocations and deformation-induced microstructures. The examples cover a wide range of rock-forming minerals from crustal rocks to those in the lower mantle, and also take into account the role of defects in important mineralogical and geological processes.

  17. Study and structural and chemical characterization of human dental smalt by electron microscopy

    International Nuclear Information System (INIS)

    Belio R, I.A.; Reyes G, J.

    1998-01-01

    The study of human dental smalt has been subject to investigation for this methods with electron microscopy, electron diffraction, X-ray diffraction and image simulation programs have been used with the purpose to determine its chemical and structural characteristics of the organic and inorganic materials. This work has been held mainly for the characterization of hydroxyapatite (Ca) 10 (PO 4 ) 6 (OH 4 ) 2 , inorganic material which conforms the dental smalt in 97%, so observing its structural unity which is composed by the prisms and these by crystals and atoms. It was subsequently initiated the study of the organic material, with is precursor of itself. (Author)

  18. Implementing atomic force microscopy (AFM) for studying kinetics of gold nanoparticle's growth

    DEFF Research Database (Denmark)

    Georgiev, P.; Bojinova, A.; Kostova, B.

    2013-01-01

    In a novel experimental approach Atomic Force Microscopy (AFM) was applied as a tool for studying the kinetics of gold nanoparticle growth. The gold nanoparticles were obtained by classical Turkevich citrate synthesis at two different temperatures. From the analysis of AFM images during...... the synthesis process the nanoparticle s' sizes were obtained. To demonstrate the applicability and the reliability of the proposed experimental approach we studied the nanoparticles growth at two different temperatures by spectrophotometric measurements and compared them with the results from AFM experimental...

  19. Embryological study of Herminium monorchis (Orchidaceae) using confocal scanning laser microscopy

    International Nuclear Information System (INIS)

    Fredrikson, M.

    1990-01-01

    The embryology of Herminium monorchis (Orchidaceae) was studied using confocal scanning laser microscopy (CSLM), a new technique for embryological studies. This technique may contribute new information to plant embryology. Herminium monorchis has a monosporic embryo sac development. The mature embryo sac is 8-nucleate. Two integuments, both 2-layered, are formed, but only the inner takes part in formation of the micropyle. Double fertilization takes place. The primary endosperm nucleus does not divide, but remains alive at least at the 3-celled stage of embryo development. The three antipodals do not show any sign of degeneration at this stage. (author)

  20. Recent advances in cryo-TEM imaging of soft lipid nanoparticles

    DEFF Research Database (Denmark)

    Helvig, Shen Yu; Mat Azmi, Intan Diana Binti; Moghimi, Seyed Moien

    2015-01-01

    Cryo-transmission electron microscopy (Cryo-TEM), and its technological variations thereof, have become a powerful tool for detailed morphological characterization and 3D tomography of soft lipid and polymeric nanoparticles as well as biological materials such as viruses and DNA without chemical...... fixation. Here, we review and discuss recent advances in Cryo-TEM analysis of lipid-based drug nanocarriers with particular emphasis on morphological and internal nanostructure characterization of lyotropic liquid crystalline nanoparticles such as cubosomes and hexosomes....

  1. Graphene as a transparent conductive support for studying biological molecules by transmission electron microscopy

    International Nuclear Information System (INIS)

    Nair, R. R.; Anissimova, S.; Novoselov, K. S.; Blake, P.; Blake, J. R.; Geim, A. K.; Zan, R.; Bangert, U.; Golovanov, A. P.; Morozov, S. V.; Latychevskaia, T.

    2010-01-01

    We demonstrate the application of graphene as a support for imaging individual biological molecules in transmission electron microscope (TEM). A simple procedure to produce free-standing graphene membranes has been designed. Such membranes are extremely robust and can support practically any submicrometer object. Tobacco mosaic virus has been deposited on graphene samples and observed in a TEM. High contrast has been achieved even though no staining has been applied.

  2. Investigation of C3 S hydration mechanism by transmission electron microscope (TEM) with integrated Super-XTM EDS system.

    Science.gov (United States)

    Sakalli, Y; Trettin, R

    2017-07-01

    Tricalciumsilicate (C 3 S, Alite) is the major component of the Portland cement clinker. Hydration of Alite is decisive in influencing the properties of the resulting material. This is due to its high content in cement. The mechanism of the hydration of C 3 S is very complicated and not yet fully understood. There are different models describing the hydration of C 3 S in various ways. In this work for a better understanding of hydration mechanism, the hydrated C 3 S was investigated by using the transmission electron microscope (TEM) and for the first time, the samples for the investigations were prepared by using of focused ion beam from sintered pellets of C 3 S. Also, an FEI Talos F200x with an integrated Super-X EDS system was used for the investigations. FEI Talos F200X combines outstanding high-resolution S/TEM and TEM imaging with energy dispersive X-ray spectroscopy signal detection, and 3D chemical characterization with compositional mapping. TEM is a very powerful tool for material science. A high energy beam of electrons passes through a very thin sample, and the interactions between the electrons and the atoms can be used to observe the structure of the material and other features in the structure. TEM can be used to study the growth of layers and their composition. TEM produces high-resolution, two-dimensional images and will be used for a wide range of educational, science and industry applications. Chemical analysis can also be performed. The purpose of these investigations was to get the information about the composition of the C-S-H phases and some details of the nanostructure of the C-S-H phases. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

  3. Some techniques for studying actomyosin by electron microscopy; Quelques techniques d'etude de l'actomyosine par microscopie electronique

    Energy Technology Data Exchange (ETDEWEB)

    Herzberg, M [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires. Departement de Biologie

    1967-07-01

    A method has been developed for shadowing using a platinum-carbon alloy; it has been applied to the study of the interaction of actomyosin with its substrate ATP. The results obtained seem to favour the hypothesis of a dissociation of the actomyosin into its two components: actin and myosin. Pictures have been obtained showing particles resembling non-polymerized myosin but no rigorous proof of this exists. (author) [French] Une methode d'ombrage par un alliage de platine et carbone a ete mise au point et appliquee a l'etude de l'interaction de l'actomyosine et de son substrat l'ATP. Les resultats obtenus semblent pencher en faveur de la these d'une dissociation de l'actomyosine en ses deux constituants: l'actine et la myosine. Des images ont ete obtenues montrant des particules dont l'identite avec la myosine non polymerisee reste a demontrer plus rigoureusement. (auteur)

  4. Transmission electron microscopy analysis of hydroxyapatite nanocrystals from cattle bones

    International Nuclear Information System (INIS)

    Patel, Sangeeta; Wei, Shanghai; Han, Jie; Gao, Wei

    2015-01-01

    In this present study, hydroxyapatite which was obtained from cattle bones has been heat treated at temperature 400 °C and 600 °C. The microstructure after the treatment has been studied in detail using Transmission electron microscopy (TEM) and X-ray diffraction techniques. The TEM results indicate that natural bone consists of collagen and hydroxyapatite nano-crystals which are needle shaped. The heat treatment influences the crystallinity and growth of these hydroxyapatite nano-crystals known as ‘crystal maturation’ or ‘crystal ageing’. - Highlights: • Hydroxyapatite is obtained from cattle bones. • Material has been characterised using XRD and TEM. • Crystal growth and orientation has been studied in detail.

  5. Transmission electron microscopy analysis of hydroxyapatite nanocrystals from cattle bones

    Energy Technology Data Exchange (ETDEWEB)

    Patel, Sangeeta, E-mail: spt658@aucklanduni.ac.nz [Department of Chemical and Materials Engineering, The University of Auckland, 20 Symonds Street, Auckland 1010 (New Zealand); Wei, Shanghai [Department of Chemical and Materials Engineering, The University of Auckland, 20 Symonds Street, Auckland 1010 (New Zealand); Han, Jie [Department of Civil and Environmental Engineering, University of Illinois at Urbana-Champaign, 205 North Mathews Avenue, Urbana, IL (United States); Gao, Wei [Department of Chemical and Materials Engineering, The University of Auckland, 20 Symonds Street, Auckland 1010 (New Zealand)

    2015-11-15

    In this present study, hydroxyapatite which was obtained from cattle bones has been heat treated at temperature 400 °C and 600 °C. The microstructure after the treatment has been studied in detail using Transmission electron microscopy (TEM) and X-ray diffraction techniques. The TEM results indicate that natural bone consists of collagen and hydroxyapatite nano-crystals which are needle shaped. The heat treatment influences the crystallinity and growth of these hydroxyapatite nano-crystals known as ‘crystal maturation’ or ‘crystal ageing’. - Highlights: • Hydroxyapatite is obtained from cattle bones. • Material has been characterised using XRD and TEM. • Crystal growth and orientation has been studied in detail.

  6. Secondary phases in AlxCoCrFeNi high-entropy alloys : An in-situ TEM heating study and thermodynamic appraisal

    NARCIS (Netherlands)

    Rao, J. C.; Diao, H. Y.; Ocelík, V.; Vainchtein, D.; Zhang, C.; Kuo, C. C.; Tang, Z.; Guo, W.; Poplawsky, J. D.; Zhou, Y.; Liaw, P. K.; De Hosson, J. Th M.

    2017-01-01

    Secondary phases, either introduced by alloying or heat treatment, are commonly present in most high-entropy alloys (HEAs). Understanding the formation of secondary phases at high temperatures, and their effect on mechanical properties, is a critical issue that is undertaken in the present study,

  7. Application of atomic force microscopy to the study of natural and model soil particles.

    Science.gov (United States)

    Cheng, S; Bryant, R; Doerr, S H; Rhodri Williams, P; Wright, C J

    2008-09-01

    The structure and surface chemistry of soil particles has extensive impact on many bulk scale properties and processes of soil systems and consequently the environments that they support. There are a number of physiochemical mechanisms that operate at the nanoscale which affect the soil's capability to maintain native vegetation and crops; this includes soil hydrophobicity and the soil's capacity to hold water and nutrients. The present study used atomic force microscopy in a novel approach to provide unique insight into the nanoscale properties of natural soil particles that control the physiochemical interaction of material within the soil column. There have been few atomic force microscopy studies of soil, perhaps a reflection of the heterogeneous nature of the system. The present study adopted an imaging and force measurement research strategy that accounted for the heterogeneity and used model systems to aid interpretation. The surface roughness of natural soil particles increased with depth in the soil column a consequence of the attachment of organic material within the crevices of the soil particles. The roughness root mean square calculated from ten 25 microm(2) images for five different soil particles from a Netherlands soil was 53.0 nm, 68.0 nm, 92.2 nm and 106.4 nm for the respective soil depths of 0-10 cm, 10-20 cm, 20-30 cm and 30-40 cm. A novel analysis method of atomic force microscopy phase images based on phase angle distribution across a surface was used to interpret the nanoscale distribution of organic material attached to natural and model soil particles. Phase angle distributions obtained from phase images of model surfaces were found to be bimodal, indicating multiple layers of material, which changed with the concentration of adsorbed humic acid. Phase angle distributions obtained from phase images of natural soil particles indicated a trend of decreasing surface coverage with increasing depth in the soil column. This was consistent with

  8. Vibrational spectroscopy and analytical electron microscopy studies of Fe-V-O and In-V-O thin films

    CERN Document Server

    Vuk, A S; Drazic, G; Colomban, P

    2002-01-01

    Orthovanadate (M sup 3 sup + VO sub 4; M= Fe, In) and vanadate (Fe sub 2 V sub 4 O sub 1 sub 3) thin films were prepared using sol-gel synthesis and dip coating deposition. Using analytical electron microscopy (AEM), the chemical composition and the degree of crystallization of the phases present in the thin Fe-V-O films were investigated. TEM samples were prepared in both orientations: parallel (plan view) and perpendicular (cross section) to the substrate. In the first stages of crystallization, when the particle sizes were in the nanometer range, the classical identification of phases using electron diffraction was not possible. Instead of measuring d values, experimentally selected area electron diffraction (SAED) patterns were compared to calculated (simulated) patterns in order to determine the phase composition. The problems of evaluating the ratio of amorphous and crystalline phases in thin films are reported. Results of TEM and XRD as well as IR and Raman spectroscopy showed that the films made at lo...

  9. Atomic force and scanning near-field optical microscopy study of carbocyanine dye J-aggregates

    Czech Academy of Sciences Publication Activity Database

    Prokhorov, V.V.; Petrova, M.G.; Kovaleva, Natalia; Demikhov, E.I.

    2014-01-01

    Roč. 10, č. 5 (2014), s. 700-704 ISSN 1573-4137 Institutional support: RVO:68378271 Keywords : carbocyanine dye * elementary fibri * high-resolution atomic force microscopy * J-aggregate * probe microscopy * scanning near-field optical microscopy Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.096, year: 2014

  10. SiO2-supported Pt particles studied by electron microscopy

    International Nuclear Information System (INIS)

    Wang, D.; Penner, S.; Su, D.S.; Rupprechter, G.; Hayek, K.; Schloegl, R.

    2003-01-01

    Regularly grown Pt particles supported by amorphous SiO 2 were heated in hydrogen at 873 K after an oxidising treatment. The morphological and structural changes were studied by electron microscopy. Platinum silicides Pt 3 Si with L1 2 (Cu 3 Au) structure, monoclinic Pt 3 Si and tetragonal Pt 12 Si 5 were identified after the treatment. The mechanisms of coalescence of the particles and the formation of irregular large particles are suggested. A topotactic structural transformation accompanied with the migration of Si from the substrate to the particles are suggested to take place during Pt 3 Si formation

  11. Reaction of LiD with water vapor: thermogravimetric and scanning electron microscopy studies

    International Nuclear Information System (INIS)

    Balooch, M; Dinh, L N; LeMay, J D

    2000-01-01

    The kinetics of hydroxide film growth on LiD have been studied by the thermogravimetric method in nitrogen saturated with water vapor and by scanning electron microscopy (SEM) of samples that have been exposed to air with 50% relative humidity. The reaction probability is estimated to be 4 x 10 -7 for LiD exposed to ambient air with 50% relative humidity, suggesting that the diffusion through the hydroxide film is not the limiting step on the overall process at high moisture levels. The rate of growth is drastically reduced when the temperature is increased to 60 C

  12. Surface adhesion properties of graphene and graphene oxide studied by colloid-probe atomic force microscopy

    International Nuclear Information System (INIS)

    Ding Yanhuai; Zhang Ping; Ren Huming; Zhuo Qin; Yang Zhongmei; Jiang Xu; Jiang Yong

    2011-01-01

    Surface adhesion properties are important to various applications of graphene-based materials. Atomic force microscopy is powerful to study the adhesion properties of samples by measuring the forces on the colloidal sphere tip as it approaches and retracts from the surface. In this paper we have measured the adhesion force between the colloid probe and the surface of graphene (graphene oxide) nanosheet. The results revealed that the adhesion force on graphene and graphene oxide surface were 66.3 and 170.6 nN, respectively. It was found the adhesion force was mainly determined by the water meniscus, which was related to the surface contact angle of samples.

  13. Interferometric scattering (iSCAT) microscopy: studies of biological membrane dynamics

    Science.gov (United States)

    Reina, Francesco; Galiani, Silvia; Shrestha, Dilip; Sezgin, Erdinc; Lagerholm, B. Christoffer; Cole, Daniel; Kukura, Philipp; Eggeling, Christian

    2018-02-01

    The study of the organization and dynamics of molecules in model and cellular membranes is an important topic in contemporary biophysics. Imaging and single particle tracking in this particular field, however, proves particularly demanding, as it requires simultaneously high spatio-temporal resolution and high signal-to-noise ratios. A remedy to this challenge might be Interferometric Scattering (iSCAT) microscopy, due to its fast sampling rates, label-free imaging capabilities and, most importantly, tuneable signal level output. Here we report our recent advances in the imaging and molecular tracking on phase-separated model membrane systems and live-cell membranes using this technique.

  14. Scanning tunneling microscopy of monoatomic gold chains on vicinal Si(335) surface: experimental and theoretical study

    Energy Technology Data Exchange (ETDEWEB)

    Krawiec, M.; Kwapinski, T.; Jalochowski, M. [Institute of Physics and Nanotechnology Center, M. Curie-Sklodowska University, pl. M. Curie-Sklodowskiej 1, 20-031 Lublin (Poland)

    2005-02-01

    We study electronic and topographic properties of the Si(335) surface, containing Au wires parallel to the steps. We use scanning tunneling microscopy (STM) supplemented by reflection of high energy electron diffraction (RHEED) technique. The STM data show the space and voltage dependent oscillations of the distance between STM tip and the surface which can be explained within one band tight binding Hubbard model. We calculate the STM current using nonequilibrium Keldysh Green function formalism. (copyright 2005 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  15. Positron annihilation and electron microscopy study in the early stage of fatigue of polycrystalline copper

    International Nuclear Information System (INIS)

    Diaz, L.; Pareja, R.; Pedrosa, M.A.; Gonzalez, R.

    1985-01-01

    Positron annihilation and transmission electron microscopy are used to study the early stage of fatigue in polycrystalline copper cyclically deformed at various temperatures. The concentration of positron traps is correlated to the cumulative plastic strain and to the work done during deformation. The average lifetimes of the trapped positrons are (177 +- 4) and (186 +- 3) ps for samples fatigued at T 15 s -1 for the samples deformed at T <= 293 K. Vacancy clusters like small dislocation loops, are proposed as the main defects responsible for the positron trapping. (author)

  16. Transmission electron microscopy study of vertical quantum dots molecules grown by droplet epitaxy

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez-Maldonado, D., E-mail: david.hernandez@uca.es [Departamento de Ciencia de los Materiales e I.M. y Q.I., Facultad de Ciencias, Universidad de Cadiz, Campus Rio San Pedro, s/n, 11510 Puerto Real, Cadiz (Spain); Herrera, M.; Sales, D.L. [Departamento de Ciencia de los Materiales e I.M. y Q.I., Facultad de Ciencias, Universidad de Cadiz, Campus Rio San Pedro, s/n, 11510 Puerto Real, Cadiz (Spain); Alonso-Gonzalez, P.; Gonzalez, Y.; Gonzalez, L. [Instituto de Microelectronica de Madrid (CNM-CSIC), Isaac Newton 8 (PTM), 28760 Tres Cantos, Madrid (Spain); Pizarro, J.; Galindo, P.L. [Departamento de Lenguajes y Sistemas Informaticos, CASEM, Universidad de Cadiz, Campus Rio San Pedro, s/n, 11510 Puerto Real, Cadiz (Spain); Molina, S.I. [Departamento de Ciencia de los Materiales e I.M. y Q.I., Facultad de Ciencias, Universidad de Cadiz, Campus Rio San Pedro, s/n, 11510 Puerto Real, Cadiz (Spain)

    2010-07-01

    The compositional distribution of InAs quantum dots grown by molecular beam epitaxy on GaAs capped InAs quantum dots has been studied in this work. Upper quantum dots are nucleated preferentially on top of the quantum dots underneath, which have been nucleated by droplet epitaxy. The growth process of these nanostructures, which are usually called as quantum dots molecules, has been explained. In order to understand this growth process, the analysis of the strain has been carried out from a 3D model of the nanostructure built from transmission electron microscopy images sensitive to the composition.

  17. Light-free magnetic resonance force microscopy for studies of electron spin polarized systems

    International Nuclear Information System (INIS)

    Pelekhov, Denis V.; Selcu, Camelia; Banerjee, Palash; Chung Fong, Kin; Chris Hammel, P.; Bhaskaran, Harish; Schwab, Keith

    2005-01-01

    Magnetic resonance force microscopy is a scanned probe technique capable of three-dimensional magnetic resonance imaging. Its excellent sensitivity opens the possibility for magnetic resonance studies of spin accumulation resulting from the injection of spin polarized currents into a para-magnetic collector. The method is based on mechanical detection of magnetic resonance which requires low noise detection of cantilever displacement; so far, this has been accomplished using optical interferometry. This is undesirable for experiments on doped silicon, where the presence of light is known to enhance spin relaxation rates. We report a non-optical displacement detection scheme based on sensitive microwave capacitive readout

  18. Transmission electron microscopy studies on nanometer-sized ω phase produced in Gum Metal

    International Nuclear Information System (INIS)

    Yano, Takaaki; Murakami, Yasukazu; Shindo, Daisuke; Hayasaka, Yuichiro; Kuramoto, Shigeru

    2010-01-01

    The morphology, numerical density and average spacing of the ω phase formed in Gum Metal, a Ti-based alloy showing unique mechanical properties, were studied by transmission electron microscopy. Based on dark-field image observations and precise thickness measurements using a thin-foil specimen, the average spacing of the nanometer-sized ω phase was determined to be 6 nm. This spacing appeared to be sufficiently small for trapping dislocations. The results are discussed in conjunction with the dislocation-free deformation mechanism proposed for Gum Metal.

  19. Transmission electron microscopy study of vertical quantum dots molecules grown by droplet epitaxy

    International Nuclear Information System (INIS)

    Hernandez-Maldonado, D.; Herrera, M.; Sales, D.L.; Alonso-Gonzalez, P.; Gonzalez, Y.; Gonzalez, L.; Pizarro, J.; Galindo, P.L.; Molina, S.I.

    2010-01-01

    The compositional distribution of InAs quantum dots grown by molecular beam epitaxy on GaAs capped InAs quantum dots has been studied in this work. Upper quantum dots are nucleated preferentially on top of the quantum dots underneath, which have been nucleated by droplet epitaxy. The growth process of these nanostructures, which are usually called as quantum dots molecules, has been explained. In order to understand this growth process, the analysis of the strain has been carried out from a 3D model of the nanostructure built from transmission electron microscopy images sensitive to the composition.

  20. Study on orientation mechanisms of poly(vinylidenefluoride-trifluoroethylene) molecules aligned by atomic force microscopy

    International Nuclear Information System (INIS)

    Kimura, Kuniko; Kobayashi, Kei; Yamada, Hirofumi; Horiuchi, Toshihisa; Ishida, Kenji; Matsushige, Kazumi

    2006-01-01

    We have developed a molecular orientation control technique for polymers utilizing contact-mode atomic force microscopy (AFM). In this paper, we studied the molecular alignment mechanism of this technique by applying it to poly(vinylidenefluoride-trifluoroethylene) (P(VDF-TrFE)). The resultant alignment and formed crystal size were strongly dependent on the temperature during the modification. They also depended on the scan line spacing of the modification. These results made the alignment mechanism clear. The obtained molecular alignment was stable against the heat treatment even at the temperatures just below T m

  1. Non-Invasive Study of Nerve Fibres using Laser Interference Microscopy

    DEFF Research Database (Denmark)

    Brazhe, A. R.; Brazhe, N. A.; Rodionova, N. N.

    2008-01-01

    This paper presents the results of a laser interference microscopy study of the morphology and dynamical properties of myelinated nerve fibres. We describe the principles of operation of the phase-modulated laser interference microscope and show how this novel technique allows us to obtain...... information non-invasively about the internal structure of different regions of a nerve fibre. We also analyse the temporal variations in the internal optical properties in order to detect the rhythmic activity in the nerve fibre at different time scales and to shed light on the underlying biological...

  2. In situ TEM observations of unusual nanocrystallization in a Ti-based bulk metallic glass

    International Nuclear Information System (INIS)

    Yan, M.; Wang, D.J.; Shen, J.; Qian, M.

    2011-01-01

    In situ transmission electron microscopy (TEM) has been used to witness the nanocrystallization of amorphous Ti 42.5 Cu 40 Zr 10 Ni 5 Sn 2.5 . A crystallization front exists to separate the TEM sample into two parts with different thermal stabilities. The number density of the crystallization products varies significantly, with the precipitate sizes ranging from a few nanometres to ∼100 nm. Detailed TEM analysis suggests that oxygen is the most likely reason for realizing the unusual nanocrystallization. External thermal analysis also indicates that oxygen affects the crystallization.

  3. Atomic force microscopy analysis of synthetic membranes applied in release studies

    Energy Technology Data Exchange (ETDEWEB)

    Olejnik, Anna, E-mail: annamar@amu.edu.pl; Nowak, Izabela

    2015-11-15

    Graphical abstract: - Highlights: • We compare eight synthetic membranes by atomic force microscopy. • We predict the behavior of membranes in the release experiments. • The polymeric synthetic membranes varied in shape and size. • We detect substructures in pores of cellulose esters and nylon membranes. • Substructures limit the release rate of active compound. - Abstract: Synthetic membranes are commonly used in drug release studies and are applied mostly in quality control. They contain pores through which the drug can be diffused directly into the receptor fluid. Investigation of synthetic membranes permits determination of their structure and characterization of their properties. We suggest that the preliminary characterization of the membranes can be relevant to the interpretation of the release results. The aim of this study was to compare eight synthetic membranes by using atomic force microscopy in order to predict and understand their behavior in the release experiments. The results proved that polytetrafluoroethylene membrane was not suitable for the release study of tetrapeptide due to its hydrophobic nature, thickness and the specific structure with high trapezoid shaped blocks. The additional substructures in pores of mixed cellulose esters and nylon membranes detected by AFM influenced the diffusion rate of the active compound. These findings indicate that the selection of the membrane for the release studies should be performed cautiously by taking into consideration the membrane properties and by analyzing them prior the experiment.

  4. Single-particle electron microscopy in the study of membrane protein structure.

    Science.gov (United States)

    De Zorzi, Rita; Mi, Wei; Liao, Maofu; Walz, Thomas

    2016-02-01

    Single-particle electron microscopy (EM) provides the great advantage that protein structure can be studied without the need to grow crystals. However, due to technical limitations, this approach played only a minor role in the study of membrane protein structure. This situation has recently changed dramatically with the introduction of direct electron detection device cameras, which allow images of unprecedented quality to be recorded, also making software algorithms, such as three-dimensional classification and structure refinement, much more powerful. The enhanced potential of single-particle EM was impressively demonstrated by delivering the first long-sought atomic model of a member of the biomedically important transient receptor potential channel family. Structures of several more membrane proteins followed in short order. This review recounts the history of single-particle EM in the study of membrane proteins, describes the technical advances that now allow this approach to generate atomic models of membrane proteins and provides a brief overview of some of the membrane protein structures that have been studied by single-particle EM to date. © The Author 2015. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  5. Atomic force microscopy analysis of synthetic membranes applied in release studies

    International Nuclear Information System (INIS)

    Olejnik, Anna; Nowak, Izabela

    2015-01-01

    Graphical abstract: - Highlights: • We compare eight synthetic membranes by atomic force microscopy. • We predict the behavior of membranes in the release experiments. • The polymeric synthetic membranes varied in shape and size. • We detect substructures in pores of cellulose esters and nylon membranes. • Substructures limit the release rate of active compound. - Abstract: Synthetic membranes are commonly used in drug release studies and are applied mostly in quality control. They contain pores through which the drug can be diffused directly into the receptor fluid. Investigation of synthetic membranes permits determination of their structure and characterization of their properties. We suggest that the preliminary characterization of the membranes can be relevant to the interpretation of the release results. The aim of this study was to compare eight synthetic membranes by using atomic force microscopy in order to predict and understand their behavior in the release experiments. The results proved that polytetrafluoroethylene membrane was not suitable for the release study of tetrapeptide due to its hydrophobic nature, thickness and the specific structure with high trapezoid shaped blocks. The additional substructures in pores of mixed cellulose esters and nylon membranes detected by AFM influenced the diffusion rate of the active compound. These findings indicate that the selection of the membrane for the release studies should be performed cautiously by taking into consideration the membrane properties and by analyzing them prior the experiment.

  6. Investigation of the agglomeration and amorphous transformation effects of neutron irradiation on the nanocrystalline silicon carbide (3C-SiC) using TEM and SEM methods

    Energy Technology Data Exchange (ETDEWEB)

    Huseynov, Elchin M., E-mail: elchin.h@yahoo.com [Department of Nanotechnology and Radiation Material Science, National Nuclear Research Center, Inshaatchilar pr. 4, AZ 1073 Baku (Azerbaijan); Institute of Radiation Problems of Azerbaijan National Academy of Sciences, B.Vahabzade 9, AZ 1143 Baku (Azerbaijan)

    2017-04-01

    Nanocrystalline 3C-SiC particles irradiated by neutron flux during 20 h in TRIGA Mark II light water pool type research reactor. Silicon carbide nanoparticles were analyzed by Scanning Electron Microscope (SEM) and Transmission Electron Microscopy (TEM) devices before and after neutron irradiation. The agglomeration of nanoparticles was studied comparatively before and after neutron irradiation. After neutron irradiation the amorphous layer surrounding the nanoparticles was analyzed in TEM device. Neutron irradiation defects in the 3C-SiC nanoparticles and other effects investigated by TEM device. The effect of irradiation on the crystal structure of the nanomaterial was studied by selected area electron diffraction (SAED) and electron diffraction patterns (EDP) analysis.

  7. Preparation of TEM specimen by cross-section technique

    International Nuclear Information System (INIS)

    Hamada, Shozo

    1986-01-01

    Transmission electron microscopy (TEM) is applied to the direct observation of the depth dependent damage structure in ion-irradiated stainless steel by using the cross-section technique; obtaining the TEM specimen from a slice of the irradiated stainless steel with thick Ni plating. Here has been developed the specimen preparation method of cross-section technique without heat treatment, which was necessary in the conventional method to strengthen the bonding between Ni and stainless steel. Nickel plating with good bonding to stainless steel is enabled by the following manner. First, the irradiated stainless steel is immersed in the Wood's nickel solution at room temperature for 60s to activate the surface, followed by the stricking for 300s at a current density of 300 A/m 2 in the solution to make fine and homogeneous nucleation of Ni on the stainless steel. Then, the sample is plated with Ni in the Watt's nickel plating solution at 333 K with current density of 900 ∼ 1,000 A/m 2 . The TEM disc is obtained by mechanical slicing from the specimen with Ni plating of more than 3 mm thickness. Electropolishing is accomplished by using both Ballmann method and jet electropolishing to perforate the disc accurately at the aimed point for the observation of the damage structure. (author)

  8. Mobile microscopy as a screening tool for oral cancer in India: A pilot study.

    Directory of Open Access Journals (Sweden)

    Arunan Skandarajah

    Full Text Available Oral cancer is the most common type of cancer among men in India and other countries in South Asia. Late diagnosis contributes significantly to this mortality, highlighting the need for effective and specific point-of-care diagnostic tools. The same regions with high prevalence of oral cancer have seen extensive growth in mobile phone infrastructure, which enables widespread access to telemedicine services. In this work, we describe the evaluation of an automated tablet-based mobile microscope as an adjunct for telemedicine-based oral cancer screening in India. Brush biopsy, a minimally invasive sampling technique was combined with a simplified staining protocol and a tablet-based mobile microscope to facilitate local collection of digital images and remote evaluation of the images by clinicians. The tablet-based mobile microscope (CellScope device combines an iPad Mini with collection optics, LED illumination and Bluetooth-controlled motors to scan a slide specimen and capture high-resolution images of stained brush biopsy samples. Researchers at the Mazumdar Shaw Medical Foundation (MSMF in Bangalore, India used the instrument to collect and send randomly selected images of each slide for telepathology review. Evaluation of the concordance between gold standard histology, conventional microscopy cytology, and remote pathologist review of the images was performed as part of a pilot study of mobile microscopy as a screening tool for oral cancer. Results indicated that the instrument successfully collected images of sufficient quality to enable remote diagnoses that show concordance with existing techniques. Further studies will evaluate the effectiveness of oral cancer screening with mobile microscopy by minimally trained technicians in low-resource settings.

  9. A TEM study of martensite habit planes and orientation relationships in Cu-Al-Ni shape memory alloys using a fast Δg-based method

    International Nuclear Information System (INIS)

    No, M.L.; Caillard, D.; San Juan, J.

    2009-01-01

    Shape memory alloys undergo a martensitic transformation, where thermomechanical properties are basically controlled by the austenite-martensite interphases, exhibiting complex orientation relationships and irrational habit planes. They are usually determined by the phenomenological theory. In this work an experimental study of nine different habit planes and orientation relationships is first realized. Then, an analysis of the interphases in the reciprocal space shows that they cannot be univocally determined by the usual two-dimensional edge-to-edge matching method. Finally, we propose a new method, based on the three-dimensional edge-to-edge matching of dense planes across the interface, to determine the habit planes and the orientation relationships. This method requires only one selected area diffraction pattern on the edge-on interface and a three-dimensional simulation of the reciprocal lattices of both structures. The habit planes determined on CuAlNi by this method agree with the values proposed by the phenomenological theory

  10. Numerical study of the lateral resolution in electrostatic force microscopy for dielectric samples

    International Nuclear Information System (INIS)

    Riedel, C; AlegrIa, A; Colmenero, J; Schwartz, G A; Saenz, J J

    2011-01-01

    We present a study of the lateral resolution in electrostatic force microscopy for dielectric samples in both force and gradient modes. Whereas previous studies have reported expressions for metallic surfaces having potential heterogeneities (Kelvin probe force microscopy), in this work we take into account the presence of a dielectric medium. We introduce a definition of the lateral resolution based on the force due to a test particle being either a point charge or a polarizable particle on the dielectric surface. The behaviour has been studied over a wide range of typical experimental parameters: tip-sample distance (1-20) nm, sample thickness (0-5) μm and dielectric constant (1-20), using the numerical simulation of the equivalent charge method. For potential heterogeneities on metallic surfaces expressions are in agreement with the bibliography. The lateral resolution of samples having a dielectric constant of more than 10 tends to metallic behaviour. We found a characteristic thickness of 100 nm, above which the lateral resolution measured on the dielectric surface is close to that of an infinite medium. As previously reported, the lateral resolution is better in the gradient mode than in the force mode. Finally, we showed that for the same experimental conditions, the lateral resolution is better for a polarizable particle than for a charge, i.e. dielectric heterogeneities should always look 'sharper' (better resolved) than inhomogeneous charge distributions. This fact should be taken into account when interpreting images of heterogeneous samples.

  11. Binding studies of costunolide and dehydrocostuslactone with HSA by spectroscopy and atomic force microscopy

    International Nuclear Information System (INIS)

    Gao Wenhua; Li Nana; Chen Gaopan; Xu Yanping; Chen Yaowen; Hu Shunlin; Hu Zhide

    2011-01-01

    Human serum albumin (HSA), a major plasma protein and plasma-derived therapeutic, interacts with a wide variety of drugs and native plasma metabolites. In this study the interactions of costunolide (CE) and dehydrocostuslactone (DE) with HSA were investigated by molecule modeling, atomic force microscopy (AFM), and different optical techniques. In the mechanism discussion, it was proved that fluorescence quenching of HSA by both of the drugs is a result of the formation of drug-HSA complexes. Binding parameters for the reactions were determined according to the Stern-Volmer equation and static quenching. The results of thermodynamic parameters ΔG 0 , ΔH 0 , and ΔS 0 at different temperatures indicated that hydrogen bonding interactions play a major role in the drug-HSA associations process. The binding properties were further studied by quantitative analysis of CD, FTIR, and Raman spectra. Furthermore, AFM results showed that the dimension of HSA molecules became more swollen after binding with the drugs. - Highlights: → Interactions of costunolide and dehydrocostuslactone with HSA have been investigated for the first time. → Raman spectra were used to analyze the drug-HSA interactions. → Atomic force microscopy has been used to study the topography change of HSA by addition of the drugs. → These results are important for the drugs containing costunolide and dehydrocostuslactone distribution and metabolism.

  12. Numerical study of the lateral resolution in electrostatic force microscopy for dielectric samples

    Energy Technology Data Exchange (ETDEWEB)

    Riedel, C; AlegrIa, A; Colmenero, J [Departamento de Fisica de Materiales UPV/EHU, Facultad de Quimica, Apartado 1072, 20080 San Sebastian (Spain); Schwartz, G A [Centro de Fisica de Materiales CSIC-UPV/EHU, Paseo Manuel de Lardizabal 5, 20018 San Sebastian (Spain); Saenz, J J, E-mail: riedel@ies.univ-montp2.fr [Donostia International Physics Center, Paseo Manuel de Lardizabal 4, 20018 San Sebastian (Spain)

    2011-07-15

    We present a study of the lateral resolution in electrostatic force microscopy for dielectric samples in both force and gradient modes. Whereas previous studies have reported expressions for metallic surfaces having potential heterogeneities (Kelvin probe force microscopy), in this work we take into account the presence of a dielectric medium. We introduce a definition of the lateral resolution based on the force due to a test particle being either a point charge or a polarizable particle on the dielectric surface. The behaviour has been studied over a wide range of typical experimental parameters: tip-sample distance (1-20) nm, sample thickness (0-5) {mu}m and dielectric constant (1-20), using the numerical simulation of the equivalent charge method. For potential heterogeneities on metallic surfaces expressions are in agreement with the bibliography. The lateral resolution of samples having a dielectric constant of more than 10 tends to metallic behaviour. We found a characteristic thickness of 100 nm, above which the lateral resolution measured on the dielectric surface is close to that of an infinite medium. As previously reported, the lateral resolution is better in the gradient mode than in the force mode. Finally, we showed that for the same experimental conditions, the lateral resolution is better for a polarizable particle than for a charge, i.e. dielectric heterogeneities should always look 'sharper' (better resolved) than inhomogeneous charge distributions. This fact should be taken into account when interpreting images of heterogeneous samples.

  13. In situ Transmission Electron Microscopy of catalyst sintering

    DEFF Research Database (Denmark)

    DeLaRiva, Andrew T.; Hansen, Thomas Willum; Challa, Sivakumar R.

    2013-01-01

    Recent advancements in the field of electron microscopy, such as aberration correctors, have now been integrated into Environmental Transmission Electron Microscopes (TEMs), making it possible to study the behavior of supported metal catalysts under operating conditions at atomic resolution. Here......, we focus on in situ electron microscopy studies of catalysts that shed light on the mechanistic aspects of catalyst sintering. Catalyst sintering is an important mechanism for activity loss, especially for catalysts that operate at elevated temperatures. Literature from the past decade is reviewed...... along with our recent in situ TEM studies on the sintering of Ni/MgAl2O4 catalysts. These results suggest that the rapid loss of catalyst activity in the earliest stages of catalyst sintering could result from Ostwald ripening rather than through particle migration and coalescence. The smallest...

  14. Fluorescence microscopy.

    Science.gov (United States)

    Sanderson, Michael J; Smith, Ian; Parker, Ian; Bootman, Martin D

    2014-10-01

    Fluorescence microscopy is a major tool with which to monitor cell physiology. Although the concepts of fluorescence and its optical separation using filters remain similar, microscope design varies with the aim of increasing image contrast and spatial resolution. The basics of wide-field microscopy are outlined to emphasize the selection, advantages, and correct use of laser scanning confocal microscopy, two-photon microscopy, scanning disk confocal microscopy, total internal reflection, and super-resolution microscopy. In addition, the principles of how these microscopes form images are reviewed to appreciate their capabilities, limitations, and constraints for operation. © 2014 Cold Spring Harbor Laboratory Press.

  15. Analytical TEM investigations of nanoscale magnetic materials

    International Nuclear Information System (INIS)

    Meingast, A.

    2015-01-01

    Analytical transmission electron microscopy has been applied within this thesis to investigate several novel approaches to design and fabricate nanoscale magnetic materials. As the size of the features of interest rank in the sub-nanometer range, it is necessary to employ techniques with a resolution – both spatial and analytical – well below this magnitude. Only at this performance level it is possible to examine material properties, necessary for the further tailoring of materials. Within this work two key aspects have been covered: First, analytical TEM (transmission electron microscopy) investigations were carried out to get insight into novel magnetic materials with high detail. Second, new analytical and imaging possibilities enabled with the commissioning of the new ASTEM (Austrian scanning transmission electron microscope) were explored. The aberration corrected TITAN® microscope (© FEI Company) allows resolving features in scanning transmission mode (STEM) with 70 pm distance. Thereby, direct imaging of light elements in STEM mode by using the annular bright field method becomes possible. Facilitated through high beam currents within the electron probe, an increased acquisition speed of analytical signals is possible. For energy dispersive X-ray spectroscopy (EDXS) a new four detector disc geometry around the specimen was implemented, which increases the accessible collection angle. With the integration of the latest generation of image filter and electron spectrometer (GIF QuantumERS), electron energy loss spectroscopy (EELS) is boosted through the high acquisition speed and the dual spectroscopy mode. The high acquisition speed allows to record up to 1000 spectra per second and the possibility to record atomically resolved EELS maps is at hand. Hereby it is important to avoid beam damage and alteration of the material during imaging and analysis. With the simultaneous acquisition of the low and the high loss spectral region, an extended range for

  16. Two-Photon Excitation Microscopy for the Study of Living Cells and Tissues

    Science.gov (United States)

    Benninger, Richard K.P.; Piston, David W.

    2013-01-01

    Two-photon excitation microscopy is an alternative to confocal microscopy that provides advantages for three-dimensional and deep tissue imaging. This unit will describe the basic physical principles behind two-photon excitation and discuss the advantages and limitations of its use in laser-scanning microscopy. The principal advantages of two-photon microscopy are reduced phototoxicity, increased imaging depth, and the ability to initiate highly localized photochemistry in thick samples. Practical considerations for the application of two-photon microscopy will then be discussed, including recent technological advances. This unit will conclude with some recent applications of two-photon microscopy that highlight the key advantages over confocal microscopy and the types of experiments which would benefit most from its application. PMID:23728746

  17. Kerr microscopy study of exchange-coupled FePt/Fe exchange spring magnets

    Energy Technology Data Exchange (ETDEWEB)

    Hussain, Zaineb; Kumar, Dileep [UGC-DAE Consortium for Scientific Research, University Campus, Khandwa Road, Indore 452001 (India); Reddy, V. Raghavendra, E-mail: varimalla@yahoo.com [UGC-DAE Consortium for Scientific Research, University Campus, Khandwa Road, Indore 452001 (India); Gupta, Ajay [Amity Center for Spintronic Materials, Amity University, Noida 201303 (India)

    2017-05-15

    Magnetization reversal and magnetic microstructure of top soft magnetic layer (Fe) in exchange spring coupled L1{sub 0} FePt/Fe is studied using high resolution Kerr microscopy. With remnant state of the hard magnetic layer (L1{sub 0} FePt) as initial condition, magnetization loops along with magnetic domains are recorded for the top soft magnetic layer (Fe) using Kerr microscopy. Considerable shifting of Fe layer hysteresis loop from center which is similar to exchange bias phenomena is observed. It is also observed that one can tune the magnitude of hysteresis shift by reaching the remanent state from different saturating fields (H{sub SAT}) and also by varying the angle between measuring field and H{sub SAT}. The hysteresis loops and magnetic domains of top soft Fe layer demonstrate unambiguously that soft magnetic layer at remanent state in such exchange coupled system is having unidirectional anisotropy. An analogy is drawn and the observations are explained in terms of established model of exchange bias phenomena framed for field-cooled ferromagnetic - antiferromagnetic bilayer systems. - Highlights: • Kerr microscopy of top soft magnetic Fe layer in exchange spring coupled L1{sub 0} FePt (30 nm)/Fe (22 nm) is reported. • Considerable shifting of Fe layer hysteresis loop from center which is similar to exchange bias phenomena is observed. • Tuneable nature of magnitude of hysteresis shift is shown. • It is unambiguously shown that the top soft Fe magnetic layer at remanent state is having unidirectional anisotropy.

  18. Illuminating Electron Microscopy of Photocatalysts

    DEFF Research Database (Denmark)

    Cavalca, Filippo

    Photocatalysts are of fundamental interest for sustainable energy research because of their wide range of applications and great potential for state of the art and future usages [1]. By means of Transmission Electron Microscopy (TEM) it is possible to give a deep insight in the structure, composi...

  19. Transmission electron microscopy of bone

    NARCIS (Netherlands)

    Everts, Vincent; Niehof, Anneke; Tigchelaar-Gutter, Wikky; Beertsen, Wouter

    2012-01-01

    This chapter describes procedures to process mineralized tissues obtained from different sources for transmission electron microscopy (TEM). Methods for fixation, resin embedding, staining of semi-thin sections and ultrathin sections are presented. In addition, attention will be paid to processing

  20. DNA adsorption and desorption on mica surface studied by atomic force microscopy

    International Nuclear Information System (INIS)

    Sun Lanlan; Zhao Dongxu; Zhang Yue; Xu Fugang; Li Zhuang

    2011-01-01

    The adsorption of DNA molecules on mica surface and the following desorption of DNA molecules at ethanol-mica interface were studied using atomic force microscopy. By changing DNA concentration, different morphologies on mica surface have been observed. A very uniform and orderly monolayer of DNA molecules was constructed on the mica surface with a DNA concentration of 30 ng/μL. When the samples were immersed into ethanol for about 15 min, various desorption degree of DNA from mica (0-99%) was achieved. It was found that with the increase of DNA concentration, the desorption degree of DNA from the mica at ethanol-mica interface decreased. And when the uniform and orderly DNA monolayers were formed on the mica surface, almost no DNA molecule desorbed from the mica surface in this process. The results indicated that the uniform and orderly DNA monolayer is one of the most stable DNA structures formed on the mica surface. In addition, we have studied the structure change of DNA molecules after desorbed from the mica surface with atomic force microscopy, and found that the desorption might be ascribed to the ethanol-induced DNA condensation.

  1. DNA adsorption and desorption on mica surface studied by atomic force microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Sun Lanlan [State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Graduate school of the Chinese Academy of Sciences, Chinese Academy of Sciences, Renmin Street 5625, Changchun 130022 (China); Key Laboratory of Excited State Processes, Changchun Institute of Optics, Fine Mechanics and Physics, Chinese Academy of Sciences, 16 East Nan-Hu Road, Open Economic Zone, Changchun 130033 (China); Zhao Dongxu [Key Laboratory of Excited State Processes, Changchun Institute of Optics, Fine Mechanics and Physics, Chinese Academy of Sciences, 16 East Nan-Hu Road, Open Economic Zone, Changchun 130033 (China); Zhang Yue; Xu Fugang [State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Graduate school of the Chinese Academy of Sciences, Chinese Academy of Sciences, Renmin Street 5625, Changchun 130022 (China); Li Zhuang, E-mail: zli@ciac.jl.cn [State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Graduate school of the Chinese Academy of Sciences, Chinese Academy of Sciences, Renmin Street 5625, Changchun 130022 (China)

    2011-05-15

    The adsorption of DNA molecules on mica surface and the following desorption of DNA molecules at ethanol-mica interface were studied using atomic force microscopy. By changing DNA concentration, different morphologies on mica surface have been observed. A very uniform and orderly monolayer of DNA molecules was constructed on the mica surface with a DNA concentration of 30 ng/{mu}L. When the samples were immersed into ethanol for about 15 min, various desorption degree of DNA from mica (0-99%) was achieved. It was found that with the increase of DNA concentration, the desorption degree of DNA from the mica at ethanol-mica interface decreased. And when the uniform and orderly DNA monolayers were formed on the mica surface, almost no DNA molecule desorbed from the mica surface in this process. The results indicated that the uniform and orderly DNA monolayer is one of the most stable DNA structures formed on the mica surface. In addition, we have studied the structure change of DNA molecules after desorbed from the mica surface with atomic force microscopy, and found that the desorption might be ascribed to the ethanol-induced DNA condensation.

  2. Deformation of nanotubes in peeling contact with flat substrate: An in situ electron microscopy nanomechanical study

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Xiaoming; Zheng, Meng; Wei, Qing; Ke, Changhong, E-mail: cke@binghamton.edu [Department of Mechanical Engineering, State University of New York at Binghamton, Binghamton, New York 13902-6000 (United States); Signetti, Stefano [Laboratory of Bio-Inspired and Graphene Nanomechanics, Department of Civil, Environmental and Mechanical Engineering, University of Trento, Trento (Italy); Pugno, Nicola M. [Laboratory of Bio-Inspired and Graphene Nanomechanics, Department of Civil, Environmental and Mechanical Engineering, University of Trento, Trento (Italy); Centre for Materials and Microsystems, Fondazione Bruno Kessler, Povo (Trento) (Italy); School of Engineering and Materials Science, Queen Mary University of London, London (United Kingdom)

    2016-04-21

    Peeling of one-dimensional (1D) nanostructures from flat substrates is an essential technique in studying their adhesion properties. The mechanical deformation of the nanostructure in the peeling experiment is critical to the understanding of the peeling process and the interpretation of the peeling measurements, but it is challenging to measure directly and quantitatively at the nanoscale. Here, we investigate the peeling deformation of a bundled carbon nanotube (CNT) fiber by using an in situ scanning electron microscopy nanomechanical peeling technique. A pre-calibrated atomic force microscopy cantilever is utilized as the peeling force sensor, and its back surface acts as the peeling contact substrate. The nanomechanical peeling scheme enables a quantitative characterization of the deformational behaviors of the CNT fiber in both positive and negative peeling configurations with sub-10 nm spatial and sub-nN force resolutions. Nonlinear continuum mechanics models and finite element simulations are employed to interpret the peeling measurements. The measurements and analysis reveal that the structural imperfections in the CNT fiber may have a substantial influence on its peeling deformations and the corresponding peeling forces. The research findings reported in this work are useful to the study of mechanical and adhesion properties of 1D nanostructures by using nanomechanical peeling techniques.

  3. A pilot study of short-duration sputum pretreatment procedures for optimizing smear microscopy for tuberculosis.

    Directory of Open Access Journals (Sweden)

    Peter Daley

    2009-05-01

    Full Text Available Direct sputum smear microscopy for tuberculosis (TB lacks sensitivity for the detection of acid fast bacilli. Sputum pretreatment procedures may enhance sensitivity. We did a pilot study to compare the diagnostic accuracy and incremental yield of two short-duration (<1 hour sputum pretreatment procedures to optimize direct smears among patients with suspected TB at a referral hospital in India.Blinded laboratory comparison of bleach and universal sediment processing (USP pretreated centrifuged auramine smears to direct Ziehl-Neelsen (ZN and direct auramine smears and to solid (Loweinstein-Jensen (LJ and liquid (BACTEC 460 culture. 178 pulmonary and extrapulmonary TB suspects were prospectively recruited during a one year period. Thirty six (20.2% were positive by either solid or liquid culture. Direct ZN smear detected 22 of 36 cases and direct auramine smears detected 26 of 36 cases. Bleach and USP centrifugation detected 24 cases each, providing no incremental yield beyond direct smears. When compared to combined culture, pretreated smears were not more sensitive than direct smears (66.6% vs 61.1 (ZN or 72.2 (auramine, and were not more specific (92.3% vs 93.0 (ZN or 97.2 (auramine.Short duration sputum pretreatment with bleach and USP centrifugation did not increase yield as compared to direct sputum smears. Further work is needed to confirm this in a larger study and also determine if longer duration pre-treatment might be effective in optimizing smear microscopy for TB.

  4. Oil refinery dusts: morphological and size analysis by TEM.

    Science.gov (United States)

    Sielicki, Przemysław; Janik, Helena; Guzman, Agnieszka; Broniszewski, Mieczysław; Namieśnik, Jacek

    2011-03-01

    The objectives of this work were to develop a means of sampling atmospheric dusts on the premises of an oil refinery for electron microscopic study to carry out preliminary morphological analyses and to compare these dusts with those collected at sites beyond the refinery limits. Carbon and collodion membranes were used as a support for collection of dust particles straight on transmission electron microscopy (TEM) grids. Micrographs of the dust particles were taken at magnifications from ×4,000 to ×80,000 with a Tesla BS500 transmission electron microscope. Four parameters were defined on the basis of the micrographs: surface area, Feret diameter, circumference, and shape coefficient. The micrographs and literature data were used to classify the atmospheric dusts into six groups: particles with an irregular shape and rounded edges; particles with an irregular shape and sharp edges; soot and its aggregates; spherical particles; singly occurring, ultrafine dust particles; and particles not allocated to any of the previous five groups. The types of dusts found in all the samples were similar, although differences did exist between the various morphological parameters. Dust particles with the largest Feret diameter were present in sample 3 (mean, 0.739 μm)-these were collected near the refinery's effluent treatment plant. The particles with the smallest diameter were found in the sample that had been intended to be a reference sample for the remaining results (mean, 0.326 μm). The dust particles collected in the refinery had larger mean Feret diameters, even 100% larger, than those collected beyond it. Particles with diameters from 0.1 to 0.2 μm made up the most numerous group in all the samples collected in the refinery.

  5. Oil refinery dusts: morphological and size analysis by TEM

    Energy Technology Data Exchange (ETDEWEB)

    Sielicki, Przemyslaw; Janik, Helena; Guzman, Agnieszka [Gdansk University of Technology, Department of Polymer Technology, Chemical Faculty, Gdansk (Poland); Broniszewski, Mieczyslaw [Environmental Protection Office, Lotos Group, Gdansk (Poland); Namiesnik, Jacek [Gdansk University of Technology, Department of Analytical Chemistry, Chemical Faculty, Gdansk (Poland)

    2011-03-15

    The objectives of this work were to develop a means of sampling atmospheric dusts on the premises of an oil refinery for electron microscopic study to carry out preliminary morphological analyses and to compare these dusts with those collected at sites beyond the refinery limits. Carbon and collodion membranes were used as a support for collection of dust particles straight on transmission electron microscopy (TEM) grids. Micrographs of the dust particles were taken at magnifications from x 4,000 to x 80,000 with a Tesla BS500 transmission electron microscope. Four parameters were defined on the basis of the micrographs: surface area, Feret diameter, circumference, and shape coefficient. The micrographs and literature data were used to classify the atmospheric dusts into six groups: particles with an irregular shape and rounded edges; particles with an irregular shape and sharp edges; soot and its aggregates; spherical particles; singly occurring, ultrafine dust particles; and particles not allocated to any of the previous five groups. The types of dusts found in all the samples were similar, although differences did exist between the various morphological parameters. Dust particles with the largest Feret diameter were present in sample 3 (mean, 0.739 {mu}m) - these were collected near the refinery's effluent treatment plant. The particles with the smallest diameter were found in the sample that had been intended to be a reference sample for the remaining results (mean, 0.326 {mu}m). The dust particles collected in the refinery had larger mean Feret diameters, even 100% larger, than those collected beyond it. Particles with diameters from 0.1 to 0.2 {mu}m made up the most numerous group in all the samples collected in the refinery. (orig.)

  6. Nickel oxide reduction studied by environmental TEM

    DEFF Research Database (Denmark)

    Jeangros, Q.; Hansen, Thomas Willum; Wagner, Jakob Birkedal

    2012-01-01

    In situ reduction of an industrial NiO powder is performed under 1.3 mbar of H2 (2 mlN/min) in a differentially pumped FEI Titan 80-300 environmental transmission electron microscope (ETEM). Images, diffraction patterns and electron energy loss spectra (EELS) are acquired to monitor the structura...

  7. Correlative scanning-transmission electron microscopy reveals that a chimeric flavivirus is released as individual particles in secretory vesicles.

    Directory of Open Access Journals (Sweden)

    Julien Burlaud-Gaillard

    Full Text Available The intracellular morphogenesis of flaviviruses has been well described, but flavivirus release from the host cell remains poorly documented. We took advantage of the optimized production of an attenuated chimeric yellow fever/dengue virus for vaccine purposes to study this phenomenon by microscopic approaches. Scanning electron microscopy (SEM showed the release of numerous viral particles at the cell surface through a short-lived process. For transmission electron microscopy (TEM studies of the intracellular ultrastructure of the small number of cells releasing viral particles at a given time, we developed a new correlative microscopy method: CSEMTEM (for correlative scanning electron microscopy - transmission electron microscopy. CSEMTEM analysis suggested that chimeric flavivirus particles were released as individual particles, in small exocytosis vesicles, via a regulated secretory pathway. Our morphological findings provide new insight into interactions between flaviviruses and cells and demonstrate that CSEMTEM is a useful new method, complementary to SEM observations of biological events by intracellular TEM investigations.

  8. Study by electronic microscopy of corrosion features of graphite after hot oxidation (air, 620 C)

    International Nuclear Information System (INIS)

    Jodon de Villeroche, Suzanne

    1968-01-01

    The author reports the study of corrosion features of graphite after hot oxidation in the air at 620 C. It is based on observations made by electronic microscopy. This study comes after another one dedicated to oxidation features obtained by hot corrosion of natural graphite, and aims at comparing pyrolytic graphite before and after irradiation in an atomic pile, and at performing tests on a graphite processed with ozone. After a recall of generalities about natural graphite and of some issues related to hot corrosion of natural graphite, the author presents some characteristics and features of irradiated and non-irradiated pyrolytic graphite. He reports the study of the oxidation of samples of pyrolytic graphite: production of thin lamellae, production of glaze-carbon replicates, oxidation of irradiated and of non-irradiated graphite, healing of irradiation defects, and oxidation of ozone-processed natural graphite [fr

  9. Electron microscopy study of Ni induced crystallization in amorphous Si thin films

    International Nuclear Information System (INIS)

    Radnóczi, G. Z.; Battistig, G.; Pécz, B.; Dodony, E.; Vouroutzis, N.; Stoemenos, J.; Frangis, N.; Kovács, A.

    2015-01-01

    The crystallization of amorphous silicon is studied by transmission electron microscopy. The effect of Ni on the crystallization is studied in a wide temperature range heating thinned samples in-situ inside the microscope. Two cases of limited Ni source and unlimited Ni source are studied and compared. NiSi 2 phase started to form at a temperature as low as 250°C in the limited Ni source case. In-situ observation gives a clear view on the crystallization of silicon through small NiSi 2 grain formation. The same phase is observed at the crystallization front in the unlimited Ni source case, where a second region is also observed with large grains of Ni 3 Si 2 . Low temperature experiments show, that long annealing of amorphous silicon at 410 °C already results in large crystallized Si regions due to the Ni induced crystallization

  10. High resolution, high speed ultrahigh vacuum microscopy

    International Nuclear Information System (INIS)

    Poppa, Helmut

    2004-01-01

    The history and future of transmission electron microscopy (TEM) is discussed as it refers to the eventual development of instruments and techniques applicable to the real time in situ investigation of surface processes with high resolution. To reach this objective, it was necessary to transform conventional high resolution instruments so that an ultrahigh vacuum (UHV) environment at the sample site was created, that access to the sample by various in situ sample modification procedures was provided, and that in situ sample exchanges with other integrated surface analytical systems became possible. Furthermore, high resolution image acquisition systems had to be developed to take advantage of the high speed imaging capabilities of projection imaging microscopes. These changes to conventional electron microscopy and its uses were slowly realized in a few international laboratories over a period of almost 40 years by a relatively small number of researchers crucially interested in advancing the state of the art of electron microscopy and its applications to diverse areas of interest; often concentrating on the nucleation, growth, and properties of thin films on well defined material surfaces. A part of this review is dedicated to the recognition of the major contributions to surface and thin film science by these pioneers. Finally, some of the important current developments in aberration corrected electron optics and eventual adaptations to in situ UHV microscopy are discussed. As a result of all the path breaking developments that have led to today's highly sophisticated UHV-TEM systems, integrated fundamental studies are now possible that combine many traditional surface science approaches. Combined investigations to date have involved in situ and ex situ surface microscopies such as scanning tunneling microscopy/atomic force microscopy, scanning Auger microscopy, and photoemission electron microscopy, and area-integrating techniques such as x-ray photoelectron

  11. Garlic (Allium sativum) feeding impairs Sertoli cell junctional proteins in male Wistar rat testis: microscopy study.

    Science.gov (United States)

    Hammami, I; Nahdi, A; Atig, F; El May, A; El May, M V

    2016-12-01

    Sertoli cell junctions, such as adhesion junction (AJ), gap junction (GJ) and tight junction (TJ), are important for maintaining spermatogenesis. In previous studies, we showed the inhibitory effect of crude garlic (Allium sativum, As) on spermatogenesis and steroidogenesis. The aim of this work was to complete our investigation on the impact of this plant, especially on Sertoli cell junctional proteins (SCJPs). During 1 month, 24 male rats were divided into groups: group control (0% of As) and treated groups fed 5%, 10% and 15% of As. Light and electron microscopy observations were performed to localise junctional proteins: connexin-43, Zona Occluding-1 and N-cadherin (immunohistochemistry) and to describe junctions. We showed that the specific cells involved in the localisation of the SCJP were similar in both control and treated groups, but with different immunoreactivity intensity between them. The electron microscopy observation focused on TJs between Sertoli cells, constituting the blood-testis barrier, showed ultrastructural changes such as fragmentation of TJs between adjacent Sertoli cell membranes and dilatation of rough endoplasmic reticulum saccules giving an aspect of scale to these junctions. We concluded that crude garlic consumption during 1 month induces perturbations on Sertoli cell junctions. These alterations can explain apoptosis in testicular germ cells previously showed. © 2016 Blackwell Verlag GmbH.

  12. A resolution study for electrostatic force microscopy on bimetallic samples using the boundary element method

    International Nuclear Information System (INIS)

    Shen Yongxing; Lee, Minhwan; Lee, Wonyoung; Barnett, David M; Pinsky, Peter M; Prinz, Friedrich B

    2008-01-01

    Electrostatic force microscopy (EFM) is a special design of non-contact atomic force microscopy used for detecting electrostatic interactions between the probe tip and the sample. Its resolution is limited by the finite probe size and the long-range characteristics of electrostatic forces. Therefore, quantitative analysis is crucial to understanding the relationship between the actual local surface potential distribution and the quantities obtained from EFM measurements. To study EFM measurements on bimetallic samples with surface potential inhomogeneities as a special case, we have simulated such measurements using the boundary element method and calculated the force component and force gradient component that would be measured by amplitude modulation (AM) EFM and frequency modulation (FM) EFM, respectively. Such analyses have been performed for inhomogeneities of various shapes and sizes, for different tip-sample separations and tip geometries, for different applied voltages, and for different media (e.g., vacuum or water) in which the experiment is performed. For a sample with a surface potential discontinuity, the FM-EFM resolution expression agrees with the literature; however, the simulation for AM-EFM suggests the existence of an optimal tip radius of curvature in terms of resolution. On the other hand, for samples with strip- and disk-shaped surface potential inhomogeneities, we have obtained quantitative expressions for the detectability size requirements as a function of experimental conditions for both AM- and FM-EFMs, which suggest that a larger tip radius of curvature is moderately favored for detecting the presence of such inhomogeneities

  13. Microstructure and properties of laser clad coatings studied by orientation imaging microscopy

    International Nuclear Information System (INIS)

    Ocelik, V.; Furar, I.; De Hosson, J.Th.M.

    2010-01-01

    In this work orientation imaging microscopy (OIM), based on electron backscatter diffraction in scanning electron microscopy, was employed to examine in detail the relationship between laser cladding processing parameters and he properties and the microstructure of single and overlapping laser tracks. The study was performed on thick (∼1 mm) Co-based coatings prepared by 2 kW Nd:YAG laser cladding a 42CrMo4 steel substrate using different laser beam scanning speeds (1.0-15 mm s -1 ). It was found that the directional growth of individual primary grains led to the formation of a typical solidification fiber texture. The dependence of this texture on the processing speed and the shape of the solidification front were investigated in detail. Strong epitaxial growth of Co grains on austenitic steel substrate grains was found, which did not depend on the laser beam scanning velocity. During laser cladding a strong temperature gradient exists just below the coating-substrate interface that promotes the formation of a Greninger-Troiano orientation relationship between martensitic plates and the original austenitic grain inside the heat affected zone: {1 1 1} γ ∼ 1 o to {1 1 0} α and γ ∼ 2 o to α . Relatively drastic changes in grain size at the internal coating interfaces did not exhibit sharp changes in microhardness.

  14. Systematic study of alginate-based microcapsules by micropipette aspiration and confocal fluorescence microscopy.

    Science.gov (United States)

    Kleinberger, Rachelle M; Burke, Nicholas A D; Dalnoki-Veress, Kari; Stöver, Harald D H

    2013-10-01

    Micropipette aspiration and confocal fluorescence microscopy were used to study the structure and mechanical properties of calcium alginate hydrogel beads (A beads), as well as A beads that were additionally coated with poly-L-lysine (P) and sodium alginate (A) to form, respectively, AP and APA hydrogels. A beads were found to continue curing for up to 500 h during storage in saline, due to residual calcium chloride carried over from the gelling bath. In subsequent saline washes, micropipette aspiration proved to be a sensitive indicator of gel weakening and calcium loss. Aspiration tests were used to compare capsule stiffness before and after citrate extraction of calcium. They showed that the initial gel strength is largely due to the calcium alginate gel cores, while the long term strength is solely due to the poly-L-lysine-alginate polyelectrolyte complex (PEC) shells. Confocal fluorescence microscopy showed that calcium chloride exposure after PLL deposition led to PLL redistribution into the hydrogel bead, resulting in thicker but more diffuse and weaker PEC shells. Adding a final alginate coating to form APA capsules did not significantly change the PEC membrane thickness and stiffness, but did speed the loss of calcium from the bead core. © 2013.

  15. Electron microscopy of surfaces

    International Nuclear Information System (INIS)

    Venables, J.A.

    1981-01-01

    Electron beam techniques used to study clean surfaces and surface processes on a microscopic scale are reviewed. Recent experimental examples and possible future developments are discussed. Special emphasis is given to (i) transmission diffraction and microscopy techniques, including atomic imaging; (ii) Auger microscopy on bulk and thin film samples; (iii) secondary electron microscopy, especially low energy secondaries for work-function imaging and photoelectron imaging; and (iv) reflection electron microscopy and diffraction. (orig.)

  16. Evaluation of the therapeutic results of actinic keratosis treated with topical 5% fluorouracil by reflectance confocal laser microscopy: preliminary study*

    Science.gov (United States)

    Ishioka, Priscila; Maia, Marcus; Rodrigues, Sarita Bartholomei; Marta, Alessandra Cristina; Hirata, Sérgio Henrique

    2015-01-01

    Topical treatment for actinic keratosis with 5% fluorouracil has a recurrence rate of 54% in 12 months of follow-up. This study analyzed thirteen actinic keratoses on the upper limbs through confocal microscopy, at the time of clinical diagnosis and after 4 weeks of treatment with fluorouracil. After the treatment was established and evidence of clinical cure was achieved, in two of the nine actinic keratoses, confocal microscopy enabled visualization of focal areas of atypical honeycomb pattern in the epidermis indicating therapeutic failure. Preliminary data suggest the use of confocal microscopy as a tool for diagnosis and therapeutic control of actinic keratosis. PMID:26131881

  17. The study of optimal conditions of electrochemical etching of tunnel electron microscopy tungsten tips

    International Nuclear Information System (INIS)

    Anguiano, E.; Aguilar, M.; Olivar, A.I.

    1996-01-01

    We present the experimental results obtained during the study made in the electrochemical etching of tunneling electron microscopy tungsten tips. The experiments was made using DC and two usual electrolytes: KOH and NaOH. For the tip preparation we used a electrochemical cell with stainless steel cathode and the tungsten wire as anode. the electrodes was introduced in a glass recipient containing the electrolytic solution. We study the effects of applied voltage, polish time, tip length and electrolyte concentration as process relevant parameters. The best condition for tip preparation was obtained with a metallurgical microscope and with a SEM.EDX and Auger analysis was made. The results shown the better tips was made with KOH as electrolyte with a limited concentration range (2-4 normal) and applied voltage (2-6 volts) (Author) 20 refs

  18. Structural and dynamical aspects of skin studied by multiphoton excitation fluorescence microscopy-based methods

    DEFF Research Database (Denmark)

    Bloksgaard, Maria; Brewer, Jonathan R.; Bagatolli, Luis

    2013-01-01

    ' parameters. Specifically, by applying these methods, spatially resolved maps of water dipolar relaxation (generalized polarization function using the 6-lauroyl-2-(N,N-dimethylamino)naphthale probe), activity of protons (fluorescence lifetime imaging using a proton sensitive fluorescence probe--2,7-bis-(2......-carboxyethyl)-5-(and-6)-carboxyfluorescein) and diffusion coefficients of distinct fluorescence probes (raster imaging correlation spectroscopy) can be obtained from different regions of the tissue. Comparative studies of different tissue strata, but also between equivalent regions of normal and abnormal......This mini-review reports on applications of particular multiphoton excitation microscopy-based methodologies employed in our laboratory to study skin. These approaches allow in-depth optical sectioning of the tissue, providing spatially resolved information on specific fluorescence probes...

  19. Electromigration in integrated circuit interconnects studied by X-ray microscopy

    CERN Document Server

    Schneider, G; Anderson, E; Bates, W; Salmassi, F; Nachimuthu, P; Pearson, A; Richardson, D; Hambach, D; Hoffmann, N; Hasse, W; Hoffmann, K

    2003-01-01

    To study mass transport phenomena in advanced microelectronic devices with X-rays requires penetration of dielectric and Si layers up to 30 mu m thick. X-ray imaging at 1.8 keV photon energy provides a high amplitude contrast between Cu or Al interconnects and dielectric layers and can penetrate through the required thickness. To perform X-ray microscopy at 1.8 keV, a new Ru/Si multilayer was designed for the transmission X-ray microscope XM-1 installed at the Advanced Light Source in Berkeley. The mass flow in a passivated Cu interconnect was studied at current densities up to 10 sup 7 A/cm sup 2. In addition, we demonstrated the high material contrast from different elements in integrated circuits with a resolution of about 40 nm.

  20. Study of the creep of germanium bi-crystals by X ray topography and electronic microscopy

    International Nuclear Information System (INIS)

    Gay, Marie-Odile

    1981-01-01

    This research thesis addresses the study of the microscopic as well as macroscopic aspect of the role of grain boundary during deformation, by studying the creep of Germanium bi-crystals. The objective was to observe interactions of network dislocations with the boundary as well as the evolution of dislocations in each grain. During the first stages of deformation, samples have been examined by X ray topography, a technique which suits well the observation of low deformed samples, provided their initial dislocation density is very low. At higher deformation, more conventional techniques of observation of sliding systems and electronic microscopy have been used. After some general recalls, the definition of twin boundaries and of their structure in terms of dislocation, a look at germanium deformation, and an overview of works performed on bi-crystals deformation, the author presents the experimental methods and apparatuses. He reports and discusses the obtained results at the beginning of deformation as well as during next phases

  1. Electromigration in integrated circuit interconnects studied by X-ray microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Schneider, G. E-mail: gschnei1@gwdg.de; Denbeaux, G.; Anderson, E.; Bates, W.; Salmassi, F.; Nachimuthu, P.; Pearson, A.; Richardson, D.; Hambach, D.; Hoffmann, N.; Hasse, W.; Hoffmann, K

    2003-01-01

    To study mass transport phenomena in advanced microelectronic devices with X-rays requires penetration of dielectric and Si layers up to 30 {mu}m thick. X-ray imaging at 1.8 keV photon energy provides a high amplitude contrast between Cu or Al interconnects and dielectric layers and can penetrate through the required thickness. To perform X-ray microscopy at 1.8 keV, a new Ru/Si multilayer was designed for the transmission X-ray microscope XM-1 installed at the Advanced Light Source in Berkeley. The mass flow in a passivated Cu interconnect was studied at current densities up to 10{sup 7} A/cm{sup 2}. In addition, we demonstrated the high material contrast from different elements in integrated circuits with a resolution of about 40 nm.

  2. The effect of cigarette smoke extract on thrombomodulin-thrombin binding: an atomic force microscopy study.

    Science.gov (United States)

    Wei, Yujie; Zhang, Xuejie; Xu, Li; Yi, Shaoqiong; Li, Yi; Fang, Xiaohong; Liu, Huiliang

    2012-10-01

    Cigarette smoking is a well-known risk factor for cardiovascular disease. Smoking can cause vascular endothelial dysfunction and consequently trigger haemostatic activation and thrombosis. However, the mechanism of how smoking promotes thrombosis is not fully understood. Thrombosis is associated with the imbalance of the coagulant system due to endothelial dysfunction. As a vital anticoagulation cofactor, thrombomodulin (TM) located on the endothelial cell surface is able to regulate intravascular coagulation by binding to thrombin, and the binding results in thrombosis inhibition. This work focused on the effects of cigarette smoke extract (CSE) on TM-thrombin binding by atomic force microscopy (AFM) based single-molecule force spectroscopy. The results from both in vitro and live-cell experiments indicated that CSE could notably reduce the binding probability of TM and thrombin. This study provided a new approach and new evidence for studying the mechanism of thrombosis triggered by cigarette smoking.

  3. Atomic force microscopy and scanning electron microscopy evaluation of efficacy of scaling and root planing using magnification: A randomized controlled clinical study

    Directory of Open Access Journals (Sweden)

    Ranjana Mohan

    2013-01-01

    Full Text Available Aim: A randomized controlled clinical study was undertaken to evaluate the effectiveness of scaling and root planing (SRP by using Magnifying Loupes (ML and dental operating microscope (DOM. Materials and Methods: A total of 90 human teeth scheduled for extraction from 18 patients aged between 25 and 65 years suffering from generalized chronic severe periodontitis were randomly assigned to three treatment groups. Group 1 consisted SRP performed without using magnification (unaided, Group 2-SRP with ML and Group 3-SRP with DOM. Following extractions, samples were prepared for (i evaluation of surface topography by atomic force microscopy, (ii presence of smear layer, debris by scanning electron microscopy (iii elemental analysis by energy dispersive X-ray analysis. Data was subjected to statistical analysis using analysis of variance, post-hoc (Tukey-HSD and Chi-square test. Results: Statistically significant (P < 0.001 difference was found among the different treatment groups. Group 3 was the best while Group 1 was the least effective technique for SRP. Order of efficacy in terms of the surface was found to be - Palatal < Lingual < Distal ≅ Mesial < Buccal. Efficiency in mandibular to maxillary teeth was found to be significant (P < 0.05, also anterior to posterior teeth (P < 0.05. Conclusion: Magnification tools significantly enhance the efficacy of supragingival and subgingival SRP.

  4. A study of phase separation in peptide-loaded HPMC films using T(zero)-modulated temperature DSC, atomic force microscopy, and scanning electron microscopy.

    Science.gov (United States)

    Hussain, Samana; Grandy, David B; Reading, Mike; Craig, Duncan Q M

    2004-07-01

    Despite the widespread use of drug-loaded polymeric systems, there is still considerable uncertainty with regard to the nature of the distribution of the drug within the polymer matrix. The aim of this investigation was to develop thermal and microscopic techniques whereby the miscibility and spatial distribution of a model peptide, cyclosporin A (CyA), in hydroxypropyl methylcellulose (HPMC) films may be studied. The new technique of T(zero)-modulated temperature differential scanning calorimetry (T(zero) MTDSC), scanning electron microscopy (SEM), and pulse force mode atomic force microscopy (PFM-AFM) were used in conjunction to study films prepared using a solvent evaporation process, with a solvent extraction study performed to elucidate the nature of the observed phases. T(zero) MTDSC studies showed glass transitions for both the HPMC and CycA, with the T(g) for the HPMC and CycA seen for the mixed systems. SEM showed two spherical phases of differing electron density. PFM-AFM also showed spheres of differing adhesion that increased in size on addition of drug. Pixel intensity analysis indicated that the smaller spheres corresponded to CycA. Exposure of the films to dichloromethane, in which CycA is soluble but HPMC is not, resulted in the presence of voids that corresponded well to the spheres suggested to correspond to the drug. It was concluded that the system had undergone extensive or complete phase separation, and that the thermal and microscopic techniques outlined above are an effective means by which this issue may be studied. Copyright 2004 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 93:1672-1681, 2004

  5. Local elasticity and adhesion of nanostructures on Drosophila melanogaster wing membrane studied using atomic force microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Wagner, Ryan, E-mail: rbwagner@purdue.edu [School of Mechanical Engineering, Purdue University, West Lafayette (United States); Brick Nanotechnology Center, Purdue University, West Lafayette (United States); Pittendrigh, Barry R. [Department of Entomology, University of Illinois, Champaign (United States); Raman, Arvind, E-mail: raman@purdue.edu [School of Mechanical Engineering, Purdue University, West Lafayette (United States); Brick Nanotechnology Center, Purdue University, West Lafayette (United States)

    2012-10-15

    Highlights: Black-Right-Pointing-Pointer We studied the wing membrane of Drosophila melanogaster with atomic force microscopy. Black-Right-Pointing-Pointer We report the structure, elasticity, and adhesion on the wing membrane in air and nitrogen environments. Black-Right-Pointing-Pointer Results provide insight into the nature of the wing membrane enabling the development of biomimetic surface and micro air vehicles. - Abstract: Insect wings have a naturally occurring, complex, functional, hierarchical microstructure and nanostructure, which enable a remarkably water-resistant and self-cleaning surface. Insect wings are used as a basis for engineering biomimetic materials; however, the material properties of these nanostructures such as local elastic modulus and adhesion are poorly understood. We studied the wings of the Canton-S strain of Drosophila melanogaster (hereafter referred to as Drosophila) with atomic force microscopy (AFM) to quantify the local material properties of Drosophila wing surface nanostructures. The wings are found to have a hierarchical structure of 10-20 {mu}m long, 0.5-1 {mu}m diameter hair, and at a much smaller scale, 100 nm diameter and 30-60 nm high bumps. The local properties of these nanoscale bumps were studied under ambient and dry conditions with force-volume AFM. The wing membrane was found to have a elastic modulus on the order of 1000 MPa and the work of adhesion between the probe and wing membrane surface was found to be on the order of 100 mJ/m{sup 2}, these properties are the same order of magnitude as common thermoplastic polymers such as polyethylene. The difference in work of adhesion between the nanoscale bump and membrane does not change significantly between ambient (relative humidity of 30%) or dry conditions. This suggests that the nanoscale bumps and the surrounding membrane are chemically similar and only work to increase hydrophobicity though surface roughening or the geometric lotus effect.

  6. Multiphoton microscopy: an efficient tool for in-situ study of cultural heritage artifacts

    Science.gov (United States)

    Latour, Gaël.; Echard, Jean-Philippe; Didier, Marie; Schanne-Klein, Marie-Claire

    2013-05-01

    We present multimodal nonlinear optical imaging of historical artifacts by combining Two-Photon Excited Fluorescence (2PEF) and Second Harmonic Generation (SHG) microscopies. Three-dimensional (3D) non-contact laser-scanning imaging with micrometer resolution is performed without any preparation of the objects under study. 2PEF signals are emitted by a wide range of fluorophores such as pigments and binder, which can be discriminated thanks to their different emission spectral bands by using suitable spectral filters in the detection channel. SHG signals are specific for dense non-centrosymmetric organizations such as the crystalline cellulose within the wood cell walls. We also show that plaster particles exhibit SHG signals. These particles are bassanite crystals with a non-centrosymmetric crystalline structure, while the other types of calcium sulphates exhibit a centrosymmetric crystalline structure with no SHG signal. In our study, we first characterize model single-layered samples: wood, gelatin-based films containing plaster or cochineal lake and sandarac film containing cochineal lake. We then study multilayered coating systems on wood and show that multimodal nonlinear microscopy successfully reveals the 3D distribution of all components within the stratified sample. We also show that the fine structure of the wood can be assessed, even through a thick multilayered varnish coating. Finally, in situ multimodal nonlinear imaging is demonstrated in a historical violin. SHG/2PEF imaging thus appears as an efficient non-destructive and contactless 3D imaging technique for in situ investigation of historical coatings and more generally for wood characterization and coating analysis at micrometer scale.

  7. Local elasticity and adhesion of nanostructures on Drosophila melanogaster wing membrane studied using atomic force microscopy

    International Nuclear Information System (INIS)

    Wagner, Ryan; Pittendrigh, Barry R.; Raman, Arvind

    2012-01-01

    Highlights: ► We studied the wing membrane of Drosophila melanogaster with atomic force microscopy. ► We report the structure, elasticity, and adhesion on the wing membrane in air and nitrogen environments. ► Results provide insight into the nature of the wing membrane enabling the development of biomimetic surface and micro air vehicles. - Abstract: Insect wings have a naturally occurring, complex, functional, hierarchical microstructure and nanostructure, which enable a remarkably water-resistant and self-cleaning surface. Insect wings are used as a basis for engineering biomimetic materials; however, the material properties of these nanostructures such as local elastic modulus and adhesion are poorly understood. We studied the wings of the Canton-S strain of Drosophila melanogaster (hereafter referred to as Drosophila) with atomic force microscopy (AFM) to quantify the local material properties of Drosophila wing surface nanostructures. The wings are found to have a hierarchical structure of 10–20 μm long, 0.5–1 μm diameter hair, and at a much smaller scale, 100 nm diameter and 30–60 nm high bumps. The local properties of these nanoscale bumps were studied under ambient and dry conditions with force-volume AFM. The wing membrane was found to have a elastic modulus on the order of 1000 MPa and the work of adhesion between the probe and wing membrane surface was found to be on the order of 100 mJ/m 2 , these properties are the same order of magnitude as common thermoplastic polymers such as polyethylene. The difference in work of adhesion between the nanoscale bump and membrane does not change significantly between ambient (relative humidity of 30%) or dry conditions. This suggests that the nanoscale bumps and the surrounding membrane are chemically similar and only work to increase hydrophobicity though surface roughening or the geometric lotus effect.

  8. Imaging and Quantification of Extracellular Vesicles by Transmission Electron Microscopy.

    Science.gov (United States)

    Linares, Romain; Tan, Sisareuth; Gounou, Céline; Brisson, Alain R

    2017-01-01

    Extracellular vesicles (EVs) are cell-derived vesicles that are present in blood and other body fluids. EVs raise major interest for their diverse physiopathological roles and their potential biomedical applications. However, the characterization and quantification of EVs constitute major challenges, mainly due to their small size and the lack of methods adapted for their study. Electron microscopy has made significant contributions to the EV field since their initial discovery. Here, we describe the use of two transmission electron microscopy (TEM) techniques for imaging and quantifying EVs. Cryo-TEM combined with receptor-specific gold labeling is applied to reveal the morphology, size, and phenotype of EVs, while their enumeration is achieved after high-speed sedimentation on EM grids.

  9. Environmental Transmission Electron Microscopy (ETEM) Studies of Single Iron Nanoparticle Carburization in Synthesis Gas

    DEFF Research Database (Denmark)

    Liu, Xi; Zhang, Chenghua; Li, Yongwang

    2017-01-01

    Structuralevolution of iron nanoparticles involving the formationand growth of iron carbide nuclei in the iron nanoparticle was directlyvisualized at the atomic level, using environmental transmission electronmicroscopy (TEM) under reactive conditions mimicking Fischer–Tropschsynthesis. Formation...... and electronenergy-loss spectra provides a detailed picture from initial activationto final degradation of iron under synthesis gas....

  10. Transient absorption microscopy studies of energy relaxation in graphene oxide thin film.

    Science.gov (United States)

    Murphy, Sean; Huang, Libai

    2013-04-10

    Spatial mapping of energy relaxation in graphene oxide (GO) thin films has been imaged using transient absorption microscopy (TAM). Correlated AFM images allow us to accurately determine the thickness of the GO films. In contrast to previous studies, correlated TAM-AFM allows determination of the effect of interactions of GO with the substrate and between stacked GO layers on the relaxation dynamics. Our results show that energy relaxation in GO flakes has little dependence on the substrate, number of stacked layers, and excitation intensity. This is in direct contrast to pristine graphene, where these factors have great consequences in energy relaxation. This suggests intrinsic factors rather than extrinsic ones dominate the excited state dynamics of GO films.

  11. Transient absorption microscopy studies of energy relaxation in graphene oxide thin film

    International Nuclear Information System (INIS)

    Murphy, Sean; Huang, Libai

    2013-01-01

    Spatial mapping of energy relaxation in graphene oxide (GO) thin films has been imaged using transient absorption microscopy (TAM). Correlated AFM images allow us to accurately determine the thickness of the GO films. In contrast to previous studies, correlated TAM–AFM allows determination of the effect of interactions of GO with the substrate and between stacked GO layers on the relaxation dynamics. Our results show that energy relaxation in GO flakes has little dependence on the substrate, number of stacked layers, and excitation intensity. This is in direct contrast to pristine graphene, where these factors have great consequences in energy relaxation. This suggests intrinsic factors rather than extrinsic ones dominate the excited state dynamics of GO films. (paper)

  12. Macroscopic Ensembles of Aligned Carbon Nanotubes in Bubble Imprints Studied by Polarized Raman Microscopy

    Directory of Open Access Journals (Sweden)

    Shota Ushiba

    2014-01-01

    Full Text Available We study the alignment of single-wall carbon nanotubes (SWCNTs in bubble imprints through polarized Raman microscopy. A hemispherical bubble containing SWCNTs is pressed against a glass substrate, resulting in an imprint of the bubble membrane with a coffee ring on the substrate. We find that macroscopic ensembles of aligned SWCNTs are obtained in the imprints, in which there are three patterns of orientations: (i azimuthal alignment on the coffee ring, (ii radial alignment at the edge of the membrane, and (iii random orientation at the center of the membrane. We also find that the alignment of SWCNTs in the imprints can be manipulated by spinning bubbles. The orientation of SWCNTs on the coffee ring is directed radially, which is orthogonal to the case of unspun bubbles. This approach enables one to align SWCNTs in large quantities and in a short time, potentially opening up a wide range of CNT-based electronic and optical applications.

  13. Nucleation of diamond by pure carbon ion bombardment--a transmission electron microscopy study

    International Nuclear Information System (INIS)

    Yao, Y.; Liao, M.Y.; Wang, Z.G.; Lifshitz, Y.; Lee, S.

    2005-01-01

    A cross-sectional high-resolution transmission electron microscopy (HRTEM) study of a film deposited by a 1 keV mass-selected carbon ion beam onto silicon held at 800 deg. C is presented. Initially, a graphitic film with its basal planes perpendicular to the substrate is evolving. The precipitation of nanodiamond crystallites in upper layers is confirmed by HRTEM, selected area electron diffraction, and electron energy loss spectroscopy. The nucleation of diamond on graphitic edges as predicted by Lambrecht et al. [W. R. L. Lambrecht, C. H. Lee, B. Segall, J. C. Angus, Z. Li, and M. Sunkara, Nature, 364 607 (1993)] is experimentally confirmed. The results are discussed in terms of our recent subplantation-based diamond nucleation model

  14. Devolatilization Studies of Oil Palm Biomass for Torrefaction Process through Scanning Electron Microscopy

    Science.gov (United States)

    Daud, D.; Abd. Rahman, A.; Shamsuddin, A. H.

    2016-03-01

    In this work, palm oil biomass consisting of empty fruit bunch (EFB), mesocarp fibre and palm kernel shell (PKS) were chosen as raw material for torrefaction process. Torrefaction process was conducted at various temperatures of 240 °C, 270 °C and 300 °C with a residence time of 60 minutes. The morphology of the raw and torrefied biomass was then observed through Scanning Electron Microscopy (SEM) images. Also, through this experiment the correlation between the torrefaction temperatures with the volatile gases released were studied. From the observation, the morphology structure of the biomass exhibited inter-particle gaps due to the release of volatile gases and it is obviously seen more at higher temperatures. Moreover, the change of the biomass structure is influenced by the alteration of the lignocellulose biomass.

  15. Atomic Force Microscopy Techniques for Nanomechanical Characterization: A Polymeric Case Study

    Science.gov (United States)

    Reggente, Melania; Rossi, Marco; Angeloni, Livia; Tamburri, Emanuela; Lucci, Massimiliano; Davoli, Ivan; Terranova, Maria Letizia; Passeri, Daniele

    2015-04-01

    Atomic force microscopy (AFM) is a versatile tool to perform mechanical characterization of surface samples at the nanoscale. In this work, we review two of such methods, namely contact resonance AFM (CR-AFM) and torsional harmonics AFM (TH-AFM). First, such techniques are illustrated and their applicability on materials with elastic moduli in different ranges are discussed, together with their main advantages and limitations. Then, a case study is presented in which we report the mechanical characterization using both CR-AFM and TH-AFM of polyaniline and polyaniniline doped with nanodiamond particles tablets prepared by a pressing process. We determined the indentation modulus values of their surfaces, which were found in fairly good agreement, thus demonstrating the accuracy of the techniques. Finally, the determined surface elastic moduli have been compared with the bulk ones measured through standard indentation testing.

  16. The Use of Atomic-Force Microscopy for Studying the Crystallization Process of Amorphous Alloys

    Science.gov (United States)

    Elmanov, G. N.; Ivanitskaya, E. A.; Dzhumaev, P. S.; Skrytniy, V. I.

    The crystallization process of amorphous alloys is accompanied by the volume changes as a result of structural phase transitions. This leads to changes in the surface topography, which was studied by atomic force microscopy (AFM). The changes of the surface topography, structure and phase composition during multistage crystallization process of the metallic glasses with composition Ni71,5Cr6,8Fe2,7B11,9Si7,1 and Ni63,4Cr7,4Fe4,3Mn0,8B15,6Si8,5 (AWS BNi2) has been investigated. The obtained results on changing of the surface topography in crystallization process are in good agreement with the data of X-ray diffraction analysis (XRD). The nature of redistribution of some alloy components in the crystallization process has been suggested.

  17. Atomic force microscopy study of anion intercalation into highly oriented pyrolytic graphite

    Energy Technology Data Exchange (ETDEWEB)

    Alliata, D; Haering, P; Haas, O; Koetz, R [Paul Scherrer Inst. (PSI), Villigen (Switzerland); Siegenthaler, H [University of Berne (Switzerland)

    1999-08-01

    In the context of ion transfer batteries, we studied highly oriented pyrolytic graphite (HOPG) in perchloric acid, as a model to elucidate the mechanism of electrochemical intercalation in graphite. Aim of the work is the local and time dependent investigation of dimensional changes of the host material during electrochemical intercalation processes on the nanometer scale. We used atomic force microscopy (AFM), combined with cyclic voltammetry, as in-situ tool of analysis during intercalation and expulsion of perchloric anions into the HOPG electrodes. According to the AFM measurements, the HOPG interlayer spacing increases by 32% when perchloric anions intercalate, in agreement with the formation of stage IV of graphite intercalation compounds. (author) 3 figs., 3 refs.

  18. Inhomogeneous ozone doping and heat induced defects in graphene studied by infrared near-field microscopy

    Science.gov (United States)

    Wang, Wenjie; Zhang, Jiawei; Deng, Haiming; Liu, Megnkun; Xu, Du

    With the potential use of surface plasmon such as transfer data many orders faster than traditional wires, it has been very popular in research. The fact is that the wavelength of of plasmon is much shorter than the one of free space radiation. The UV ozone doping level can be fine controlled in room temperature creating selected plasmon circuit. We study inhomogeneous graphene plasmonics in ozone doped graphene using scattering-type scanning near-field infrared microscopy and spectroscopy. The single layer and bilayer graphene are doped with different dosage of ozone under UV exposure, which lead to surface inhomogeneity and inhomogeneous graphene plasmon polarition excitation under tip. After annealing the ozone doped graphene in air, the inhomogeneous doping induced plasmons disappear, together with the occurrence of local defects after high temperature annealing.

  19. Evaluating the NOx Storage Catalysts (NSC Aging: A Preliminary Analytical Study with Electronic Microscopy

    Directory of Open Access Journals (Sweden)

    Leonarda Bellebuono

    2017-10-01

    Full Text Available This paper describes an expeditious and reliable method for determining the thermal effects in a static condition of commercial NOx storage catalysts (NSCs using scanning electron microscopy with an energy dispersive X-ray analytical system (SEM/EDS. It is worth remarking that possible changes in the morphology and in the elemental composition of the catalyst may be considered as the most important causes of the lower conversion of NOx. The information attained in this work indicates that Pt nanoparticle sintering is strongly increased by the oxygen exposure, and this can be considered a very useful preliminary investigation for the studies already present in the literature on the efficiency of NSCs.

  20. Scanning tunneling microscopy studies of organic monolayers adsorbed on the rhodium(111) crystal surface

    Energy Technology Data Exchange (ETDEWEB)

    Cernota, Paul Davis [Univ. of California, Berkeley, CA (United States)

    1999-08-01

    Scanning Tunneling Microscopy studies were carried out on ordered overlayers on the (111) surface of rhodium. These adsorbates include carbon monoxide (CO), cyclohexane, cyclohexene, 1,4-cyclohexadiene, para-xylene, and meta-xylene. Coadsorbate systems included: CO with ethylidyne, CO with para- and meta-xylene, and para-xylene with meta-xylene. In the case of CO, the structure of the low coverage (2x2) overlayer has been observed. The symmetry of the unit cell in this layer suggests that the CO is adsorbed in the 3-fold hollow sites. There were also two higher coverage surface structures with (√7x√7) unit cells. One of these is composed of trimers of CO and has three CO molecules in each unit cell. The other structure has an additional CO molecule, making a total of four. This extra CO sits on a top site.