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

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.

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

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)

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

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

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.

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.)

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

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"

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.

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).

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.

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.

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....

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...

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....

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.

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

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)

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.

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.

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.

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.

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...

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...

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),...

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

'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

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

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

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

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

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.

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....

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.

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.

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)

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

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...

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.)

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)

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

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.

Challenges in quantitative crystallographic characterization of 3D thin films by ACOM-TEM.

Science.gov (United States)

Kobler, A; Kübel, C

2017-02-01

Automated crystal orientation mapping for transmission electron microscopy (ACOM-TEM) has become an easy to use method for the investigation of crystalline materials and complements other TEM methods by adding local crystallographic information over large areas. It fills the gap between high resolution electron microscopy and electron back scatter diffraction in terms of spatial resolution. Recent investigations showed that spot diffraction ACOM-TEM is a quantitative method with respect to sample parameters like grain size, twin density, orientation density and others. It can even be used in combination with in-situ tensile or thermal testing. However, there are limitations of the current method. In this paper we discuss some of the challenges and discuss solutions, e.g. we present an ambiguity filter that reduces the number of pixels with a '180° ambiguity problem'. For that an ACOM-TEM tilt series of nanocrystalline Pd thin films with overlapping crystallites was acquired and analyzed. Copyright © 2017. Published by Elsevier B.V.

cisTEM, user-friendly software for single-particle image processing

Science.gov (United States)

2018-01-01

We have developed new open-source software called cisTEM (computational imaging system for transmission electron microscopy) for the processing of data for high-resolution electron cryo-microscopy and single-particle averaging. cisTEM features a graphical user interface that is used to submit jobs, monitor their progress, and display results. It implements a full processing pipeline including movie processing, image defocus determination, automatic particle picking, 2D classification, ab-initio 3D map generation from random parameters, 3D classification, and high-resolution refinement and reconstruction. Some of these steps implement newly-developed algorithms; others were adapted from previously published algorithms. The software is optimized to enable processing of typical datasets (2000 micrographs, 200 k – 300 k particles) on a high-end, CPU-based workstation in half a day or less, comparable to GPU-accelerated processing. Jobs can also be scheduled on large computer clusters using flexible run profiles that can be adapted for most computing environments. cisTEM is available for download from cistem.org. PMID:29513216

cisTEM, user-friendly software for single-particle image processing.

Science.gov (United States)

Grant, Timothy; Rohou, Alexis; Grigorieff, Nikolaus

2018-03-07

We have developed new open-source software called cis TEM (computational imaging system for transmission electron microscopy) for the processing of data for high-resolution electron cryo-microscopy and single-particle averaging. cis TEM features a graphical user interface that is used to submit jobs, monitor their progress, and display results. It implements a full processing pipeline including movie processing, image defocus determination, automatic particle picking, 2D classification, ab-initio 3D map generation from random parameters, 3D classification, and high-resolution refinement and reconstruction. Some of these steps implement newly-developed algorithms; others were adapted from previously published algorithms. The software is optimized to enable processing of typical datasets (2000 micrographs, 200 k - 300 k particles) on a high-end, CPU-based workstation in half a day or less, comparable to GPU-accelerated processing. Jobs can also be scheduled on large computer clusters using flexible run profiles that can be adapted for most computing environments. cis TEM is available for download from cistem.org. © 2018, Grant et al.

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.

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)

Challenges in quantitative crystallographic characterization of 3D thin films by ACOM-TEM

Energy Technology Data Exchange (ETDEWEB)

Kobler, A. [Institute of Nanotechnology (INT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344, Eggenstein-Leopoldshafen (Germany); Karlsruhe Nano Micro Facility (KNMF), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344, Eggenstein-Leopoldshafen (Germany); Kübel, C., E-mail: christian.kuebel@kit.edu [Institute of Nanotechnology (INT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344, Eggenstein-Leopoldshafen (Germany); Karlsruhe Nano Micro Facility (KNMF), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344, Eggenstein-Leopoldshafen (Germany)

2017-02-15

Automated crystal orientation mapping for transmission electron microscopy (ACOM-TEM) has become an easy to use method for the investigation of crystalline materials and complements other TEM methods by adding local crystallographic information over large areas. It fills the gap between high resolution electron microscopy and electron back scatter diffraction in terms of spatial resolution. Recent investigations showed that spot diffraction ACOM-TEM is a quantitative method with respect to sample parameters like grain size, twin density, orientation density and others. It can even be used in combination with in-situ tensile or thermal testing. However, there are limitations of the current method. In this paper we discuss some of the challenges and discuss solutions, e.g. we present an ambiguity filter that reduces the number of pixels with a ‘180° ambiguity problem’. For that an ACOM-TEM tilt series of nanocrystalline Pd thin films with overlapping crystallites was acquired and analyzed. - Highlights: • Tilt series of nanocrystalline Pd thin films. • Quantitative ACOM-TEM data processing, including a rotation map of crystallites. • Noise filter for orientation data: Ambiguity Filter and min. distance filter.

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....

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)

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.

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

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

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.

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

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...

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.

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.

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.

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.

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...

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...

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.

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

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.

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

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.

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

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.)

Correlative microscopy of a carbide-free bainitic steel.

Science.gov (United States)

Hofer, Christina; Bliznuk, Vitaliy; Verdiere, An; Petrov, Roumen; Winkelhofer, Florian; Clemens, Helmut; Primig, Sophie

2016-02-01

In this work a carbide-free bainitic steel was examined by a novel correlative microscopy approach using transmission Kikuchi diffraction (TKD) and transmission electron microscopy (TEM). The individual microstructural constituents could be identified by TKD based on their different crystal structure for bainitic ferrite and retained austenite and by image quality for the martensite-austenite (M-A) constituent. Subsequently, the same area was investigated in the TEM and a good match of these two techniques regarding the identification of the area position and crystal orientation could be proven. Additionally, the M-A constituent was examined in the TEM for the first time after preceded unambiguous identification using a correlative microscopy approach. The selected area diffraction pattern showed satellites around the main reflexes which might indicate a structural modulation. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

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.

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.

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.

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.

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.

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...

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

Investigation of the structure of nanocrystalline refractory oxides by X-ray diffraction, electron microscopy, and atomic force microscopy

International Nuclear Information System (INIS)

Ulyanova, T. M.; Titova, L. V.; Medichenko, S. V.; Zonov, Yu. G.; Konstantinova, T. E.; Glazunova, V. A.; Doroshkevich, A. S.; Kuznetsova, T. A.

2006-01-01

The structures of nanocrystalline fibrous powders of refractory oxides have been investigated by different methods: determination of coherent-scattering regions, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and atomic-force microscopy (AFM). The sizes of nanograins of different crystalline phases of refractory metal oxides have been determined during the formation of these nanograins and the dynamics of their growth during heat treatment in the temperature range 600-1600 deg. C has been studied. The data on the structure of nanocrystalline refractory oxide powders, obtained by different methods, are in good agreement. According to the data on coherent-scattering regions, the sizes of the ZrO 2 (Y 2 O 3 ) and Al 2 O 3 grains formed are in the range 4-6 nm, and the particle sizes determined according to the TEM and AFM data are in the ranges 5-7 and 2-10 nm, respectively. SEM analysis made it possible to investigate the dynamics of nanoparticle growth at temperatures above 1000 deg. C and establish the limiting temperatures of their consolidation in fibers

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.

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.

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.

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.

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.

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.

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...

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.

Transmission electron microscopy of InP-based compound semiconductor materials and devices

International Nuclear Information System (INIS)

Chu, S.N.G.

1990-01-01

InP/InGaAsP-based heteroepitaxial structures constitute the major optoelectronic devices for state-of-the-art long wavelength optical fiber communication system.s Future advanced device structures will require thin heteroepitaxial quantum wells and superlattices a few tens of angstrom or less in thickness, and lateral dimensions ranging from a few tens angstrom for quantum dots and wires to a few μm in width for buried heterostructure lasers. Due to the increasing complexity of the device structure required by band-gap engineering, the performance of these devices becomes susceptible to any lattice imperfections present in the structure. Transmission electron microscopy (TEM), therefore, becomes the most important technique in characterizing the structural integrity of these materials. Cross-section transmission electron microscopy (XTEM) not only provides the necessary geometric information on the device structure; a careful study of the materials science behind the observed lattice imperfections provides directions for optimization of both the epitaxial growth parameters and device processing conditions. Furthermore, for device reliability studies, TEM is the only technique that unambiguously identifies the cause of device degradation. In this paper, the authors discuss areas of application of various TEM techniques, describe the TEM sample preparation technique, and review case studies to demonstrate the power of the TEM technique

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.

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

A new method to characterize dopant profiles in NMOSFETs using conventional transmission electron microscopy

International Nuclear Information System (INIS)

Kawamura, Kazuo; Ikeda, Kazuto; Terauchi, Masami

2004-01-01

We have developed a new method using conventional transmission electron microscopy (TEM) to obtain two dimensional dopant profiles in silicon and applied it to 40 nm-gate-length N + /p metal oxide semiconductor field effect transistors (MOSFETs). The results are consistent with those of selective-chemically etched samples observed by TEM. This method, using focused ion beam (FIB) sample preparation and conventional TEM, has the great advantage of simple sample preparation and high spatial resolution compared to other characterization methods, such as atomic capacitance microscopy, spreading resistance microscopy, and TEM combined with selective chemical etching. This indicates that this method can be applicable to the analysis of FETs at the 65 nm or smaller node

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...

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.

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.

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.

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.

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.

High-resolution electron microscopy

CERN Document Server

Spence, John C H

2013-01-01

This new fourth edition of the standard text on atomic-resolution transmission electron microscopy (TEM) retains previous material on the fundamentals of electron optics and aberration correction, linear imaging theory (including wave aberrations to fifth order) with partial coherence, and multiple-scattering theory. Also preserved are updated earlier sections on practical methods, with detailed step-by-step accounts of the procedures needed to obtain the highest quality images of atoms and molecules using a modern TEM or STEM electron microscope. Applications sections have been updated - these include the semiconductor industry, superconductor research, solid state chemistry and nanoscience, and metallurgy, mineralogy, condensed matter physics, materials science and material on cryo-electron microscopy for structural biology. New or expanded sections have been added on electron holography, aberration correction, field-emission guns, imaging filters, super-resolution methods, Ptychography, Ronchigrams, tomogr...

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)

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.

Optimized pre-thinning procedures of ion-beam thinning for TEM sample preparation by magnetorheological polishing.

Science.gov (United States)

Luo, Hu; Yin, Shaohui; Zhang, Guanhua; Liu, Chunhui; Tang, Qingchun; Guo, Meijian

2017-10-01

Ion-beam-thinning is a well-established sample preparation technique for transmission electron microscopy (TEM), but tedious procedures and labor consuming pre-thinning could seriously reduce its efficiency. In this work, we present a simple pre-thinning technique by using magnetorheological (MR) polishing to replace manual lapping and dimpling, and demonstrate the successful preparation of electron-transparent single crystal silicon samples after MR polishing and single-sided ion milling. Dimples pre-thinned to less than 30 microns and with little mechanical surface damage were repeatedly produced under optimized MR polishing conditions. Samples pre-thinned by both MR polishing and traditional technique were ion-beam thinned from the rear side until perforation, and then observed by optical microscopy and TEM. The results show that the specimen pre-thinned by MR technique was free from dimpling related defects, which were still residual in sample pre-thinned by conventional technique. Nice high-resolution TEM images could be acquired after MR polishing and one side ion-thinning. MR polishing promises to be an adaptable and efficient method for pre-thinning in preparation of TEM specimens, especially for brittle ceramics. Copyright © 2017 Elsevier B.V. All rights reserved.

Transmission electron microscopy in micro-nanoelectronics

CERN Document Server

Claverie, Alain

2013-01-01

Today, the availability of bright and highly coherent electron sources and sensitive detectors has radically changed the type and quality of the information which can be obtained by transmission electron microscopy (TEM). TEMs are now present in large numbers not only in academia, but also in industrial research centers and fabs.This book presents in a simple and practical way the new quantitative techniques based on TEM which have recently been invented or developed to address most of the main challenging issues scientists and process engineers have to face to develop or optimize sem

Characterization of multilayer nitride coatings by electron microscopy and modulus mapping

International Nuclear Information System (INIS)

Pemmasani, Sai Pramod; Rajulapati, Koteswararao V.; Ramakrishna, M.; Valleti, Krishna; Gundakaram, Ravi C.; Joshi, Shrikant V.

2013-01-01

This paper discusses multi-scale characterization of physical vapour deposited multilayer nitride coatings using a combination of electron microscopy and modulus mapping. Multilayer coatings with a triple layer structure based on TiAlN and nanocomposite nitrides with a nano-multilayered architecture were deposited by Cathodic arc deposition and detailed microstructural studies were carried out employing Energy Dispersive Spectroscopy, Electron Backscattered Diffraction, Focused Ion Beam and Cross sectional Transmission Electron Microscopy in order to identify the different phases and to study microstructural features of the various layers formed as a result of the deposition process. Modulus mapping was also performed to study the effect of varying composition on the moduli of the nano-multilayers within the triple layer coating by using a Scanning Probe Microscopy based technique. To the best of our knowledge, this is the first attempt on modulus mapping of cathodic arc deposited nitride multilayer coatings. This work demonstrates the application of Scanning Probe Microscopy based modulus mapping and electron microscopy for the study of coating properties and their relation to composition and microstructure. - Highlights: • Microstructure of a triple layer nitride coating studied at multiple length scales. • Phases identified by EDS, EBSD and SAED (TEM). • Nanolayered, nanocomposite structure of the coating studied using FIB and TEM. • Modulus mapping identified moduli variation even in a nani-multilayer architecture

Determination of Size Distributions in Nanocrystalline Powders by TEM, XRD and SAXS

DEFF Research Database (Denmark)

Jensen, Henrik; Pedersen, Jørgen Houe; Jørgensen, Jens Erik

2006-01-01

Crystallite size distributions and particle size distributions were determined by TEM, XRD, and SAXS for three commercially available TiO2 samples and one homemade. The theoretical Guinier Model was fitted to the experimental data and compared to analytical expressions. Modeling of the XRD spectra...... the size distribution obtained from the XRD experiments; however, a good agreement was obtained between the two techniques. Electron microscopy, SEM and TEM, confirmed the primary particle sizes, the size distributions, and the shapes obtained by XRD and SAXS. The SSEC78 powder and the commercially...

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

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.

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)

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.

An electron microscopy appraisal of tensile fracture in metallic glasses

International Nuclear Information System (INIS)

Matthews, D.T.A.; Ocelik, V.; Bronsveld, P.M.; De Hosson, J.Th.M.

2008-01-01

Three glass-forming alloy compositions were chosen for ribbon production and subsequent electron microscopy studies. In situ tensile testing with transmission electron microscopy (TEM), followed by ex situ TEM and ex situ scanning electron microscopy (SEM), allowed the deformation processes in tensile fracture of metallic glasses to be analysed. In situ shear band propagation was found to be jump-like, with the jump sites correlating with the formation of secondary shear bands. The effect of structural relaxation by in situ heating is also discussed. Nanocrystallization near the fracture surface was observed; however, no crystallization was also reported in the same sample and the reasons for this are discussed. Both the TEM and the SEM observations confirmed the presence of a liquid-like layer on or near the fracture surface of the ribbons. The formation of a liquid-like layer was characterized by the vein geometries and vein densities on the fracture surfaces and its dependence on shear displacement, δ, is discussed. A simple model is adapted to relate the temperature rise during shear banding to the glass transition and melting temperatures and this is used to explain the variety of fracture surfaces which are developed for macroscopically identical tensile testing of metallic glasses together with features which exhibit local melting

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.

Aberration-corrected STEM/TEM imaging at 15 kV

International Nuclear Information System (INIS)

Sasaki, Takeo; Sawada, Hidetaka; Hosokawa, Fumio; Sato, Yuta; Suenaga, Kazu

2014-01-01

The performance of aberration-corrected (scanning) transmission electron microscopy (S/TEM) at an accelerating voltage of 15 kV was evaluated in a low-voltage microscope equipped with a cold-field emission gun and a higher-order aberration corrector. Aberrations up to the fifth order were corrected by the aberration measurement and auto-correction system using the diffractogram tableau method in TEM and Ronchigram analysis in STEM. TEM observation of nanometer-sized particles demonstrated that aberrations up to an angle of 50 mrad were compensated. A TEM image of Si[110] exhibited lattice fringes with a spacing of 0.192 nm, and the power spectrum of the image showed spots corresponding to distances of 0.111 nm. An annular dark-field STEM image of Si[110] showed lattice fringes of (111) and (22¯0) planes corresponding to lattice distances of 0.314 nm and 0.192 nm, respectively. At an accelerating voltage of 15 kV, the developed low-voltage microscope achieved atomic-resolution imaging with a small chromatic aberration and a large uniform phase. - Highlights: • Aberration-corrected STEM/TEM imaging at 15 kV demonstrated lattice fringes of Si[110] single crystal with a spacing of 0.192 nm. • To achieve this performance at a lower accelerating voltage, uniform phase area over 50 mrad is mandatory in Ronchigram and Diffractogram tableau. • This means a higher-order aberration of six-fold astigmatism should be compensated. • In addition, decreasing the effect of chromatic aberration plays an important role for improving the performance of linear scattering component at 15 kV TEM

Processing scarce biological samples for light and transmission electron microscopy

Directory of Open Access Journals (Sweden)

P Taupin

2008-06-01

Full Text Available Light microscopy (LM and transmission electron microscopy (TEM aim at understanding the relationship structure-function. With advances in biology, isolation and purification of scarce populations of cells or subcellular structures may not lead to enough biological material, for processing for LM and TEM. A protocol for preparation of scarce biological samples is presented. It is based on pre-embedding the biological samples, suspensions or pellets, in bovine serum albumin (BSA and bis-acrylamide (BA, cross-linked and polymerized. This preparation provides a simple and reproducible technique to process biological materials, present in limited quantities that can not be amplified, for light and transmission electron microscopy.

Cross section TEM characterization of high-energy-Xe-irradiated U-Mo

Energy Technology Data Exchange (ETDEWEB)

Ye, B., E-mail: bye@anl.gov [Nuclear Engineering Division, Argonne National Laboratory, 9700 S. Cass Ave. Lemont, IL 60439 (United States); Jamison, L.; Miao, Y. [Nuclear Engineering Division, Argonne National Laboratory, 9700 S. Cass Ave. Lemont, IL 60439 (United States); Bhattacharya, S. [Department of Materials Science and Engineering, Northwestern University, 2220 Campus Dr. Evanston, IL 60208 (United States); Hofman, G.L.; Yacout, A.M. [Nuclear Engineering Division, Argonne National Laboratory, 9700 S. Cass Ave. Lemont, IL 60439 (United States)

2017-05-15

U-Mo alloys irradiated with 84 MeV Xe ions to various doses were characterized with transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) techniques. The TEM thin foils were prepared perpendicular to the irradiated surface to allow a direct observation of the entire region modified by ions. Therefore, depth-selective microstructural information was revealed. Varied irradiation-induced phenomena such as gas bubble formation, phase reversal, and recrystallization were observed at different ion penetration depths in U-Mo. - Highlights: •Three distinct zones were observed along the ion traveling direction in U-7Mo irradiated with 84 MeV Xe ions at 350 °C. •The α-U particles within the Xe-implanted region were reverted to γ-U phase by irradiation. •High-density random intra-granular bubbles in a size of 4–5 nm were found in the irradiated region, coexisting with large inter-granular bubbles. •The high lattice stresses built up during the irradiation-induced phase reversal is probably the driving force for the small grain formation at cell boundaries.

TEM characterization of UO2-Gd2O3 nuclear fuels synthesized by coprecipitation method

International Nuclear Information System (INIS)

Soldati, A.; Gana Watkins, I.; Menghini, J.; Prado, M.

2013-01-01

We present a micro and nano structural characterization of 4% weight doped Gd 2 O 3 -UO 2 pellet using Transmission Electron Microscopy (TEM). Agglomerate morphology and crystallite sizes were determined using light/dark field and high resolution (HR-TEM) images. Convergent beam Energy Dispersive Spectroscopy (EDS) and Electron Diffraction (ED) were used to evaluate sample composition and homogeneity, even at the nanometer scale. We obtained an average crystallite size of 90±20 nm. Moreover, from TEM-EDS analyses we determined the presence of Gadolinium in all the analyzed crystallites but with 25% variation among their concentrations. These results show the capability of TEM analysis to characterize a nuclear fuel pellet with burnable poisons nano structure and homogeneity.(author)

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.

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]...

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

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...

Inducing fluorescence of uranyl acetate as a dual-purpose contrast agent for correlative light-electron microscopy with nanometre precision.

Science.gov (United States)

Tuijtel, Maarten W; Mulder, Aat A; Posthuma, Clara C; van der Hoeven, Barbara; Koster, Abraham J; Bárcena, Montserrat; Faas, Frank G A; Sharp, Thomas H

2017-09-05

Correlative light-electron microscopy (CLEM) combines the high spatial resolution of transmission electron microscopy (TEM) with the capability of fluorescence light microscopy (FLM) to locate rare or transient cellular events within a large field of view. CLEM is therefore a powerful technique to study cellular processes. Aligning images derived from both imaging modalities is a prerequisite to correlate the two microscopy data sets, and poor alignment can limit interpretability of the data. Here, we describe how uranyl acetate, a commonly-used contrast agent for TEM, can be induced to fluoresce brightly at cryogenic temperatures (-195 °C) and imaged by cryoFLM using standard filter sets. This dual-purpose contrast agent can be used as a general tool for CLEM, whereby the equivalent staining allows direct correlation between fluorescence and TEM images. We demonstrate the potential of this approach by performing multi-colour CLEM of cells containing equine arteritis virus proteins tagged with either green- or red-fluorescent protein, and achieve high-precision localization of virus-induced intracellular membrane modifications. Using uranyl acetate as a dual-purpose contrast agent, we achieve an image alignment precision of ~30 nm, twice as accurate as when using fiducial beads, which will be essential for combining TEM with the evolving field of super-resolution light microscopy.

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

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.

Comprehensive analysis of TEM methods for LiFePO₄/FePO₄ phase mapping: spectroscopic techniques (EFTEM, STEM-EELS) and STEM diffraction techniques (ACOM-TEM)

DEFF Research Database (Denmark)

Mu, X.; Kobler, A.; Wang, D.

2016-01-01

Transmission electron microscopy (TEM) has been used intensively in investigating battery materials, e.g. to obtain phase maps of partially (dis)charged (lithium) iron phosphate (LFP/FP), which is one of the most promising cathode material for next generation lithium ion (Li-ion) batteries. Due t...

Advanced electron microscopy characterization of nanomaterials for catalysis

Directory of Open Access Journals (Sweden)

Dong Su

2017-04-01

Full Text Available Transmission electron microscopy (TEM has become one of the most powerful techniques in the fields of material science, inorganic chemistry and nanotechnology. In terms of resolutions, advanced TEM may reach a high spatial resolution of 0.05 nm, a high energy-resolution of 7 meV. In addition, in situ TEM can help researchers to image the process happened within 1 ms. This paper reviews the recent technical progresses of applying advanced TEM characterization on nanomaterials for catalysis. The text is organized based on the perspective of application: for example, size, composition, phase, strain, and morphology. The electron beam induced effect and in situ TEM are also introduced. I hope this review can help the scientists in related fields to take advantage of advanced TEM to their own researches. Keywords: Advanced TEM, Nanomaterials, Catalysts, In situ

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

Transmission electron microscopy, fluorescence microscopy, and confocal raman microscopic analysis of ultrastructural and compositional heterogeneity of Cornus alba L. wood cell wall.

Science.gov (United States)

Ma, Jianfeng; Ji, Zhe; Zhou, Xia; Zhang, Zhiheng; Xu, Feng

2013-02-01

Transmission electron microscopy (TEM), fluorescence microscopy, and confocal Raman microscopy can be used to characterize ultrastructural and compositional heterogeneity of plant cell walls. In this study, TEM observations revealed the ultrastructural characterization of Cornus alba L. fiber, vessel, axial parenchyma, ray parenchyma, and pit membrane between cells, notably with the ray parenchyma consisting of two well-defined layers. Fluorescence microscopy evidenced that cell corner middle lamella was more lignified than adjacent compound middle lamella and secondary wall with variation in lignification level from cell to cell. In situ Raman images showed that the inhomogeneity in cell wall components (cellulose and lignin) among different cells and within morphologically distinct cell wall layers. As the significant precursors of lignin biosynthesis, the pattern of coniferyl alcohol and aldehyde (joint abbreviation Lignin-CAA for both structures) distribution in fiber cell wall was also identified by Raman images, with higher concentration occurring in the fiber secondary wall where there was the highest cellulose concentration. Moreover, noteworthy was the observation that higher concentration of lignin and very minor amounts of cellulose were visualized in the pit membrane areas. These complementary microanalytical methods provide more accurate and complete information with regard to ultrastructural and compositional characterization of plant cell walls.

Visualization of arrangements of carbon atoms in graphene layers by Raman mapping and atomic-resolution TEM

KAUST Repository

Cong, Chunxiao

2013-02-01

In-plane and out-of-plane arrangements of carbon atoms in graphene layers play critical roles in the fundamental physics and practical applications of these novel two-dimensional materials. Here, we report initial results on the edge/crystal orientations and stacking orders of bi-and tri-layer graphene (BLG and TLG) from Raman spectroscopy and transmission electron microscopy (TEM) experiments performed on the same sample. We introduce a new method of transferring graphene flakes onto a normal TEM grid. Using this novel method, we probed the BLG and TLG flakes that had been previously investigated by Raman scattering with high-resolution (atomic) TEM.

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.

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

Characterization of crystallite morphology for doped strontium fluoride nanophosphors by TEM and XRD

Energy Technology Data Exchange (ETDEWEB)

O' Connell, J.H. [Centre for HRTEM, Nelson Mandela Metropolitan University, PO Box 77000, Port Elizabeth ZA6031 (South Africa); Lee, M.E., E-mail: Michael.lee@nmmu.ac.za [Centre for HRTEM, Nelson Mandela Metropolitan University, PO Box 77000, Port Elizabeth ZA6031 (South Africa); Yagoub, M.Y.A.; Swart, H.C.; Coetsee, E. [Department of Physics, University of the Free State, PO Box 339, Bloemfontein ZA9300 (South Africa)

2016-01-01

Crystallite morphology for Eu-doped and undoped SrF{sub 2} nanophosphors have been determined by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The values for average crystallite size obtained by the application of the Scherrer equation and the full width at half maximum (FWHM) values for XRD peaks are compared to the results obtained using the hollow cone dark field (HCDF) TEM imaging technique. In the case of the TEM analysis, a bimodal crystallite size distribution was revealed with one of the distributions having a measured range of crystallite sizes which was in good agreement with the XRD data. HCDF in combination with FIB specimen preparation was found to be a promising technique for the determination of crystallite size distributions in nanophosphors which might facilitate a better understanding of their scintillation properties.

Characterization of crystallite morphology for doped strontium fluoride nanophosphors by TEM and XRD

International Nuclear Information System (INIS)

O'Connell, J.H.; Lee, M.E.; Yagoub, M.Y.A.; Swart, H.C.; Coetsee, E.

2016-01-01

Crystallite morphology for Eu-doped and undoped SrF_2 nanophosphors have been determined by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The values for average crystallite size obtained by the application of the Scherrer equation and the full width at half maximum (FWHM) values for XRD peaks are compared to the results obtained using the hollow cone dark field (HCDF) TEM imaging technique. In the case of the TEM analysis, a bimodal crystallite size distribution was revealed with one of the distributions having a measured range of crystallite sizes which was in good agreement with the XRD data. HCDF in combination with FIB specimen preparation was found to be a promising technique for the determination of crystallite size distributions in nanophosphors which might facilitate a better understanding of their scintillation properties.

Quantitative TEM analysis of Al/Cu multilayer systems prepared by pulsed laser deposition

DEFF Research Database (Denmark)

Liu, Haihua; Pryds, Nini; Schou, Jørgen

2010-01-01

Thin films composed of alternating Al/Cu/Al layers were deposited on a (111) Si substrate using pulsed laser deposition (PLD). The thicknesses of the film and the individual layers, and the detailed internal structure within the layers were characterized by means of transmission electron microscopy...... for the formation of the first layer of nano-sized Al grains. The results demonstrate that the PLD technique is a powerful tool to produce nano-scale multilayered metal films with controllable thickness and grain sizes....... (TEM), high-resolution TEM (HRTEM), and energy-filtered TEM (EFTEM). Each Al or Cu layer consists of a single layer of nano-sized grains of different orientations. EFTEM results revealed a layer of oxide about 2 nm thick on the surface of the Si substrate, which is considered to be the reason...

A rapid method of reprocessing for electronic microscopy of cut histological in paraffin

International Nuclear Information System (INIS)

Hernandez Chavarri, F.; Vargas Montero, M.; Rivera, P.; Carranza, A.

2000-01-01

A simple and rapid method is described for re-processing of light microscopy paraffin sections to observe they under transmission electron microscopy (TEM) and scanning electron microscopy (SEM) The paraffin-embedded tissue is sectioned and deparaffinized in toluene; then exposed to osmium vapor under microwave irradiation using a domestic microwave oven. The tissues were embedded in epoxy resin, polymerized and ultrathin sectioned. The method requires a relatively short time (about 30 minutes for TEM and 15 for SEM), and produces a reasonable quality of the ultrastructure for diagnostic purposes. (Author) [es

New constraints on deformation processes in serpentinite from sub-micron Raman Spectroscopy and TEM

Science.gov (United States)

Smith, S. A. F.; Tarling, M.; Rooney, J. S.; Gordon, K. C.; Viti, C.

2017-12-01

Extensive work has been performed to characterize the mineralogical and mechanical properties of the various serpentine minerals (i.e. antigorite, lizardite, chrysotile, polyhedral and polygonal serpentine). However, correct identification of serpentine minerals is often difficult or impossible using conventional analytical techniques such as optical- and SEM-based microscopy, X-ray diffraction and infrared spectroscopy. Transmission Electron Microscopy (TEM) is the best analytical technique to identify the serpentine minerals, but TEM requires complex sample preparation and typically results in very small analysis areas. Sub-micron confocal Raman spectroscopy mapping of polished thin sections provides a quick and relatively inexpensive way of unambiguously distinguishing the main serpentine minerals within their in-situ microstructural context. The combination of high spatial resolution (with a diffraction-limited system, 366 nm), large-area coverage (up to hundreds of microns in each dimension) and ability to map directly on thin sections allows intricate fault rock textures to be imaged at a sample-scale, which can then form the target of more focused TEM work. The potential of sub-micron Raman Spectroscopy + TEM is illustrated by examining sub-micron-scale mineral intergrowths and deformation textures in scaly serpentinites (e.g. dissolution seams, mineral growth in pressure shadows), serpentinite crack-seal veins and polished fault slip surfaces from a serpentinite-bearing mélange in New Zealand. The microstructural information provided by these techniques has yielded new insights into coseismic dehydration and amorphization processes and the interplay between creep and localised rupture in serpentinite shear zones.

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...

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)

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.

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...

Transmission Electron Microscopy Specimen Preparation Method for Multiphase Porous Functional Ceramics

DEFF Research Database (Denmark)

Zhang, Wei; Kuhn, Luise Theil; Jørgensen, Peter Stanley

2013-01-01

An optimum method is proposed to prepare thin foil transmission electron microscopy (TEM) lamellae of multiphase porous functional ceramics: prefilling the pore space of these materials with an epoxy resin prior to focused ion beam milling. Several advantages of epoxy impregnation are demonstrated...... by successful preparation of TEM specimens that maintain the structural integrity of the entire lamella. Feasibility of the TEM alignment procedure is demonstrated, and ideal TEM analyses are illustrated on solid oxide fuel cell and solid oxide electrolysis cell materials. Some potential drawbacks of the TEM...

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.

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.

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.

Polymersomes, smaller than you think: ferrocene as a TEM probe to determine core structure

International Nuclear Information System (INIS)

Johnston, A. H.; Dalton, P. D.; Newman, T. A.

2010-01-01

By incorporating ferrocene into the hydrophobic membrane of PEG-b-PCL polymersome nanoparticles it is possible to selectively visualize their core using Transmission Electron Microscopy (TEM). Two different sizes of ferrocene-loaded polymersomes with mean hydrodynamic diameters of approximately 40 and 90 nm were prepared. Image analysis of TEM pictures of these polymersomes found that the mean diameter of the core was 4-5 times smaller than the mean hydrodynamic diameter. The values obtained also allow the surface diameter and internal volume of the core to be calculated.

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.

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.

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

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)

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

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...

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.

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.

Electron microscopy characterization of Ni-Cr-B-Si-C laser deposited coatings.

Science.gov (United States)

Hemmati, I; Rao, J C; Ocelík, V; De Hosson, J Th M

2013-02-01

During laser deposition of Ni-Cr-B-Si-C alloys with high amounts of Cr and B, various microstructures and phases can be generated from the same chemical composition that results in heterogeneous properties in the clad layer. In this study, the microstructure and phase constitution of a high-alloy Ni-Cr-B-Si-C coating deposited by laser cladding were analyzed by a combination of several microscopy characterization techniques including scanning electron microscopy in secondary and backscatter imaging modes, energy dispersive spectroscopy (EDS), electron backscatter diffraction (EBSD), and transmission electron microscopy (TEM). The combination of EDS and EBSD allowed unequivocal identification of micron-sized precipitates as polycrystalline orthorhombic CrB, single crystal tetragonal Cr5B3, and single crystal hexagonal Cr7C3. In addition, TEM characterization showed various equilibrium and metastable Ni-B, Ni-Si, and Ni-Si-B eutectic products in the alloy matrix. The findings of this study can be used to explain the phase formation reactions and to tune the microstructure of Ni-Cr-B-Si-C coatings to obtain the desired properties.

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....

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...

Towards in-situ tem analysis of PLD Pb(Zr,Ti)O3 thin film membranes

NARCIS (Netherlands)

Sardan Sukas, Ö.; Berenschot, Johan W.; de Boer, Meint J.; Nguyen, Duc Minh; van Zalk, M.; Abelmann, Leon

2011-01-01

In this paper, a novel technique for fabricating Transmission Electron Microscopy (TEM) chips for investigating structural and piezoelectric properties of Pulse Laser Deposited (PLD) Lead Zirconium Titanate (PZT) thin films is presented. The method involves silicon-on-insulator (SOI) wafer

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)

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

Determination of the activation energy in a cast aluminium alloy by TEM and DSC

International Nuclear Information System (INIS)

Ovono Ovono, D.; Guillot, I.; Massinon, D.

2007-01-01

The precipitation behaviour and microstructure development of the A319 alloy during ageing were investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM and STEM). During T5 treatment, θ' precipitates with an average size of about 18 nm were observed by TEM. The precipitate sizes increased with ageing temperature and attained an average size of 107 nm. In addition, there was a linear relationship between precipitate growth temperature and the cube of the precipitate size. This indicates that precipitate growth of the A319 alloy belongs to a thermal activated process of the Arrhenius type. The activation energy for the precipitate growth was calculated to be 140.4 ± 13.3 kJ/mol. However, under continuous heating conditions, the activation energy for the precipitate growth obtained by Kissinger plot was determined to be 119.5 ± 8.3 kJ/mol. Allowing for experimental error, both values are comparable and are related to the diffusion of Cu and/or Si in Al

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.

Transmission electron and optical microscopy of the domain structure of Ni3B7O13Br ferroic boracite

International Nuclear Information System (INIS)

Castellanos-Guzman, A.G.; Trujillo-Torrez, M.; Czank, M.

2005-01-01

The study investigated the domain structure of nickel bromine boracite single crystals, by means of polarised-light in conjunction with transmission electron microscopy. Single crystals of Ni 3 B 7 O 13 Br were grown by chemical transport reactions in closed quartz ampoules, in the temperature range of 1130 K and were examined by polarising optical microscopy (PLM), and transmission electron microscopy (TEM). PLM was also used in order to study the behaviour of birefringence as a function of temperature. For TEM the single crystals were crushed and mounted on holey carbon films. Comparative electron microscope images were useful for revealing the domain structure of this fully ferroelectric/fully ferroelastic material previously observed between the crossed polars of an optical microscope. X-ray diffraction analysis of the crystal under study was performed at room temperature

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

TEM EDS analysis of epitaxially-grown self-assembled indium islands

Directory of Open Access Journals (Sweden)

Jasmine Sears

2017-05-01

Full Text Available Epitaxially-grown self-assembled indium nanostructures, or islands, show promise as nanoantennas. The elemental composition and internal structure of indium islands grown on gallium arsenide are explored using Transmission Electron Microscopy (TEM Energy Dispersive Spectroscopy (EDS. Several sizes of islands are examined, with larger islands exhibiting high (>94% average indium purity and smaller islands containing inhomogeneous gallium and arsenic contamination. These results enable more accurate predictions of indium nanoantenna behavior as a function of growth parameters.

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.

Distortion of DNA Origami on Graphene Imaged with Advanced TEM Techniques.

Science.gov (United States)

Kabiri, Yoones; Ananth, Adithya N; van der Torre, Jaco; Katan, Allard; Hong, Jin-Yong; Malladi, Sairam; Kong, Jing; Zandbergen, Henny; Dekker, Cees

2017-08-01

While graphene may appear to be the ultimate support membrane for transmission electron microscopy (TEM) imaging of DNA nanostructures, very little is known if it poses an advantage over conventional carbon supports in terms of resolution and contrast. Microscopic investigations are carried out on DNA origami nanoplates that are supported onto freestanding graphene, using advanced TEM techniques, including a new dark-field technique that is recently developed in our lab. TEM images of stained and unstained DNA origami are presented with high contrast on both graphene and amorphous carbon membranes. On graphene, the images of the origami plates show severe unwanted distortions, where the rectangular shape of the nanoplates is significantly distorted. From a number of comparative control experiments, it is demonstrated that neither staining agents, nor screening ions, nor the level of electron-beam irradiation cause this distortion. Instead, it is suggested that origami nanoplates are distorted due to hydrophobic interaction of the DNA bases with graphene upon adsorption of the DNA origami nanoplates. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

In-situ Isotopic Analysis at Nanoscale using Parallel Ion Electron Spectrometry: A Powerful New Paradigm for Correlative Microscopy

Science.gov (United States)

Yedra, Lluís; Eswara, Santhana; Dowsett, David; Wirtz, Tom

2016-01-01

Isotopic analysis is of paramount importance across the entire gamut of scientific research. To advance the frontiers of knowledge, a technique for nanoscale isotopic analysis is indispensable. Secondary Ion Mass Spectrometry (SIMS) is a well-established technique for analyzing isotopes, but its spatial-resolution is fundamentally limited. Transmission Electron Microscopy (TEM) is a well-known method for high-resolution imaging down to the atomic scale. However, isotopic analysis in TEM is not possible. Here, we introduce a powerful new paradigm for in-situ correlative microscopy called the Parallel Ion Electron Spectrometry by synergizing SIMS with TEM. We demonstrate this technique by distinguishing lithium carbonate nanoparticles according to the isotopic label of lithium, viz. 6Li and 7Li and imaging them at high-resolution by TEM, adding a new dimension to correlative microscopy. PMID:27350565

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.

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

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.

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.

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.

The experimental electron mean-free-path in Si under typical (S)TEM conditions

International Nuclear Information System (INIS)

Potapov, P.L.

2014-01-01

The electron mean-free-path in Si was measured by EELS using the test structure with the certified dimensions as a calibration standard. In a good agreement with the previous CBED measurements, the mean-free-path is 150 nm for 200 keV and 179 nm for 300 keV energy of primary electrons at large collection angles. These values are accurately predicted by the model of Iakoubovskii et al. while the model of Malis et al. incorporated in common microscopy software underestimates the mean-free-path by 15% at least. Correspondingly, the thickness of TEM samples reported in many studies of the Si-based materials last decades might be noticeably underestimated. - Highlights: • The electron inelastic mean-free-path in Si is measured for the typical (S)TEM conditions. • These reference values allow for accurate determination of the lamella thickness by EELS. • The theoretical model by Malis et al. underestimates the mean-free-path values

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

Nonlinear entropy transfer in ETG-TEM turbulence via TEM driven zonal flows

International Nuclear Information System (INIS)

Asahi, Yuuichi; Tsutsui, Hiroaki; Tsuji-Iio, Shunji; Ishizawa, Akihiro; Sugama, Hideo; Watanabe, Tomohiko

2015-01-01

Nonlinear interplay of the electron temperature gradient (ETG) modes and the trapped electron modes (TEMs) was investigated by means of gyrokinetic simulation. Focusing on the situation where both TEMs and ETG modes are linearly unstable, the effects of TEM-driven zonal flows on ETG turbulence were examined by means of entropy transfer analysis. In a statistically steady turbulence where the TEM driven zonal flows are dominant, it turned out that the zonal flows meditate the entropy transfer of the ETG modes from the low to high radial wavenumber regions. The successive entropy transfer broadens the potential fluctuation spectrum in the radial wavenumber direction. In contrast, in the situation where ETG modes are unstable but TEMs are stable, the pure ETG turbulence does not produce strong zonal flows, leading to a rather narrow spectrum in the radial wavenumber space and a higher transport level. (author)

LORENTZ PHASE IMAGING AND IN-SITU LORENTZ MICROSCOPY OF PATTERNED CO-ARRAYS

International Nuclear Information System (INIS)

VOLKOV, V.V.; ZHU, Y.

2003-01-01

Understanding magnetic structures and properties of patterned and ordinary magnetic films at nanometer length-scale is the area of immense technological and fundamental scientific importance. The key feature to such success is the ability to achieve visual quantitative information on domain configurations with a maximum ''magnetic'' resolution. Several methods have been developed to meet these demands (Kerr and Faraday effects, differential phase contrast microscopy, magnetic force microscopy, SEMPA etc.). In particular, the modern off-axis electron holography allows retrieval of the electron-wave phase shifts down to 2π/N (with typical N = 10-20, approaching in the limit N ∼ 100) in TEM equipped with field emission gun, which is already successfully employed for studies of magnetic materials at nanometer scale. However, it remains technically demanding, sensitive to noise and needs highly coherent electron sources. As possible alternative we developed a new method of Lorentz phase microscopy [1,2] based on the Fourier solution [3] of magnetic transport-of-intensity (MTIE) equation. This approach has certain advantages, since it is less sensitive to noise and does not need high coherence of the source required by the holography. In addition, it can be realized in any TEM without basic hardware changes. Our approach considers the electron-wave refraction in magnetic materials (magnetic refraction) and became possible due to general progress in understanding of noninterferometric phase retrieval [4-6] dealing with optical refraction. This approach can also be treated as further development of Fresnel microscopy, used so far for imaging of in-situ magnetization process in magnetic materials studied by TEM. Figs. 1-3 show some examples of what kind information can be retrieved from the conventional Fresnel images using the new approach. Most of these results can be compared with electron-holographic data. Using this approach we can shed more light on fine details of

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.

Immunogold scanning electron microscopy can reveal the polysaccharide architecture of xylem cell walls

Science.gov (United States)

Sun, Yuliang; Juzenas, Kevin

2017-01-01

Abstract Immunofluorescence microscopy (IFM) and immunogold transmission electron microscopy (TEM) are the two main techniques commonly used to detect polysaccharides in plant cell walls. Both are important in localizing cell wall polysaccharides, but both have major limitations, such as low resolution in IFM and restricted sample size for immunogold TEM. In this study, we have developed a robust technique that combines immunocytochemistry with scanning electron microscopy (SEM) to study cell wall polysaccharide architecture in xylem cells at high resolution over large areas of sample. Using multiple cell wall monoclonal antibodies (mAbs), this immunogold SEM technique reliably localized groups of hemicellulosic and pectic polysaccharides in the cell walls of five different xylem structures (vessel elements, fibers, axial and ray parenchyma cells, and tyloses). This demonstrates its important advantages over the other two methods for studying cell wall polysaccharide composition and distribution in these structures. In addition, it can show the three-dimensional distribution of a polysaccharide group in the vessel lateral wall and the polysaccharide components in the cell wall of developing tyloses. This technique, therefore, should be valuable for understanding the cell wall polysaccharide composition, architecture and functions of diverse cell types. PMID:28398585

Exploration of shallow subsurface resistivity structure using a portable TEM system: TEM-FAST prosystem; Kan`igata TEM ho sochi TEM-FAST prosystem ni yoru senbu hiteiko chosa

Energy Technology Data Exchange (ETDEWEB)

Miura, Y; Kumekawa, Y; Takasugi, S [GERD Geothermal Energy Research and Development Co. Ltd., Tokyo (Japan)

1997-05-27

Discussions were given on effectiveness of the TEM-FAST ProSystem which is a portable TEM system developed recently for use in exploration of shallow subsurface resistivity. The system consists of a loop type antenna, the TEM-FAST as the main equipment, and a host computer, the host computer controlling the entire system. The system acquires transient response data in secondary induced magnetic fields lasting 4 {mu} sec to 1 m sec. The number of data is 5490 stacks in one measurement, and the data acquisition time is about three minutes. Measurements were carried out by using the TEM-FAST in the vicinity of a well, whose results were compared with those of electric logging, and discussions were given on them. Although the electric logging results had no data available for depths shallower than 35 m, the measurement results from the TEM-FAST were found highly harmonious with those of the electric logging. In addition, there were transmission and telephone lines in locations about 10 m away from the well during the measurement, but extremely high data quality was discovered. 6 refs., 7 figs., 1 tab.

TEM analysis of a friction stir-welded butt joint of Al-Si-Mg alloys

International Nuclear Information System (INIS)

Cabibbo, M.; Meccia, E.; Evangelista, E.

2003-01-01

The microstructure evolution of a joint of Al-Si-Mg alloys A6056-T4 and A6056-T6 has been characterized by transmission electron microscopy (TEM). Metallurgical investigations, hardness and mechanical tests were also performed to correlate the TEM investigations to the mechanical properties of the produced friction stir-welded butt joint. After friction stir-welding thermal treatment has been carried out at 530 deg. C followed by ageing at 160 deg. C (T6). The base material (T4) and the heat-treated one (T6) were put in comparison showing a remarkable ductility reduction of the joint after T6 treatment

In situ TEM observation of the growth and decomposition of monoclinic W18O49 nanowires

International Nuclear Information System (INIS)

Chen, C L; Mori, H

2009-01-01

The growth of monoclinic W 18 O 49 nanowires by heat treatment of a tungsten filament at ∼873 K and the decomposition of these nanowires under 200 keV electron irradiation at ∼1023 K have been investigated using in situ transmission electron microscopy (TEM). In situ TEM observation of the growth confirmed the vapor-solid growth mechanism of the monoclinic W 18 O 49 nanowires. In situ irradiation experiments revealed the formation of metallic bcc tungsten from monoclinic W 18 O 49 nanowires under 200 keV electron irradiation.

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.

TEM/SEM investigation of microstructural changes within the white etching area under rolling contact fatigue and 3-D crack reconstruction by focused ion beam

International Nuclear Information System (INIS)

Grabulov, A.; Ziese, U.; Zandbergen, H.W.

2007-01-01

The white etching area (WEA) surrounding the cracks formed under high-cycle rolling contact fatigue was investigated by transmission electron microscopy (TEM) and Dual Beam (scanning electron microscopy (SEM)/focused ion beam). SEM revealed the initiation of cracks formed around artificially introduced Al 2 O 3 inclusions in the model steel (composition similar to SAE 52100). TEM investigations showed a microstructural difference between the WEA (formation of nanocrystalline ferrite) and the steel matrix (tempered martensitic structure). A three-dimensional image of the crack reconstructed from ∼400 Dual Beam cross-section images is reported

Transmission Electron Microscopy for Wood and Fiber Analysis − A Review

Directory of Open Access Journals (Sweden)

Mehedi Reza

2015-07-01

Full Text Available This review describes use of transmission electron microscopy (TEM in wood and fiber analysis. Analytical techniques and sample preparation methods are used to localize substructures of the cell wall polymers and are discussed in this review. The ultrastructural features of the wood cell walls, the structures formed by microfibrils, and the distribution of cell wall polymers, as revealed by TEM, are covered. Research investigating the distribution of lignin in tension and compression woods using TEM is reviewed. Different kinds of wood biodegrading enzymes localized using TEM are mentioned. Additional features of TEM, i.e., 3D imaging, analytical TEM, and electron diffraction are discussed. Lastly, a comparison between TEM and other imaging techniques used for wood and fiber research are made. Thus, this review provides insight into the contribution of TEM in wood research since its invention and demonstrates how to use it more effectively in the future.

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.

Characterization of nanomaterials with transmission electron microscopy

KAUST Repository

Anjum, Dalaver H.

2016-08-01

The field of nanotechnology is about research and development on materials whose at least one dimension is in the range of 1 to 100 nanometers. In recent years, the research activity for developing nano-materials has grown exponentially owing to the fact that they offer better solutions to the challenges faced by various fields such as energy, food, and environment. In this paper, the importance of transmission electron microscopy (TEM) based techniques is demonstrated for investigating the properties of nano-materials. Specifically the nano-materials that are investigated in this report include gold nano-particles (Au-NPs), silver atom-clusters (Ag-ACs), tantalum single-atoms (Ta-SAs), carbon materials functionalized with iron cobalt (Fe-Co) NPs and titania (TiO2) NPs, and platinum loaded Ceria (Pt-CeO2) Nano composite. TEM techniques that are employed to investigate nano-materials include aberration corrected bright-field TEM (BF-TEM), high-angle dark-field scanning TEM (HAADF-STEM), electron energy-loss spectroscopy (EELS), and BF-TEM electron tomography (ET). With the help presented of results in this report, it is proved herein that as many TEM techniques as available in a given instrument are essential for a comprehensive nano-scale analysis of nanomaterials.

Characterization of defects and nanostructural alterations in the Nimonic 80A superalloy by using Transmission Electron Microscopy

International Nuclear Information System (INIS)

Guillen Giron, Teodolito; Leon Salazar, Jose Luis

2015-01-01

TEM (Transmission Electron Microscopy) probes are analyzed in aeronautical applications. Intercrystalline defects present in the Nimonic 80A superalloy are studied after being thermally treated and then subjecting the specimens to cyclic stresses. The TEM test specimens are pre-tested under high frequency (1 000 Hz and 20 000 Hz) fatigue at the University of Siegen in Germany simulating the working conditions of this alloy in aircraft turbines or other types of aeronautical applications. The mechanical stress has generated many deformations and nanometric defects in this material, evidenced in the dislocations. Defects are observed using very powerful microscopy techniques such as TEM. The results are obtained from the TEM analysis and have revealed characteristic precipitates in the Nimonic 80A sample when subjected to thermal treatments. The alloy has evidenced the formation of dislocations resulting from the mechanical stresses of the specimens. The influence of rainfall is evidenced in the mechanism of formation, grouping and movement of the dislocations in the microstructure of the samples used. (author) [es

TEM investigation of irradiation damage in single crystal CeO2

International Nuclear Information System (INIS)

Ye Bei; Kirk, Mark A.; Chen, Weiying; Oaks, Aaron; Rest, Jeffery; Yacout, Abdellatif; Stubbins, James F.

2011-01-01

In order to understand the evolution of radiation damage in oxide nuclear fuel, 150-1000 keV Kr ions were implanted into single crystal CeO 2 , as a simulation of fluorite ceramic UO 2 , while in situ transmission electron microscopy (TEM) observations were carried out. Two characteristic defect structures were investigated: dislocation/dislocation loops and nano-size gas bubbles. The growth behavior of defect clusters induced by 1 MeV Kr ions up to doses of 5 x 10 15 ions/cm 2 were followed at 600 deg. C and 800 deg. C. TEM micrographs clearly show the development of defect structures: nucleation of dislocation loops, transformation to extended dislocation lines, and the formation of tangled dislocation networks. The difference in dislocation growth rates at 600 deg. C and 800 deg. C revealed the important role which Ce-vacancies play in the loop formation process. Bubble formation, studied through 150 keV Kr implantations at room temperature and 600 deg. C, might be influenced by either the mobility of metal-vacancies correlated with at threshold temperature or the limitation of gas solubility as a function of temperature.

Transmission Electron Microscopy as Key Technique for the Characterization of Telocytes.

Science.gov (United States)

Cantarero, Irene; Luesma, Maria Jose; Alvarez-Dotu, Jose Miguel; Muñoz, Eduardo; Junquera, Concepcion

2016-01-01

It was 50 years ago when the details of cellular structure were first observed with an electron microscope (EM). Today, transmission electron microscopy (TEM) still provides the highest resolution detail of cellular ultrastructure. The existence of telocytes (TCs) has been described by Hinescu and Popescu in 2005 and up to now, many studies have been done in different tissues. EM has been fundamental in identification and recognition of TC and relationship between TC and stem cells (SCs) in recent years. We present a review on the importance of TEM to provide major advances in the knowledge of the biology of these cells.

A TEM quantitative evaluation of strengthening in an Mg-RE alloy reinforced with SiC

International Nuclear Information System (INIS)

Cabibbo, Marcello; Spigarelli, Stefano

2011-01-01

Magnesium alloys containing rare earth elements are known to have high specific strength, good creep and corrosion resistance up to 523 K. The addition of SiC ceramic particles strengthens the metal matrix composite resulting in better wear and creep resistance while maintaining good machinability. The role of the reinforcement particles in enhancing strength can be quantitatively evaluated using transmission electron microscopy (TEM). This paper presents a quantitative evaluation of the different strengthening contributions, determined through TEM inspections, in an SiC Mg-RE composite alloy containing yttrium, neodymium, gadolinium and dysprosium. Compression tests at temperatures ranging between 290 and 573 K were carried out. The microstructure strengthening mechanism was studied for all the compression conditions. Strengthening was compared to the mechanical results and the way the different contributions were combined is also discussed and justified. - Research Highlights: → TEM yield strengthening terms evaluation on a Mg-RE SiC alloy. → The evaluation has been extended to different compression temperature conditions. → Linear and Quadratic sum has been proposed and validated. → Hall-Petch was found to be the most prominent strengthening contributions.

Characterisation of archaeological glass mosaics by electron microscopy and X-ray microanalysis

International Nuclear Information System (INIS)

Roe, M; Plant, S; Henderson, J; Andreescu-Treadgold, I; Brown, P D

2006-01-01

The combined techniques of scanning electron microscopy, energy dispersive X-ray analysis, transmission electron microscopy (TEM) and selected area electron diffraction are used to characterise the microstructures of opaque coloured glass mosaics from a mediaeval church in Torcello, Italy. Comparison of MgO/K 2 O ratios allows distinction between mediaeval and modern glass artefacts to be made. TEM investigation of inclusions indicates that relict silica is responsible for the speckled appearance of an impure mediaeval glass artefact, whilst a fine scale dispersion of elemental Cu nanoparticles is considered responsible for the orange-red colouration of a modern glass artefact

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.

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.

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.

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)

PROPOSED ASTM METHOD FOR THE DETERMINATION OF ASBESTOS IN AIR BY TEM AND INFORMATION ON INTERFERING FIBERS

Science.gov (United States)

The draft of the ASTM Test Method for air entitled: "Airborne Asbestos Concentration in Ambient and Indoor Atmospheres as Determined by Transmission Electron Microscopy Direct Transfer (TEM)" (ASTM Z7077Z) is an adaptation of the International Standard, ISO 10312. It is currently...

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

Preparation of herpes simplex virus-infected primary neurons for transmission electron microscopy.

Science.gov (United States)

Miranda-Saksena, Monica; Boadle, Ross; Cunningham, Anthony L

2014-01-01

Transmission electron microscopy (TEM) provides the resolution necessary to identify both viruses and subcellular components of cells infected with many types of viruses, including herpes simplex virus. Recognized as a powerful tool in both diagnostic and research-based virology laboratories, TEM has made possible the identification of new viruses and has contributed to the elucidation of virus life cycle and virus-host cell interaction. Whilst there are many sample preparation techniques for TEM, conventional processing using chemical fixation and resin embedding remains a useful technique, available in virtually all EM laboratories, for studying virus/cell ultrastructure. In this chapter, we describe the preparation of herpes simplex virus-infected primary neurons, grown on plastic cover slips, to allow sectioning of neurons and axons in their growth plane. This technique allows TEM examination of cell bodies, axons, growth cones, and varicosities, providing powerful insights into virus-cell interaction.

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

Quantitative evaluation of temporal partial coherence using 3D Fourier transforms of through-focus TEM images

International Nuclear Information System (INIS)

Kimoto, Koji; Sawada, Hidetaka; Sasaki, Takeo; Sato, Yuta; Nagai, Takuro; Ohwada, Megumi; Suenaga, Kazu; Ishizuka, Kazuo

2013-01-01

We evaluate the temporal partial coherence of transmission electron microscopy (TEM) using the three-dimensional (3D) Fourier transform (FT) of through-focus images. Young's fringe method often indicates the unexpected high-frequency information due to non-linear imaging terms. We have already used the 3D FT of axial (non-tilted) through-focus images to reduce the effect of non-linear terms on the linear imaging term, and demonstrated the improvement of monochromated lower-voltage TEM performance [Kimoto et al., Ultramicroscopy 121 (2012) 31–39]. Here we apply the 3D FT method with intentionally tilted incidence to normalize various factors associated with a TEM specimen and an imaging device. The temporal partial coherence of two microscopes operated at 30, 60 and 80 kV is evaluated. Our method is applicable to such cases where the non-linear terms become more significant in lower acceleration voltage or aberration-corrected high spatial resolution TEM. - Highlights: • We assess the temporal partial coherence of TEM using a 3-dimensional (3D) Fourier transform (FT) of through-focus images. • We apply the 3D FT method with intentionally tilted incidence to normalize various factors associated with a TEM specimen and an imaging device. • The spatial frequency at which information transfer decreases to 1/e 2 (13.5%) is determined for two lower-voltage TEM systems

Contributions of electron microscopy to the understanding of reactions on compound semiconductor surfaces

International Nuclear Information System (INIS)

Sands, T.

1986-01-01

Reacted films on compound semiconductor substrates present challenging materials characterization problems which often require the application of transmission electron microscopy (TEM) techniques. In this paper, both the problem - solving potential of the TEM techniques and the limits imposed by preparation of thin film/compound semiconductor TEM specimens are discussed. Studies of the Ni/GaAs, CuCl/aq)/CdS and Pd/GaAs reactions exemplify the role of TEM in identifying and determining the spatial distribution of interface - stabilized polymorphs and new ternary phases (e.g. tetragonal Cu/sub 2/S, Ni/sub 3/GaAs and Pd/sub x/GaAs). These examples also serve to clarify the relationship between TEM and complementary analysis techniques such as Rutherford backscattering spectrometry, Auger electron spectroscopy and glancing-angle x-ray diffraction. In particular, it is argued that a combination of (1) high-spatial-resolution information obtained by TEM and (2) an indication of the ''average'' behavior provided by data from a complementary characterization technique provide the minimum quality and quantity of data necessary to understand most reactions on compound semiconductor substrates

Post Irradiation TEM Investigation of ZrN Coated U(Mo) Particles Prepared with FIB

Energy Technology Data Exchange (ETDEWEB)

Van Renterghem, W.; Leenaers, A.; Van den Berghe, S.; Miller, B. D.; Gan, J.; Madden, J. W.; Keiser, D. D.; Palancher, H.; Hofman, G. L.; Breitkreuz, H.

2015-10-01

In the framework of the Selenium project, two dispersion fuel plates were fabricated with Si and ZrN coated fuel particles and irradiated in the Br2 reactor of SCK•CEN to high burn-up. The first analysis of the irradiated plate proved the reduced swelling of the fuel plate and interaction layer growth up to 70% burn-up. The question was raised how the structure of the interaction layer had been affected by the irradiation and how the structure of the fuel particles had evolved. Hereto, samples from the ZrN coated UMo particles were prepared for transmission electron microscopy (TEM) using focused ion beam milling (FIB) at INL. The FIB technique allowed to precisely select the area of the interaction layer and/or fuel to produce a sample that is TEM transparent over an area of 20 by 20 µm. In this contribution, the first TEM results will be presented from the 66% burn-up sample.

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.

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)

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)

TEM characterization of plate-shaped L12-(Al,Ag)3Ti precipitates in a Ag-modified TiAl based intermetallics

International Nuclear Information System (INIS)

Yuan, Y.; Liu, H.W.; Zhao, X.N.; Meng, X.K.; Liu, Z.G.

2006-01-01

L1 2 -(Al,Ag) 3 Ti phase in a L1 0 -TiAl(Ag) intermetallic compound with a nominal composition of Ti-54 at.% Al-4 at.% Ag has been studied by transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray (EDX). TEM observations revealed that the alloy aged at 1273 K consists of L1 0 phase and L1 2 phase. The compositions of L1 2 phase and the matrix have been determined. The habit plane of L1 2 phase was analyzed by trace line method. It was revealed that the habit plane changed to one of {1 1 2) planes compared with our previous result. The semi-coherent interface was formed between L1 0 phase and L1 2 phase. HRTEM characterized the interface structure directly. The dislocation loops and ledges at the interphase boundary were observed. The results were discussed in terms of the competition between elastic strain and interfacial energy, ledge mechanism of phase transformation caused by long-range diffusion of the atoms

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.

In Situ Electron Microscopy of Lactomicroselenium Particles in Probiotic Bacteria

Directory of Open Access Journals (Sweden)

Gabor Nagy

2016-06-01

Full Text Available Electron microscopy was used to test whether or not (a in statu nascendi synthesized, and in situ measured, nanoparticle size does not differ significantly from the size of nanoparticles after their purification; and (b the generation of selenium is detrimental to the bacterial strains that produce them. Elemental nano-sized selenium produced by probiotic latic acid bacteria was used as a lactomicroselenium (lactomicroSel inhibitor of cell growth in the presence of lactomicroSel, and was followed by time-lapse microscopy. The size of lactomicroSel produced by probiotic bacteria was measured in situ and after isolation and purification. For these measurements the TESLA BS 540 transmission electron microscope was converted from analog (aTEM to digital processing (dTEM, and further to remote-access internet electron microscopy (iTEM. Lactobacillus acidophilus produced fewer, but larger, lactomicroSel nanoparticles (200–350 nm than Lactobacillus casei (L. casei, which generated many, smaller lactomicroSel particles (85–200 nm and grains as a cloudy, less electrodense material. Streptococcus thermophilus cells generated selenoparticles (60–280 nm in a suicidic manner. The size determined in situ in lactic acid bacteria was significantly lower than those measured by scanning electron microscopy after the isolation of lactomicroSel particles obtained from lactobacilli (100–500 nm, but higher relative to those isolated from Streptococcus thermopilus (50–100 nm. These differences indicate that smaller lactomicroSel particles could be more toxic to the producing bacteria themselves and discrepancies in size could have implications with respect to the applications of selenium nanoparticles as prebiotics.

Comprehensive analysis of TEM methods for LiFePO4/FePO4 phase mapping: spectroscopic techniques (EFTEM, STEM-EELS) and STEM diffraction techniques (ACOM-TEM).

Science.gov (United States)

Mu, X; Kobler, A; Wang, D; Chakravadhanula, V S K; Schlabach, S; Szabó, D V; Norby, P; Kübel, C

2016-11-01

Transmission electron microscopy (TEM) has been used intensively in investigating battery materials, e.g. to obtain phase maps of partially (dis)charged (lithium) iron phosphate (LFP/FP), which is one of the most promising cathode material for next generation lithium ion (Li-ion) batteries. Due to the weak interaction between Li atoms and fast electrons, mapping of the Li distribution is not straightforward. In this work, we revisited the issue of TEM measurements of Li distribution maps for LFP/FP. Different TEM techniques, including spectroscopic techniques (energy filtered (EF)TEM in the energy range from low-loss to core-loss) and a STEM diffraction technique (automated crystal orientation mapping (ACOM)), were applied to map the lithiation of the same location in the same sample. This enabled a direct comparison of the results. The maps obtained by all methods showed excellent agreement with each other. Because of the strong difference in the imaging mechanisms, it proves the reliability of both the spectroscopic and STEM diffraction phase mapping. A comprehensive comparison of all methods is given in terms of information content, dose level, acquisition time and signal quality. The latter three are crucial for the design of in-situ experiments with beam sensitive Li-ion battery materials. Furthermore, we demonstrated the power of STEM diffraction (ACOM-STEM) providing additional crystallographic information, which can be analyzed to gain a deeper understanding of the LFP/FP interface properties such as statistical information on phase boundary orientation and misorientation between domains. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

Novel Transrotational Solid State Order Discovered by TEM in Crystallizing Amorphous Films

Science.gov (United States)

Kolosov, Vladimir

Exotic thin crystals with unexpected transrotational microstructures have been discovered by transmission electron microscopy (TEM) for crystal growth in thin (10-100 nm) amorphous films of different chemical nature (oxides, chalcogenides, metals and alloys) prepared by various methods. Primarily we use our TEM bend contour technique. The unusual phenomenon can be traced in situ in TEM column: dislocation independent regular internal bending of crystal lattice planes in a growing crystal. Such transrotation (unit cell trans lation is complicated by small rotationrealized round an axis lying in the film plane) can result in strong regular lattice orientation gradients (up to 300 degrees per micrometer) of different geometries: cylindrical, ellipsoidal, toroidal, saddle, etc. Transrotation is increasing as the film gets thinner. Transrotational crystal resembles ideal single crystal enclosed in a curved space. Transrotational micro crystals have been eventually recognized by other authors in some vital thin film materials, i.e. PCMs for memory, silicides, SrTiO3. Atomic model and possible mechanisms of the phenomenon are discussed. New transrotational nanocrystalline model of amorphous state is also proposed Support of RF Ministry of Education and Science is acknowledged.

EBSD and FIB/TEM examination of shape memory effect deformation structures in U-14 at.% Nb

Energy Technology Data Exchange (ETDEWEB)

Clarke, A.J. [Materials Science and Technology Division, Mail Stop G770, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)], E-mail: aclarke@lanl.gov; Field, R.D.; McCabe, R.J.; Cady, C.M.; Hackenberg, R.E.; Thoma, D.J. [Materials Science and Technology Division, Mail Stop G770, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)

2008-06-15

Detailed examinations of shape memory effect (SME) deformation structures in martensite of U-14 at.% Nb were performed with electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). An accommodation strain analysis, which has been previously used to predict SME deformation structures and texture evolution in polycrystalline material, was also performed. Martensite variants and twin relationships observed with EBSD after compressive or tensile deformation were determined to be consistent with those expected from calculated accommodation strains. Focused ion beam (FIB) was used to select twinned regions identified with EBSD for more detailed TEM analysis to verify the presence of these specific twins. The observed SME twinning systems in the martensite agree with previous TEM observations and the predicted {l_brace}1-bar76{r_brace} twinning system was observed experimentally for the first time in U-14 at.% Nb using these complementary techniques.

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.

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.

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.

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)

The tetraspanin web revisited by super-resolution microscopy.

Science.gov (United States)

Zuidscherwoude, Malou; Göttfert, Fabian; Dunlock, Vera Marie E; Figdor, Carl G; van den Bogaart, Geert; van Spriel, Annemiek B

2015-07-17

The spatial organization of membrane proteins in the plasma membrane is critical for signal transduction, cell communication and membrane trafficking. Tetraspanins organize functional higher-order protein complexes called 'tetraspanin-enriched microdomains (TEMs)' via interactions with partner molecules and other tetraspanins. Still, the nanoscale organization of TEMs in native plasma membranes has not been resolved. Here, we elucidated the size, density and distribution of TEMs in the plasma membrane of human B cells and dendritic cells using dual color stimulated emission depletion (STED) microscopy. We demonstrate that tetraspanins form individual nanoclusters smaller than 120 nm and quantified that a single tetraspanin CD53 cluster contains less than ten CD53 molecules. CD53 and CD37 domains were adjacent to and displayed only minor overlap with clusters containing tetraspanins CD81 or CD82. Moreover, CD53 and CD81 were found in closer proximity to their partners MHC class II and CD19 than to other tetraspanins. Although these results indicate that tetraspanin domains are adjacently positioned in the plasma membrane, they challenge the current view of the tetraspanin web of multiple tetraspanin species organized into a single domain. This study increases the molecular understanding of TEMs at the nanoscale level which is essential for comprehending tetraspanin function in cell biology.

TEM microstructural analysis of creep deformed CM186LC single crystal Ni-base superalloy

Energy Technology Data Exchange (ETDEWEB)

Dubiel, B.; Czyrska-Filemonowicz, A. [AGH Univ. of Science and Technology, Krakow (Poland); Blackler, M. [Howmet Ltd., Exeter (United Kingdom); Barnard, P.M. [ALSTOM Power Turbo-Systems Technology Centre, Rugby (United Kingdom)

2006-07-01

The nickel based single crystal superalloy CM186LC was extensively investigated as a potential low cost material for industrial gas turbine vanes within the COST522 programme. The alloy exhibits inhomogeneous structure consisting of dendritic regions and eutectic colonies. In the present work attention is focused on microstructural changes observed in single crystal CM186LC following creep deformation at 750 C. Creep tests were conducted at 750 C with an applied stress of 560 or 675 MPa for up to 11440 hours. The microstructure o ruptured and terminated specimens was investigated by scanning (SEM) and transmission (TEM) electron microscopy. TEM analysis revealed the microstructural changes in the CM186LC at primary and secondary creep as well as after creep rupture. (orig.)

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...

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.

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.

Post-ion beam induced degradation of copper layers in transmission electron microscopy specimens

Science.gov (United States)

Seidel, F.; Richard, O.; Bender, H.; Vandervorst, W.

2015-11-01

Copper containing transmission electron microscopy (TEM) specimens frequently show corrosion after focused ion beam (FIB) preparation. This paper reveals that the corrosion product is a Cu-S phase growing over the specimen surface. The layer is identified by energy-dispersive x-ray spectroscopy, and lattice spacing indexing of power spectra patterns. The corrosion process is further studied by TEM on cone-shaped specimens, which are intentionally stored after FIB preparation with S flakes for short time. Furthermore, a protective method against corrosion is developed by varying the time in the FIB vacuum and the duration of a subsequent plasma cleaning.

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.

Measurement and correlation of optical and TEM twins in Y/sub 1/Ba/sub 2/Cu/sub 3/O/sub 7-δ/

International Nuclear Information System (INIS)

Chumbley, L.S.; Verhoeven, J.D.; Kim, M.R.; Cornelius, A.L.; Kramer, M.J.

1989-01-01

The spacing of the twins present in Y/sub 1/Ba/sub 2/Cu/sub 3/O/sub 7-δ/ has been investigated using optical and Transmission Electron Microscopy (TEM). Studies have reported that the value of the average twin spacing obtained by optical measurements is much larger than that measured in thin foils prepared for TEM observation, and controversy exists as to the exact nature of the optical twins. Experiments have been conducted which show that the twins observed optically correspond to those seen using TEM and are not produced by an optical interference effect. Using electron channeling, equations have been formulated which allow optical determination of the true spacing of twins present in a selected grain as well as the orientation of that grain. The average twin spacing measured in TEM has been found to vary with sample preparation method, being smaller for crushed chip samples than for bulk samples prepared by ion milling or jet-polishing. A variation of the twin spacing with grain size has also been noted

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

In situ measurements and transmission electron microscopy of carbon nanotube field-effect transistors

International Nuclear Information System (INIS)

Kim, Taekyung; Kim, Seongwon; Olson, Eric; Zuo Jianmin

2008-01-01

We present the design and operation of a transmission electron microscopy (TEM)-compatible carbon nanotube (CNT) field-effect transistor (FET). The device is configured with microfabricated slits, which allows direct observation of CNTs in a FET using TEM and measurement of electrical transport while inside the TEM. As demonstrations of the device architecture, two examples are presented. The first example is an in situ electrical transport measurement of a bundle of carbon nanotubes. The second example is a study of electron beam radiation effect on CNT bundles using a 200 keV electron beam. In situ electrical transport measurement during the beam irradiation shows a signature of wall- or tube-breakdown. Stepwise current drops were observed when a high intensity electron beam was used to cut individual CNT bundles in a device with multiple bundles

Dynamics of soft Nanomaterials captured by transmission electron microscopy in liquid water

Energy Technology Data Exchange (ETDEWEB)

Proetto, Maria T.; Rush, Anthony M.; Chien, Miao-Ping; Abellan Baeza, Patricia; Patterson, Joseph P.; Thompson, Matthew P.; Olson, Norman H.; Moore, Curtis E.; Rheingold, Arnold L.; Andolina, Christopher; Millstone, Jill; Howell, Stephen B.; Browning, Nigel D.; Evans, James E.; Gianneschi, Nathan C.

2014-01-14

In this paper 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 characterization 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 polymerization of an oxaliplatin analog, designed for an ongoing program in novel chemotherapeutic delivery systems. The resulting nanoparticles provided sufficient contrast for facile imaging in situ, and point toward key design parameters that enable this new characterization approach for organic nanomaterials. We describe the preparation of the synthetic micellar nanoparticles to- gether with their characterization in liquid water.

Electron holography for polymer microscopy

International Nuclear Information System (INIS)

Joy, D.C.

1992-01-01

Electron holography provides a radically new approach to the problem of imaging objects such as macromolecules, which exhibit little or no contrast when viewed in the conventional transmission electron microscope (TEM). This is overcome in electron holography by using the macromolecule as a phase object. Computer reconstruction of the hologram then allows the phase to be viewed as an image, and amplified. Holography requires a TEM with a field emission gun, and with an electro-static biprism to produce the interference pattern. The hologram requires a similar radiation dose to conventional microscopy but many different images (e.g. a through focal series) can be extracted from the same hologram. Further developments of the technique promise to combine high contrast imaging of the bulk of the macromolecule together with high spatial resolution imaging of surface detail

Quantitative electron microscopy and spectroscopy of MgB2 wires and tapes

International Nuclear Information System (INIS)

Birajdar, B; Peranio, N; Eibl, O

2008-01-01

In MgB 2 the correlation of microstructure with superconducting properties, in particular the critical current density, requires powerful analytical tools. Critical current densities and electrical resistivities of different MgB 2 superconductors differ by orders of magnitudes and the current limiting mechanisms have not been fully understood. Granularity of MgB 2 is one significant reason for reduced critical current densities and is introduced intrinsically by the anisotropy of B c2 but also extrinsically by the microstructure of the material. B c2 enhancement by doping is another important challenge for chemical analysis and, at present, doping levels are not well controlled on the sub-μm scale. In this paper the quantitative electron microscopy and spectroscopy methods essential for the microstructural analysis of MgB 2 are described. By quantitative electron microscopy and spectroscopy we mean a combined SEM and TEM analysis that covers various length scales from μm to nm. Contamination-free sample preparation, chemical mapping including B, and advanced chemical quantification using x-ray microanalysis were essential elements of the applied methodology. The methodology was applied to in situ and ex situ MgB 2 wires and tapes with and without SiC additives. Quantitative B analysis by EDX spectroscopy was applied quantitatively in the SEM and TEM, which is a major achievement. Although MgB 2 is a binary system, the thermodynamics of phase formation is complex, and the complexity is dramatically increased if additives like SiC are used. The small, sub-μm grain sizes of the matrix and secondary phases require TEM methods. However, granularity on the μm scale was also identified and underlines the importance of the combined SEM and TEM studies. Significant differences in the microstructure were observed for in situ and ex situ samples. This holds particularly if SiC was added and yielded Mg 2 Si for in situ samples annealed at 600-650 deg. C and Mg-Si-O phases

MT3FT-15OR0204122: Report on the acquisition and installation of FEI Talos F200X S/TEM

Energy Technology Data Exchange (ETDEWEB)

Parish, Chad M. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

2015-09-01

This document describes the installation, performance, and early results from the FCRD-funded acquisition of a new advanced analytical scanning / transmission electron microscopy (S/TEM) at the Oak Ridge National Laboratory Low Activation Materials Development and Analysis (LAMDA) facility.

TEM investigation of discommensurations in a Bi-Sr-Ca-Cu-O superconductor

International Nuclear Information System (INIS)

El boussiri, K.; Rais, T.; Schneck, J.; Toledano, J.C.; Morin, D.

1997-01-01

We were able to observe, by transmission electron microscopy (TEM), a certain type ot defects in the superconducting bismuth cuprates. High-resolution evidence for the translation slip across a wall is obtained in this material. A consistent relationship is established between the observed characteristics of the walls in this family: number of walls merging at a node, average distance between discommensurations, value of the modulation wavenumber. We show that a wide range of ''latent'' commensurate periods ''4b'', determine the characteristics of the walls. (orig.)

Transmission electron microscopy and diffractometry of materials

CERN Document Server

Fultz, Brent

2001-01-01

This book teaches graduate students the concepts of trans- mission electron microscopy (TEM) and x-ray diffractometry (XRD) that are important for the characterization of materi- als. It emphasizes themes common to both techniques, such as scattering from atoms and the formation and analysis of dif- fraction patterns. It also describes unique aspects of each technique, especially imaging and spectroscopy in the TEM. The textbook thoroughly develops both introductory and ad- vanced-level material, using over 400 accompanying illustra- tions. Problems are provided at the end of each chapter to reinforce key concepts. Simple citatioins of rules are avoi- ded as much as possible, and both practical and theoretical issues are explained in detail. The book can be used as both an introductory and advanced-level graduate text since sec- tions/chapters are sorted according to difficulty and grou- ped for use in quarter and semester courses on TEM and XRD.

Reference nano-dimensional metrology by scanning transmission electron microscopy

International Nuclear Information System (INIS)

Dai, Gaoliang; Fluegge, Jens; Bosse, Harald; Heidelmann, Markus; Kübel, Christian; Prang, Robby

2013-01-01

Traceable and accurate reference dimensional metrology of nano-structures by scanning transmission electron microscopy (STEM) is introduced in the paper. Two methods, one based on the crystal lattice constant and the other based on the pitch of a feature pair, were applied to calibrate the TEM magnification. The threshold value, which was defined as the half-intensity of boundary materials, is suggested to extract the boundary position of features from the TEM image. Experimental investigations have demonstrated the high potential of the proposed methods. For instance, the standard deviation from ten repeated measurements of a line structure with a nominal 100 nm critical dimension (CD) reaches 1σ = 0.023 nm, about 0.02%. By intentionally introduced defocus and larger sample alignment errors, the investigation shows that these influences may reach 0.20 and 1.3 nm, respectively, indicating the importance of high-quality TEM measurements. Finally, a strategy for disseminating the destructive TEM results is introduced. Using this strategy, the CD of a reference material has been accurately determined. Its agreement over five independent TEM measurements is below 1.2 nm. (paper)

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

"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.

TEM characterization of catalyst- and mask-free grown GaN nanorods

International Nuclear Information System (INIS)

Schowalter, M; Aschenbrenner, T; Kruse, C; Hommel, D; Rosenauer, A

2010-01-01

Catalyst- and mask-free grown GaN nanorods have been investigated using transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM) and energy filtered transmission electron microscopy (EFTEM). The nanorods were grown on nitridated r-plane sapphire substrates in a molecular beam epitaxy reactor. We investigated samples directly after the nitridation and after the overgrowth of the structure with GaN. High resolution transmission electron microscopy (HRTEM) and EFTEM revealed that AlN islands have formed due to nitridation. After overgrowth, the AlN islands could not be observed any more, neither by EFTEM nor by Z-contrast imaging. Instead, a smooth layer consisting of AlGaN was found. The investigation of the overgrown sample revealed that an a-plane GaN layer and GaN nanorods on top of the a-plane GaN have formed. The nanorods reduced from top of the a-plane GaN towards the a-plane GaN/sapphire interface suggesting that the nanorods originate at the AlN islands found after nitridation. However, this could not be shown unambiguously. The number of threading dislocations in the nanorods was very low. The analysis of the epitaxial relationship to the a-plane GaN showed that the nanorods grew along the [000-1] direction, and the [1-100] direction of the rods was parallel to the [0001] direction of the a-plane GaN.

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

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.

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)

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

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

Energy Technology Data Exchange (ETDEWEB)

Corazza, Michael, E-mail: michael.corazza@gmail.com [Department of Energy Conversion and Storage, Technical University of Denmark, Frederiksborgvej 399, 4000 Roskilde (Denmark); Simonsen, Søren B. [Department of Energy Conversion and Storage, Technical University of Denmark, Frederiksborgvej 399, 4000 Roskilde (Denmark); Gnaegi, Helmut [Diatome Ltd., Biel-Bienne (Switzerland); Thydén, Karl T.S.; Krebs, Frederik C.; Gevorgyan, Suren A. [Department of Energy Conversion and Storage, Technical University of Denmark, Frederiksborgvej 399, 4000 Roskilde (Denmark)

2016-12-15

Highlights: • Comparison of flexible solar cell sections prepared by ultramicrotomy and by FIB. • Energy filtered TEM analysis of phase separation in the P3HT:PCBM active layer. • Imaging of aging effects on solar cell cross section prepared by ultramicrotomy. • Ultramicrotomy provides great details while FIB better preserves the structure. - Abstract: 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 (PET) substrate. Focused ion beam (FIB) and ultramicrotomy were used to prepare the cross sections. The differences between the samples prepared by ultramicrotomy and FIB are addressed, focusing on the advantages and disadvantages of each technique. The sample prepared by ultramicrotomy yielded good 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 by ultramicrotomy are further discussed, which reveal particular effects of the ISOS-L-3 aging test (85 °C, 50% R.H., 0.7 Sun) onto the sample, especially pronounced in the silver layer.

Quantitative Transmission Electron Microscopy of Nanoparticles and Thin-Film Formation in Electroless Metallization of Polymeric Surfaces

Science.gov (United States)

Dutta, Aniruddha; Heinrich, Helge; Kuebler, Stephen; Grabill, Chris; Bhattacharya, Aniket

2011-03-01

Gold nanoparticles(Au-NPs) act as nucleation sites for electroless deposition of silver on functionalized SU8 polymeric surfaces. Here we report the nanoscale morphology of Au and Ag nanoparticles as studied by Transmission Electron Microscopy (TEM). Scanning TEM with a high-angle annular dark-field detector is used to obtain atomic number contrast. From the intensity-calibrated plan-view scanning TEM images we determine the mean thickness and the volume distribution of the Au-NPs on the surface of the functionalized polymer. We also report the height and the radius distribution of the gold nanoparticles obtained from STEM images taking into consideration the experimental errors. The cross sectional TEM images yield the density and the average distance of the Au and Ag nanoparticles on the surface of the polymer. Supported by grant NSF, Chemistry Division.

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)

Copper implantation defects in MgO observed by positron beam analysis, RBS and X-TEM

International Nuclear Information System (INIS)

Huis, M.A. van; Fedorov, A.V.; Veen, A. van; Smulders, P.J.M.; Kooi, B.J.; Hosson, J.Th.M. de

2000-01-01

In this work, effects of copper ion implantation in MgO were studied. (1 0 0) MgO samples were implanted with 50 keV Cu ions and thermally annealed stepwise in air for 30 minutes at 550, 750, 1000, 1250 and 1350 K. After ion implantation and after each annealing step, the samples were analysed with positron beam analysis (PBA). Use was also made of Rutherford backscattering spectrometry/channeling (RBS-C) and cross-sectional transmission electron microscopy (X-TEM). The combination of these techniques enabled to monitor the depth resolved evolution of both created defects and the copper atom depth distribution. PBA results show that copper implantation at a dose of 10 15 ions cm -2 yields a single layer of vacancy type defects after annealing. However a copper implantation at a dose of 10 16 ions cm -2 clearly yields two layers of defects in the material after annealing, separated by an intermediate layer. In both layers nanocavities have been identified. RBS experimental results show that the implanted copper atoms diffuse into the bulk material during annealing. X-TEM and channeling results show that after annealing, the lattice of the copper nanoprecipitates is epitaxial to the MgO host lattice. Under some circumstances, copper precipitates and small voids can co-exist. Furthermore, X-TEM measurements show that the nanocavities have rectangular shapes

Investigation of ceramic devices by analytical electron microscopy techniques

International Nuclear Information System (INIS)

Shiojiri, M.; Saijo, H.; Isshiki, T.; Kawasaki, M.; Yoshioka, T.; Sato, S.; Nomura, T.

1999-01-01

Ceramics are widely used as capacitors and varistors. Their electrical properties depend on the structure, which is deeply influenced not only by the composition of raw materials and additives but also by heating treatments in the production process. This paper reviews our investigations of SrTiO 3 ceramic devices, which have been performed using various microscopy techniques such as high-resolution transmission electron microscopy (HRTEM), cathodoluminescence scanning electron microscopy (CLSEM), field emission SEM (FE-SEM), energy dispersive X-ray spectroscopy (EDS), electron energy-loss spectroscopy (EELS) and high angle annular dark field (HAADF) imaging method in a FE-(scanning) transmission electron microscope(FE-(S)TEM). (author)

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

TEM microstructural characterization of melt-spun aged Al-6Si-3Cu-xMg alloys

International Nuclear Information System (INIS)

Lopez, Ismeli Alfonso; Zepeda, Cuauhtemoc Maldonado; Gonzalez Reyes, Jose Gonzalo; Flores, Ariosto Medina; Rodriguez, Juan Serrato; Gomez, Luis Bejar

2007-01-01

Three Al-6Si-3Cu-xMg alloys (x = 0.59, 3.80 and 6.78 wt.%) were produced using melt-spinning. As-melt-spun ribbons were aged at 150, 180 and 210 deg. C for times between 0.05 and 100 h. Microstructural changes were examined using transmission electron microscopy (TEM) and microhardness was measured. TEM analysis of the as-melt-spun alloys revealed 5 nm nanoparticles and larger particles (50 nm) composed of Al 2 Cu (θ) for the 0.59% Mg alloy and Al 5 Cu 2 Mg 8 Si 6 (Q) for 3.80% and 6.78% Mg alloys. Silicon solid solubility was extended to 9.0 at.% and Mg in solid solution reached 6.7 at.%. After aging treatments the 6.78% Mg alloy exhibited the most significant increase in microhardness, reaching 260 kg/mm 2 . TEM analysis of aged specimens also showed θ and Q phase (5-20 nm nanoparticles and 35-40 nm particles). The combination of the volume fraction and size of the particles plays an important role in microhardness variation

Edge-melting: nanoscale key-mechanism to explain nanoparticle formation from heated TEM grids

Energy Technology Data Exchange (ETDEWEB)

Cesaria, Maura, E-mail: maura.cesaria@le.infn.it [Department of Mathematics and Physics “E. De Giorgi”, University of Salento, Via Arnesano, 73100 Lecce (Italy); Taurino, Antonietta; Catalano, Massimo [Institute for Microelectronics and Microsystems, IMM-CNR, Via Monteroni, 73100 Lecce (Italy); Caricato, Anna Paola; Martino, Maurizio [Department of Mathematics and Physics “E. De Giorgi”, University of Salento, Via Arnesano, 73100 Lecce (Italy)

2016-03-01

Graphical abstract: - Highlights: • Nanoparticle formation from metal grids explained by edge melting as key mechanism. • The inconsistency of bulk phenomenology invoking the vapor pressure is discussed. • Surface-melting and size-dependent evaporation are questioned as unsatisfactory. • Edge-melting: edges, corners, facets invoked as highly thermally unstable surfaces. • The polycrystalline nature of the really occurring metal grids is accounted for. - Abstract: In this study, we examine at both experimental and fundamental levels, the experimental evidence of nanoparticle formation in transmission electron microscopy (TEM) metal grids annealed at temperatures lower than the melting point of the corresponding metal bulk material. Our experimental investigation considers the most thermally unstable TEM grids (i.e. Cu-grids) and inspects the possible sources and mechanisms of contamination of thin films, conventionally deposited on carbon-coated Cu-grids. The investigations are supported by morphological–compositional analyses performed in different regions of the TEM sample. Then, a general model is formulated and discussed in order to explain the grid thermal instability, based on the critical role of edge-melting (i.e. melting initiated at edges and corners of the grid bars), the enhanced rate of evaporation from a liquid surface and the polycristallinity of the grid bars. Hence, we totally disregard conventional arguments such as bulk evaporation and metal vapor pressure and, in order to emphasize and clarify the alternative point of view of our model, we also overview the nano-scale melting phenomenology relevant to our discussion and survey the discrepancies reported in the literature.

Transmission electron microscopy of nanostructures synthesized by laser and charged particle beam interaction with materials

International Nuclear Information System (INIS)

Dey, G. K.

2011-01-01

Transmission Electron Microscopy (TEM), because of its ability to image atomic arrangements directly and its ability to give spectroscopic information at similar resolution has emerged as a very powerful tool for understanding the structure of materials at atomic level. TEM has been particularly useful in resolving the interface structures in materials. This form of microscopy is very suitable for resolving the structure and defects in ultrafine microstructures such as those of the nanocrystalline phases. After a brief description of the different characterization abilities of the aberration corrected transmission electron microscope, this presentation describes the results of TEM investigations on nanocrystalline microstructures generated by laser materials interaction and due to interaction of electrons and ions with materials. Excimer laser has become an attractive choice for new and precision application for ablation and deposition in recent times. In this work, a KrF excimer laser having 30 ns pulse width and 600 mJ energy at source has been used to deposit zirconia on Zr-base alloy in order to explore the ability of the thin oxide film to act as a diffusion barrier to hydrogen ingress into the alloy. It has been found that the variation in pressure by an order of three has resulted in maximum influence on the roughness of the laser deposited oxide film that has not been possible to achieve by other parameters within the range of the instrument. Present study has also indicated an interrelation among the roughness, adherence and the film-thickness, where the last one is indicated by the XPS study. Transmission electron microscopy was carried out to study the size, size distribution and defects in the deposited film. Nanocrystalline phases generated by interaction of electron and ion irradiation of Zr based alloys; Ni based alloys and Fe based alloys have been examined in detail by conventional and high resolution transmission electron microscopy. Results of

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.

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.

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.

Static and Dynamic Electron Microscopy Investigations at the Atomic and Ultrafast Scales

Science.gov (United States)

Suri, Pranav Kumar

Advancements in the electron microscopy capabilities - aberration-corrected imaging, monochromatic spectroscopy, direct-electron detectors - have enabled routine visualization of atomic-scale processes with millisecond temporal resolutions in this decade. This, combined with progress in the transmission electron microscopy (TEM) specimen holder technology and nanofabrication techniques, allows comprehensive experiments on a wide range of materials in various phases via in situ methods. The development of ultrafast (sub-nanosecond) time-resolved TEM with ultrafast electron microscopy (UEM) has further pushed the envelope of in situ TEM to sub-nanosecond temporal resolution while maintaining sub-nanometer spatial resolution. A plethora of materials phenomena - including electron-phonon coupling, phonon transport, first-order phase transitions, bond rotation, plasmon dynamics, melting, and dopant atoms arrangement - are not yet clearly understood and could be benefitted with the current in situ TEM capabilities having atomic-level and ultrafast precision. Better understanding of these phenomena and intrinsic material dynamics (e.g. how phonons propagate in a material, what time-scales are involved in a first-order phase transition, how fast a material melts, where dopant atoms sit in a crystal) in new-generation and technologically important materials (e.g. two-dimensional layered materials, semiconductor and magnetic devices, rare-earth-element-free permanent magnets, unconventional superconductors) could bring a paradigm shift in their electronic, structural, magnetic, thermal and optical applications. Present research efforts, employing cutting-edge static and dynamic in situ electron microscopy resources at the University of Minnesota, are directed towards understanding the atomic-scale crystallographic structural transition and phonon transport in an iron-pnictide parent compound LaFeAsO, studying the mechanical stability of fast moving hard-drive heads in heat

Quantifying Chemical and Electrochemical Reactions in Liquids by in situ Electron Microscopy

DEFF Research Database (Denmark)

Canepa, Silvia

and developing a robust imaging analysis method for quantitatively understand chemical and electrochemical process during in situ liquid electron microscopy. By using two custom-made liquid cells (an electrochemical scanning electron microscopy (EC-SEM) platform and Liquid Flow S/TEM holder) beam...... of electrochemical deposition of copper (Cu) by electrochemical liquid scanning electron microscopy (EC-SEM) was done in order to direct observe the formation of dendritic structures. Finally the shape evolution from solid to hollow structures through galvanic replacement reactions were observed for different silver...

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.

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.

XRD, TEM, and thermal analysis of Arizona Ca-montmorillonites modified with didodecyldimethylammonium bromide.

Science.gov (United States)

Sun, Zhiming; Park, Yuri; Zheng, Shuilin; Ayoko, Godwin A; Frost, Ray L

2013-10-15

An Arizona SAz-2 calcium montmorillonite was modified by a typical dialkyl cationic surfactant (didodecyldimethylammonium bromide, abbreviated to DDDMA) through direct ion exchange. The obtained organoclays were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HR-TEM), high-resolution thermogravimetric analysis (HR-TG), and infrared emission spectroscopy (IES). The intercalation of surfactants greatly increased the basal spacing of the interlayers and the conformation arrangement of the loaded surfactant were assessed based on the XRD and TEM measurements. This work shows that the dialkyl surfactant can be directly intercalated into the montmorillonite without first undergoing Na(+) exchange. Moreover, the thermal stability of organoclays and the different arrangements of the surfactant molecules intercalated in the SAz-2 Ca-montmorillonite were determined by a combination of TG and IES techniques. The detailed conformational ordering of different intercalated surfactants under different conditions was also studied. The surfactant molecule DDDMA has proved to be thermally stable even at 400°C which indicates that the prepared organoclay is stable to significantly high temperatures. This study offers new insights into the structure and thermal stabilities of SAz-2 Ca-montmorillonite modified with DDDMA. The experimental results also confirm the potential applications of organic SAz-2 Ca-montmorillonites as adsorbents and polymer-clay nanocomposites. Copyright © 2013 Elsevier Inc. All rights reserved.

Novel lift-off technique for Transmission Electron Microscopy imaging of block copolymer films

International Nuclear Information System (INIS)

Roache, Fergus J.M.; Radjainia, Mazdak; Williams, David E.; Gerrard, Juliet A.; Travas-Sejdic, Jadranka; Malmström, Jenny

2015-01-01

We have developed a simple technique to allow for the lift-off and subsequent transfer of poly(styrene-block-ethylene glycol) films to Transmission Electron Microscopy (TEM) grids. The block copolymer is spin coated onto carbon coated mica and annealed. After the thin film is produced it can easily be floated onto water and picked up by a TEM grid. This method offers better control over film processing than dip coating the TEM grid and is also a significant improvement over methods using etchants such as hydrofluoric acid. - Highlights: • We have developed a simple method to lift block copolymer films to TEM grids. • Polymer films prepared on carbon coated mica are easily floated on water. • The new method circumvents the use of harsh chemicals

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.

Nanoprecipitates in single-crystal molybdenum-alloy nanopillars detected by TEM and atom probe tomography

International Nuclear Information System (INIS)

Oveisi, Emad; Bártová, Barbora; Gerstl, Stephan; Zimmermann, Julien; Marichal, Cécile; Van Swygenhoven, Helena; Hébert, Cécile

2013-01-01

Transmission electron microscopy (TEM) supported by various chemical analyses techniques as well as atom probe tomography is applied to characterize newly identified nanosized precipitates in Mo-alloy nanopillars that were prepared by directional solidification. It is shown that the α-Mo matrix contains Al-enriched face-centred cubic precipitates which have a 4.12 Å lattice parameter, and exhibit a Kurdjumov–Sachs crystallographic orientation relationship with the matrix. Such precipitates could be responsible for the unusual behaviour of the pillars during compression tests

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.

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.

Objective function analysis for electric soundings (VES), transient electromagnetic soundings (TEM) and joint inversion VES/TEM

Science.gov (United States)

Bortolozo, Cassiano Antonio; Bokhonok, Oleg; Porsani, Jorge Luís; Monteiro dos Santos, Fernando Acácio; Diogo, Liliana Alcazar; Slob, Evert

2017-11-01

Ambiguities in geophysical inversion results are always present. How these ambiguities appear in most cases open to interpretation. It is interesting to investigate ambiguities with regard to the parameters of the models under study. Residual Function Dispersion Map (RFDM) can be used to differentiate between global ambiguities and local minima in the objective function. We apply RFDM to Vertical Electrical Sounding (VES) and TEM Sounding inversion results. Through topographic analysis of the objective function we evaluate the advantages and limitations of electrical sounding data compared with TEM sounding data, and the benefits of joint inversion in comparison with the individual methods. The RFDM analysis proved to be a very interesting tool for understanding the joint inversion method of VES/TEM. Also the advantage of the applicability of the RFDM analyses in real data is explored in this paper to demonstrate not only how the objective function of real data behaves but the applicability of the RFDM approach in real cases. With the analysis of the results, it is possible to understand how the joint inversion can reduce the ambiguity of the methods.

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.

Microstructural differences between two Zr(C,N) coatings revealed by analytical transmission electron microscopy

International Nuclear Information System (INIS)

Dörfel, Ilona; Rooch, Heidemarie; Österle, Werner

2012-01-01

The microstructures of two samples of a Zr(C,N) coating on steel, which unexpectedly differed in their tribological properties, were investigated by analytical transmission electron microscopy. The samples were produced by a cathodic arc evaporation process in two commercial coating devices under similar coating conditions with the exception of the number of Zr targets. The source of the differing tribological properties of the samples was detected by analytical transmission electron microscopy (TEM) methods energy-dispersive X-ray spectroscopy (EDX), energy filtering TEM (EFTEM), electron diffraction, high resolution electron microscopy, and high angel annular dark field. The TEM preparation and the results of the TEM investigations are shown in detail. The origin of the unexpected behavior was determined to be a nano-scale multilayer structure that existed only in the tribologically superior specimen. EDX and EFTEM investigations indicated enrichment in oxygen at the interface between coating and steel substrate in the tribologically inferior sample. Findings of the microstructural configuration were obtained by taking a closer look at the structure and comparing the results of the several analytical TEM techniques. This allows the allocation of the concentration fluctuations in N, C, and Zr to the two thickness fractions of the nano multilayers and a local correlation of the identified minority phase Zr 3 (C,N) 4 to the higher N content in the narrower type of the multilayer fraction of the sample with the excellent tribological properties. The minority phase Zr 3 (C,N) 4 is randomly distributed in the sample with the defective tribological properties. Coating conditions are not topic of this work, but after discussion of the TEM results, the fact that one of the coating devices worked with one Zr target and the other one with two, could be identified as cause for the formation of the nano multilayer structure in the sample with the superior tribological

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).

In situ TEM observation of microcrack nucleation and propagation in pure tin solder

International Nuclear Information System (INIS)

Ding Ying; Wang Chunqing; Li, Mingyu; Wang Weiqiang

2006-01-01

Microcrack nucleation and propagation behavior in pure tin solder was investigated by using transmission electron microscopy (TEM) through in situ tensile test. Observation results showed that fracture process was completed in this visco-plastic material by connecting discontinuous cracks or voids. Depending on remarkable vacancy diffusion ability, microvoids were nucleated and developed in the dislocation free zone (DFZ) or super thinned area ahead of crack tip under local high stress concentration. The cracks were linked with each other by mutual dislocation emission which expedites the propagation of crack tips effectively

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.

TEM characterization of corrosion products formed on a SS-15ZR alloy

International Nuclear Information System (INIS)

Luo, J. S.; Abraham, D. P.

2000-01-01

The corrosion products formed on a stainless steel-15Zr (SS-15Zr) alloy have been characterized by transmission electron microscopy (TEM) and energy dispersive x-ray spectroscopy (EDS). Examination of alloy particles that were immersed in 90 C deionized water for two years revealed that different corrosion products were formed on the stainless steel and intermetallic phases. Two corrosion products were identified on an austenite particle: trevorite (NiFe 2 O 4 ) in the layer close to the metal and maghemite (Fe 2 O 3 ) in the outer layer. The corrosion layer formed on the intermetallic was uniform, adherent, and amorphous. The EDS analysis indicated that the layer was enriched in zirconium when compared with the intermetallic composition. High-resolution TEM images of the intermetallic-corrosion layer interface show an interlocking metal-oxide interface which may explain the relatively strong adherence of the corrosion layer to the intermetallic surface. These results will be used to evaluate corrosion mechanisms and predict long-term corrosion behavior of the alloy waste form

In situ TEM investigation on the precipitation behavior of μ phase in Ni-base single crystal superalloys

International Nuclear Information System (INIS)

Gao, Shuang; Liu, Zhi-Quan; Li, Cai-Fu; Zhou, Yizhou; Jin, Tao

2016-01-01

The precipitation behavior of μ phase in Ni-base single crystal superalloys was investigated by in situ transmission electron microscopy (TEM). A layer-by-layer growth process with a ledge propagation mechanism was first observed during in situ precipitation. Three types of μ phase with different morphologies were found, which grow along [001] μ with (001) μ planar defects, [-111] μ with (1–12) μ planar defects, as well as both directions with mixed planar defects. High-resolution TEM image and established atomic models reveal a basic growth mechanism of μ phase by stacking on (001) μ plane and randomly forming coherent planar defects, while the nucleation of incoherent (1–12) μ planar defects at the early stage of precipitation plays an important role in affecting the basic growth mechanism. The frequent faults during the stacking process of the sub-unit layers within μ lattice should be responsible for the defect formation. -- Graphical abstract: In situ transmission electron microscopy (TEM) investigations reveal the layer-by-layer growth mechanism of μ phase precipitated in Ni-base single crystal superalloys. Three types of μ phase with different morphologies were formed at 1050 °C, which grows along [001] μ with (001) μ planar defects, [-111] μ with (1–12) μ planar defects, as well as both directions with mixed planar defects respectively. Formation of (001) μ micro-twin and stacking fault is the essential feature for precipitated μ phase, while nucleation of incoherent (1–12) μ planar defects plays an important role in changing growth method. Display Omitted

HR-TEM and FT-Raman dataset of the caffeine interacted Phe–Phe peptide nanotube for possible sensing applications

Directory of Open Access Journals (Sweden)

A. Lakshmi Narayanan

2018-02-01

Full Text Available Sensing ability of caffeine interaction with Phe-Phe annotates (PNTs, is presented (Govindhan et al., 2017; Karthikeyan et al., 2014; Tavagnacco et al., 2013; Kennedy et al., 2011; Wang et al., 2017 [1–5] in this data set. Investigation of synthesized caffeine carrying peptide nanotubes are carried out by FT-Raman spectral analysis and high resolution transmission electron microscopy (HR-TEM. Particle size of the caffeine loaded PNTs is < 40 nm. The FT-Raman spectrum signals are enhanced in the region of 400–1700 cm−1. These data are ideal tool for the applications like biosensing and drug delivery research (DDS. Keywords: Caffeine, PNTs, Sensing, HR-TEM, FT-Raman data

Progress and applications of in situ transmission electron microscopy

International Nuclear Information System (INIS)

Wang Rongming; Liu Jialong; Song Yuanjun

2015-01-01

Recent progress in the application of in situ transmission electron microscopy (TEM) is briefly reviewed. It is emphasized that the development of advanced in situ TEM techniques makes it possible to investigate the evolution of materials under heat, strain, magnetic field, electric field or chemical reaction environments on the atomic scale. The mechanism of the microstructure evolution under various conditions and the relationship between the atomic structures and their properties can be obtained, which is beneficial for the design of new materials with tailored properties. The clarification of the structure-property relationship will help to develop new materials and solve related basic problems in the field of condensed matter physics. (authors)

Sample Preparation Methodologies for In Situ Liquid and Gaseous Cell Analytical Transmission Electron Microscopy of Electropolished Specimens.

Science.gov (United States)

Zhong, Xiang Li; Schilling, Sibylle; Zaluzec, Nestor J; Burke, M Grace

2016-12-01

In recent years, an increasing number of studies utilizing in situ liquid and/or gaseous cell scanning/transmission electron microscopy (S/TEM) have been reported. Because of the difficulty in the preparation of suitable specimens, these environmental S/TEM studies have been generally limited to studies of nanoscale structured materials such as nanoparticles, nanowires, or sputtered thin films. In this paper, we present two methodologies which have been developed to facilitate the preparation of electron-transparent samples from conventional bulk metals and alloys for in situ liquid/gaseous cell S/TEM experiments. These methods take advantage of combining sequential electrochemical jet polishing followed by focused ion beam extraction techniques to create large electron-transparent areas for site-specific observation. As an example, we illustrate the application of this methodology for the preparation of in situ specimens from a cold-rolled Type 304 austenitic stainless steel sample, which was subsequently examined in both 1 atm of air as well as fully immersed in a H2O environment in the S/TEM followed by hyperspectral imaging. These preparation techniques can be successfully applied as a general procedure for a wide range of metals and alloys, and are suitable for a variety of in situ analytical S/TEM studies in both aqueous and gaseous environments.

In Situ TEM Multi-Beam Ion Irradiation as a Technique for Elucidating Synergistic Radiation Effects

Energy Technology Data Exchange (ETDEWEB)

Taylor, Caitlin; Bufford, Daniel; Muntifering, Brittany; Senor, David; Steckbeck, Mackenzie; Davis, Justin; Doyle, Barney; Buller, Daniel; Hattar, Khalid

2017-09-29

Materials designed for nuclear reactors undergo microstructural changes resulting from a combination of several environmental factors, including neutron irradiation damage, gas accumulation and elevated temperatures. Typical ion beam irradiation experiments designed for simulating a neutron irradiation environment involve irradiating the sample with a single ion beam and subsequent characterization of the resulting microstructure, often by transmission electron microscopy (TEM). This method does not allow for examination of microstructural effects due to simultaneous gas accumulation and displacement cascade damage, which occurs in a reactor. Sandia’s in situ ion irradiation TEM (I3TEM) offers the unique ability to observe microstructural changes due to irradiation damage caused by concurrent multi-beam ion irradiation in real time. This allows for time-dependent microstructure analysis. A plethora of additional in situ stages can be coupled with these experiments, e.g., for more accurately simulating defect kinetics at elevated reactor temperatures. This work outlines experiments showing synergistic effects in Au using in situ ion irradiation with various combinations of helium, deuterium and Au ions, as well as some initial work on materials utilized in tritium-producing burnable absorber rods (TPBARs): zirconium alloys and LiAlO2.

In Situ TEM Multi-Beam Ion Irradiation as a Technique for Elucidating Synergistic Radiation Effects

Directory of Open Access Journals (Sweden)

Caitlin Anne Taylor

2017-09-01

Full Text Available Materials designed for nuclear reactors undergo microstructural changes resulting from a combination of several environmental factors, including neutron irradiation damage, gas accumulation and elevated temperatures. Typical ion beam irradiation experiments designed for simulating a neutron irradiation environment involve irradiating the sample with a single ion beam and subsequent characterization of the resulting microstructure, often by transmission electron microscopy (TEM. This method does not allow for examination of microstructural effects due to simultaneous gas accumulation and displacement cascade damage, which occurs in a reactor. Sandia’s in situ ion irradiation TEM (I3TEM offers the unique ability to observe microstructural changes due to irradiation damage caused by concurrent multi-beam ion irradiation in real time. This allows for time-dependent microstructure analysis. A plethora of additional in situ stages can be coupled with these experiments, e.g., for more accurately simulating defect kinetics at elevated reactor temperatures. This work outlines experiments showing synergistic effects in Au using in situ ion irradiation with various combinations of helium, deuterium and Au ions, as well as some initial work on materials utilized in tritium-producing burnable absorber rods (TPBARs: zirconium alloys and LiAlO2.

High-temperature in-situ TEM straining of the interaction with dislocations and particles for Cu-added ferritic stainless steel.

Science.gov (United States)

Kobayashi, Shuhei; Kaneko, Kenji; Yamada, Kazuhiro; Kikuchi, Masao; Kanno, Norihiro; Hamada, Junichi

2014-11-01

IntroductionCu is always present in the matrix when ferritic steels were prepared from ferrous scrap. When the ferritic steels are aged thermally, Cu precipitates start appear and disperse finely and homogeneously [1], which may make the steels strengthened by precipitation hardening. In this study, the interaction between Cu precipitates and dislocations was exmined via high-temperature in-situ TEM straining. ExperimentalCu-added ferritic stainless steel (Fe-18.4%Cr-1.5%Cu) was used in the present study. Specimen was aged at1073 K for 360 ks. Samples for TEM observation were prepared by focused ion beam (FIB; Quanta 3D 200i) method. Microstructure of specimen was analyzed by JEM-3200FSK and high-temperature in-situ TEM straining was conducted using JEM-1300NEF. Results and discussionInteraction between Cu precipitates and dislocation is seen from consecutive TEM images acquired by in-situ TEM straining at 1073 K, as shown in Fig.1. The size of Cu precipitates was about 70 nm and several dislocations were present within the field of view. In particular, progressing dislocations contacted with the Cu precipitate at right angle, as indicated by arrows in Fig.1 (b) to (d). This result implies that there is an attractive interaction between dislocations and the Cu precipitate. This is attributed to the fact that Stress field of dislocations was easily relaxed in interface between the Cu precipitate and matrix because of lattice and interface diffusion as well as slip in the interface [2,3]. Furthermore, dislocations pass through the particle after contacting it, so that the interaction with dislocations and particles should be explained by Srolovitz mechanism [4].jmicro;63/suppl_1/i28/DFU083F1F1DFU083F1Fig. 1.TEM images foucused on interaction with dislocations and partticles. © 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.

Cross-sectional transmission electron microscopy of semiconductors

International Nuclear Information System (INIS)

Sadana, D.K.

1982-10-01

A method to prepare cross-sectional (X) semiconductor specimens for transmission electron microscopy (TEM) has been described. The power and utility of XTEM has been demonstrated. It has been shown that accuracy and interpretation of indirect structural-defects profiling techniques, namely, MeV He + channeling and secondary ion mass spectrometry (SIMS) can be greatly enhanced by comparing their results with those obtained by XTEM from the same set of samples

Atomic force microscopy applied to the quantification of nano-precipitates in thermo-mechanically treated microalloyed steels

Energy Technology Data Exchange (ETDEWEB)

Renteria-Borja, Luciano [Instituto Tecnologico de Morelia, Av. Tecnologico No. 1500, Lomas de Santiaguito, 58120 Morelia (Mexico); Hurtado-Delgado, Eduardo, E-mail: hurtado@itmorelia.edu.mx [Instituto Tecnologico de Morelia, Av. Tecnologico No. 1500, Lomas de Santiaguito, 58120 Morelia (Mexico); Garnica-Gonzalez, Pedro [Instituto Tecnologico de Morelia, Av. Tecnologico No. 1500, Lomas de Santiaguito, 58120 Morelia (Mexico); Dominguez-Lopez, Ivan; Garcia-Garcia, Adrian Luis [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada-IPN Unidad Queretaro, Cerro Blanco No. 141, Colinas del Cimatario, 76090 Queretaro (Mexico)

2012-07-15

Quantification of nanometer-size precipitates in microalloyed steels has been traditionally performed using transmission electron microscopy (TEM), in spite of its complicated sample preparation procedures, prone to preparation errors and sample perturbation. In contrast to TEM procedures, atomic force microscopy (AFM) is performed on the as-prepared specimen, with sample preparation requirements similar to those for optical microscopy (OM), rendering three-dimensional representations of the sample surface with vertical resolution of a fraction of a nanometer. In AFM, contrast mechanisms are directly related to surface properties such as topography, adhesion, and stiffness, among others. Chemical etching was performed using 0.5% nital, at time intervals between 4 and 20 s, in 4 s steps, until reaching the desired surface finish. For the present application, an average surface-roughness peak-height below 200 nm was sought. Quantification results of nanometric precipitates were obtained from the statistical analysis of AFM images of the microstructure developed by microalloyed Nb and V-Mo steels. Topography and phase contrast AFM images were used for quantification. The results obtained using AFM are consistent with similar TEM reports. - Highlights: Black-Right-Pointing-Pointer We quantified nanometric precipitates in Nb and V-Mo microalloyed steels using AFM. Black-Right-Pointing-Pointer Microstructures of the thermo-mechanically treated microalloyed steels were used. Black-Right-Pointing-Pointer Topography and phase contrast AFM images were used for quantification. Black-Right-Pointing-Pointer AFM results are comparable with traditionally obtained TEM measurements.

Collaboration at the Nanoscale: Exploring Viral Genetics with Electron Microscopy

Science.gov (United States)

Duboise, S. Monroe; Moulton, Karen D.; Jamison, Jennifer L.

2009-01-01

The Maine Science Corps is a project sponsored by the National Science Foundation's (NSF) Graduate Teaching Fellows in K-12 Education (GK-12 ) program. Through this program, the University of Southern Maine's (USM) virology and transmission electron microscopy (TEM) research group provides high school teachers and students in rural areas with…

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

A developed wedge fixtures assisted high precision TEM samples pre-thinning method: Towards the batch lamella preparation

Directory of Open Access Journals (Sweden)

Dandan Wang

2017-04-01

Full Text Available Ion milling, wedge cutting or polishing, and focused ion beam (FIB milling are widely-used techniques for the transmission electron microscope (TEM sample preparation. Especially, the FIB milling provides a site-specific analysis, deposition, and ablation of materials in the micrometer and nanometer scale. However, the cost of FIB tools has been always a significant concern. Since it is inevitable to use the FIB technique, the improvement of efficiency is a key point. Traditional TEM sample preparation with FIB was routinely implemented on a single sample each time. Aiming at cost efficiency, a new pre-thinning technique for batch sample preparation was developed in this paper. The present proposal combines the sample preparation techniques with multi-samples thinning, cross-section scanning electron microscopy (SEM, wedge cutting, FIB and other sample pre-thinning techniques. The new pre-thinning technique is to prepare an edge TEM sample on a grinding and polishing fixture with a slant surface. The thickness of the wedges sample can be measured to 1∼2 μm under optical microscope. Therefore, this fixture is superior to the traditional optical method of estimating the membrane thickness. Moreover, by utilizing a multi-sample holding fixture, more samples can be pre-thinned simultaneously, which significantly improved the productivity of TEM sample preparation.

Localization of Minodronate in Mouse Femora Through Isotope Microscopy

Science.gov (United States)

Hongo, Hiromi; Sasaki, Muneteru; Kobayashi, Sachio; Hasegawa, Tomoka; Yamamoto, Tomomaya; Tsuboi, Kanako; Tsuchiya, Erika; Nagai, Tomoya; Khadiza, Naznin; Abe, Miki; Kudo, Ai; Oda, Kimimitsu; Henrique Luiz de Freitas, Paulo; Li, Minqi; Yurimoto, Hisayoshi; Amizuka, Norio

2016-01-01

Minodronate is highlighted for its marked and sustained effects on osteoporotic bones. To determine the duration of minodronate’s effects, we have assessed the localization of the drug in mouse bones through isotope microscopy, after labeling it with a stable nitrogen isotope ([15N]-minodronate). In addition, minodronate-treated bones were assessed by histochemistry and transmission electron microscopy (TEM). Eight-week-old male ICR mice received [15N]-minodronate (1 mg/kg) intravenously and were sacrificed after 3 hr, 24 hr, 1 week, and 1 month. Isotope microscopy showed that [15N]-minodronate was present mainly beneath osteoblasts rather than nearby osteoclasts. At 3 hr after minodronate administration, histochemistry and TEM showed osteoclasts with well-developed ruffled borders. However, osteoclasts were roughly attached to the bone surfaces and did not feature ruffled borders at 24 hr after minodronate administration. The numbers of tartrate-resistant acid phosphatase–positive osteoclasts and alkaline phosphatase–reactive osteoblastic area were not reduced suddenly, and apoptotic osteoclasts appeared in 1 week and 1 month after the injections. Von Kossa staining demonstrated that osteoclasts treated with minodronate did not incorporate mineralized bone matrix. Taken together, minodronate accumulates in bone underneath osteoblasts rather than under bone-resorbing osteoclasts; therefore, it is likely that the minodronate-coated bone matrix is resistant to osteoclastic resorption, which results in a long-lasting and bone-preserving effect. PMID:27666429

Practical aspects of the use of the X(2) holder for HRTEM-quality TEM sample preparation by FIB.

Science.gov (United States)

van Mierlo, Willem; Geiger, Dorin; Robins, Alan; Stumpf, Matthias; Ray, Mary Louise; Fischione, Paul; Kaiser, Ute

2014-12-01

The X(2) holder enables the effective production of thin, electron transparent samples for high-resolution transmission electron microscopy (HRTEM). Improvements to the X(2) holder for high-quality transmission electron microscopy (TEM) sample preparation are presented in this paper. We discuss the influence of backscattered electrons (BSE) from the sample holder in determining the lamella thickness in situ and demonstrate that a significant improvement in thickness determination can be achieved by comparatively simple means using the relative BSE intensity. We show (using Monte Carlo simulations) that by taking into account the finite collection angle of the electron backscatter detector, an approximately 20% underestimation of the lamella thickness in a silicon sample can be avoided. However, a correct thickness determination for light-element lamellas still remains a problem with the backscatter method; we introduce a more accurate method using the energy dispersive X-ray spectroscopy (EDX) signal for in situ thickness determination. Finally, we demonstrate how to produce a thin lamella with a nearly damage-free surface using the X(2) holder in combination with sub-kV polishing in the Fischione Instruments׳ NanoMill(®) TEM specimen preparation system. Copyright © 2014 Elsevier B.V. All rights reserved.

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

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

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.

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.

Electron beam fabrication and characterization of high- resolution magnetic force microscopy tips

NARCIS (Netherlands)

Ruhrig, M.; Rührig, M.; Porthun, S.; Porthun, S.; Lodder, J.C.; Mc vitie, S.; Heyderman, L.J.; Johnston, A.B.; Chapman, J.N.

1996-01-01

The stray field, magnetic microstructure, and switching behavior of high‐resolution electron beam fabricated thin film tips for magnetic force microscopy (MFM) are investigated with different imaging modes in a transmission electron microscope (TEM). As the tiny smooth carbon needles covered with a

Fourier-space TEM reconstructions with symmetry adapted functions for all rotational point groups.

Science.gov (United States)

Trapani, Stefano; Navaza, Jorge

2013-05-01

A general-purpose and simple expression for the coefficients of symmetry adapted functions referred to conveniently oriented symmetry axes is given for all rotational point groups. The expression involves the computation of reduced Wigner-matrix elements corresponding to an angle specific to each group and has the computational advantage of leading to Fourier-space TEM (transmission electron microscopy) reconstruction procedures involving only real valued unknowns. Using this expression, a protocol for ab initio view and center assignment and reconstruction so far used for icosahedral particles has been tested with experimental data in other point groups. Copyright © 2013 Elsevier Inc. All rights reserved.

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...

Advanced scanning transmission stereo electron microscopy of structural and functional engineering materials

International Nuclear Information System (INIS)

Agudo Jácome, L.; Eggeler, G.; Dlouhý, A.

2012-01-01

Stereo transmission electron microscopy (TEM) provides a 3D impression of the microstructure in a thin TEM foil. It allows to perform depth and TEM foil thickness measurements and to decide whether a microstructural feature lies inside of a thin foil or on its surface. It allows appreciating the true three-dimensional nature of dislocation configurations. In the present study we first review some basic elements of classical stereo TEM. We then show how the method can be extended by working in the scanning transmission electron microscope (STEM) mode of a modern analytical 200 kV TEM equipped with a field emission gun (FEG TEM) and a high angle annular dark field (HAADF) detector. We combine two micrographs of a stereo pair into one anaglyph. When viewed with special colored glasses the anaglyph provides a direct and realistic 3D impression of the microstructure. Three examples are provided which demonstrate the potential of this extended stereo TEM technique: a single crystal Ni-base superalloy, a 9% Chromium tempered martensite ferritic steel and a NiTi shape memory alloy. We consider the effect of camera length, show how foil thicknesses can be measured, and discuss the depth of focus and surface effects. -- Highlights: ► The advanced STEM/HAADF diffraction contrast is extended to 3D stereo-imaging. ► The advantages of the new technique over stereo-imaging in CTEM are demonstrated. ► The new method allows foil thickness measurements in a broad range of conditions. ► We show that features associated with ion milling surface damage can be beneficial for appreciating 3D features of the microstructure.

Advanced scanning transmission stereo electron microscopy of structural and functional engineering materials

Energy Technology Data Exchange (ETDEWEB)

Agudo Jacome, L., E-mail: leonardo.agudo@bam.de [Institut fuer Werkstoffe, Ruhr-Universitaet Bochum, D-44780 Bochum (Germany); Eggeler, G., E-mail: gunther.eggeler@ruhr-uni-bochum.de [Institut fuer Werkstoffe, Ruhr-Universitaet Bochum, D-44780 Bochum (Germany); Dlouhy, A., E-mail: dlouhy@ipm.cz [Institute of Physics of Materials, Academy of Sciences of the Czech Republic, Zizkova 22, 616 62 Brno (Czech Republic)

2012-11-15

Stereo transmission electron microscopy (TEM) provides a 3D impression of the microstructure in a thin TEM foil. It allows to perform depth and TEM foil thickness measurements and to decide whether a microstructural feature lies inside of a thin foil or on its surface. It allows appreciating the true three-dimensional nature of dislocation configurations. In the present study we first review some basic elements of classical stereo TEM. We then show how the method can be extended by working in the scanning transmission electron microscope (STEM) mode of a modern analytical 200 kV TEM equipped with a field emission gun (FEG TEM) and a high angle annular dark field (HAADF) detector. We combine two micrographs of a stereo pair into one anaglyph. When viewed with special colored glasses the anaglyph provides a direct and realistic 3D impression of the microstructure. Three examples are provided which demonstrate the potential of this extended stereo TEM technique: a single crystal Ni-base superalloy, a 9% Chromium tempered martensite ferritic steel and a NiTi shape memory alloy. We consider the effect of camera length, show how foil thicknesses can be measured, and discuss the depth of focus and surface effects. -- Highlights: Black-Right-Pointing-Pointer The advanced STEM/HAADF diffraction contrast is extended to 3D stereo-imaging. Black-Right-Pointing-Pointer The advantages of the new technique over stereo-imaging in CTEM are demonstrated. Black-Right-Pointing-Pointer The new method allows foil thickness measurements in a broad range of conditions. Black-Right-Pointing-Pointer We show that features associated with ion milling surface damage can be beneficial for appreciating 3D features of the microstructure.

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.

Detailed characterisation of focused ion beam induced lateral damage on silicon carbide samples by electrical scanning probe microscopy and transmission electron microscopy

Science.gov (United States)

Stumpf, F.; Abu Quba, A. A.; Singer, P.; Rumler, M.; Cherkashin, N.; Schamm-Chardon, S.; Cours, R.; Rommel, M.

2018-03-01

The lateral damage induced by focused ion beam on silicon carbide was characterized using electrical scanning probe microscopy (SPM), namely, scanning spreading resistance microscopy and conductive atomic force microscopy (c-AFM). It is shown that the damage exceeds the purposely irradiated circles with a radius of 0.5 μm by several micrometres, up to 8 μm for the maximum applied ion dose of 1018 cm-2. Obtained SPM results are critically compared with earlier findings on silicon. For doses above the amorphization threshold, in both cases, three different areas can be distinguished. The purposely irradiated area exhibits resistances smaller than the non-affected substrate. A second region with strongly increasing resistance and a maximum saturation value surrounds it. The third region shows the transition from maximum resistance to the base resistance of the unaffected substrate. It correlates to the transition from amorphized to defect-rich to pristine crystalline substrate. Additionally, conventional transmission electron microscopy (TEM) and annular dark-field STEM were used to complement and explain the SPM results and get a further understanding of the defect spreading underneath the surface. Those measurements also show three different regions that correlate well with the regions observed from electrical SPM. TEM results further allow to explain observed differences in the electrical results for silicon and silicon carbide which are most prominent for ion doses above 3 × 1016 cm-2. Furthermore, the conventional approach to perform current-voltage measurements by c-AFM was critically reviewed and several improvements for measurement and analysis process were suggested that result in more reliable and impactful c-AFM data.

Fabrication of thin TEM sample of ionic liquid for high-resolution ELNES measurements

Energy Technology Data Exchange (ETDEWEB)

Miyata, Tomohiro, E-mail: tomo-m@iis.u-tokyo.ac.jp; Mizoguchi, Teruyasu, E-mail: teru@iis.u-tokyo.ac.jp

2017-07-15

Investigation of the local structure, ionic and molecular behavior, and chemical reactions at high spatial resolutions in liquids has become increasingly important. Improvements in these areas help to develop efficient batteries and improve organic syntheses. Transmission electron microscopy (TEM) and scanning-TEM (STEM) have excellent spatial resolution, and the electron energy-loss near edge structure (ELNES) measured by the accompanied electron energy-loss spectroscopy (EELS) is effective to analyze the liquid local structure owing to reflecting the electronic density of states. In this study, we fabricate a liquid-layer-only sample with thickness of single to tens nanometers using an ionic liquid. Because the liquid film has a thickness much less than the inelastic mean free path (IMFP) of the electron beam, the fine structure of the C-K edge electron energy loss near edge structure (ELNES) can be measured with sufficient resolution to allow meaningful analysis. The ELNES spectrum from the thin liquid film has been interpreted using first principles ELNES calculations. - Highlights: • A fabrication method of thin liquid film samples for STEM-EELS observations is proposed. • The thickness of the fabricated thin liquid film is about 10 nm. • An ELNES is measured from the thin liquid with a high energy resolution. • The peaks of the ELNES are interpreted using first principles calculations.

Lights Will Guide You : Sample Preparation and Applications for Integrated Laser and Electron Microscopy

Science.gov (United States)

Karreman, M. A.

2013-03-01

Correlative microscopy is the combined use of two different forms of microscopy in the study of a specimen, allowing for the exploitation of the advantages of both imaging tools. The integrated Laser and Electron Microscope (iLEM), developed at Utrecht University, combines a fluorescence microscope (FM) and a transmission electron microscope (TEM) in a single set-up. The region of interest in the specimen is labeled or tagged with a fluorescent probe and can easily be identified within a large field of view with the FM. Next, this same area is retraced in the TEM and can be studied at high resolution. The iLEM demands samples that can be imaged with both FM and TEM. Biological specimen, typically composed of light elements, generate low image contrast in the TEM. Therefore, these samples are often ‘contrasted’ with heavy metal stains. FM, on the other hand, images fluorescent samples. Sample preparation for correlative microscopy, and iLEM in particular, is complicated by the fact that the heavy metals stains employed for TEM quench the fluorescent signal of the probe that is imaged with FM. The first part of this thesis outlines preparation procedures for biological material yielding specimen that can be imaged with the iLEM. Here, approaches for the contrasting of thin sections of cells and tissue are introduced that do not affect the fluorescence signal of the probe that marks the region of interest. Furthermore, two novel procedures, VIS2FIXH and VIS2FIX­FS are described that allow for the chemical fixation of thin sections of cryo-immobilized material. These procedures greatly expedite the sample preparation process, and open up novel possibilities for the immuno-labeling of difficult antigens, eg. proteins and lipids that are challenging to preserve. The second part of this thesis describes applications of iLEM in research in the field of life and material science. The iLEM was employed in the study of UVC induced apoptosis (programmed cell death) of

Thin dielectric film thickness determination by advanced transmission electron microscopy

Energy Technology Data Exchange (ETDEWEB)

Diebold, A.C.; Foran, B.; Kisielowski, C.; Muller, D.; Pennycook, S.; Principe, E.; Stemmer, S.

2003-09-01

High Resolution Transmission Electron Microscopy (HR-TEM) has been used as the ultimate method of thickness measurement for thin films. The appearance of phase contrast interference patterns in HR-TEM images has long been confused as the appearance of a crystal lattice by non-specialists. Relatively easy to interpret crystal lattice images are now directly observed with the introduction of annular dark field detectors for scanning TEM (STEM). With the recent development of reliable lattice image processing software that creates crystal structure images from phase contrast data, HR-TEM can also provide crystal lattice images. The resolution of both methods was steadily improved reaching now into the sub Angstrom region. Improvements in electron lens and image analysis software are increasing the spatial resolution of both methods. Optimum resolution for STEM requires that the probe beam be highly localized. In STEM, beam localization is enhanced by selection of the correct aperture. When STEM measurement is done using a highly localized probe beam, HR-TEM and STEM measurement of the thickness of silicon oxynitride films agree within experimental error. In this paper, the optimum conditions for HR-TEM and STEM measurement are discussed along with a method for repeatable film thickness determination. The impact of sample thickness is also discussed. The key result in this paper is the proposal of a reproducible method for film thickness determination.

35 years of electron microscopy in Costa Rica

International Nuclear Information System (INIS)

Hernandez Chavarria, Francisco

2011-01-01

Electron microscopy has celebrated in 2009 the XXXV anniversary in Costa Rica. The history of the electron microscopy was initiated with the donation of a microscope by Japan and the establishment of the Unidad de Microscopia Electronica (UME), which later, has been consolidated as the Centro de Investigacion en Estructuras Microscopicas (CIEMic) of the Universidad de Costa Rica (UCR). This center has realized its own research and has gave support to different units of the UCR, state universities and the private sector. Currently, the CIEMic has had two transmission electron microscopes (TEM) and two scanning electron microscopes (SEM), besides of optical microscopy equipment, including a laser confocal microscope. The two fundamental types of electron microscopes (TEM and SEM) have generated different images. While the first has had a resolution that has allowed to analyze virus, usually their images have been flat; however, with some special techniques can obtain three-dimensional images. The image in the TEM is generated by electrons that have passed through the sample, and to interact with its atoms have changed its energy and trajectory. This, at the end, has impacted on a photosensitive screen that has become in flashes, whose intensity has depended on its energy and form the image. Meanwhile, in the MER, the image has been normal type, although with less resolution. The electrons in the MER are focused on a small area of the sample in which have interacted with the atoms of this, and has generated a a series of signals, including the most used were the secondary electrons and characteristic X-rays. In both cases, an electron from beam has generated in the filament a collision against an electron of the sample and has given part of its energy to the degree of release of its atom and issued out of the sample; this has been called secondary electrons. X-rays have been generated when an electron of the same atom that has lost the secondary electron, but in an

Characterization of konjac glucomannan-ethyl cellulose film formation via microscopy.

Science.gov (United States)

Xiao, Man; Wan, Li; Corke, Harold; Yan, Wenli; Ni, Xuewen; Fang, Yapeng; Jiang, Fatang

2016-04-01

Konjac glucomannan-ethyl cellulose (KGM-EC, 7:3, w/w) blended film shows good mechanical and moisture resistance properties. To better understand the basis for the KGM-EC film formation, optical microscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and atomic force microscopy (AFM) were used to observe the formation of the film from emulsion. Optical microscopy images showed that EC oil droplets were homogeneously dispersed in KGM water phase without obviously coalescence throughout the entire drying process. SEM images showed the surface and cross-sectional structures of samples maintained continuous and homogeneous appearance from the emulsion to dried film. AFM images indicated that KGM molecules entangled EC molecules in the emulsion. Interactions between KGM and EC improved the stability of KGM-EC emulsion, and contributed to uniformed structures of film formation. Based on these output information, a schematic model was built to elucidate KGM-EC film-forming process. Copyright © 2015 Elsevier B.V. All rights reserved.

On the Progress of Scanning Transmission Electron Microscopy (STEM) Imaging in a Scanning Electron Microscope.

Science.gov (United States)

Sun, Cheng; Müller, Erich; Meffert, Matthias; Gerthsen, Dagmar

2018-04-01

Transmission electron microscopy (TEM) with low-energy electrons has been recognized as an important addition to the family of electron microscopies as it may avoid knock-on damage and increase the contrast of weakly scattering objects. Scanning electron microscopes (SEMs) are well suited for low-energy electron microscopy with maximum electron energies of 30 keV, but they are mainly used for topography imaging of bulk samples. Implementation of a scanning transmission electron microscopy (STEM) detector and a charge-coupled-device camera for the acquisition of on-axis transmission electron diffraction (TED) patterns, in combination with recent resolution improvements, make SEMs highly interesting for structure analysis of some electron-transparent specimens which are traditionally investigated by TEM. A new aspect is correlative SEM, STEM, and TED imaging from the same specimen region in a SEM which leads to a wealth of information. Simultaneous image acquisition gives information on surface topography, inner structure including crystal defects and qualitative material contrast. Lattice-fringe resolution is obtained in bright-field STEM imaging. The benefits of correlative SEM/STEM/TED imaging in a SEM are exemplified by structure analyses from representative sample classes such as nanoparticulates and bulk materials.

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

Characterization of virus-like particles by atomic force microscopy in ambient conditions

International Nuclear Information System (INIS)

Oropesa, Reinier; Ramos, Jorge R; Falcón, Viviana; Felipe, Ariel

2013-01-01

Recombinant virus-like particles (VLPs) are attractive candidates for vaccine design since they resemble native viroids in size and morphology, but they are non-infectious due to the absence of a viral genome. The visualization of surface morphologies and structures can be used to deepen the understanding of physical, chemical, and biological phenomena. Atomic force microscopy (AFM) is a useful tool for the visualization of soft biological samples in a nanoscale resolution. In this work we have investigated the morphology of recombinant surface antigens of hepatitis B (rHBsAg) VLPs from Cuban vaccine against hepatitis B. The rHBsAg VLPs sizes estimated by AFM between 15 and 30 nm are similar to those reported on previous transmission electron microscopy (TEM) studies. (paper)

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.

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

Integrated Transmission Electron and Single‐Molecule Fluorescence Microscopy Correlates Reactivity with Ultrastructure in a Single Catalyst Particle

OpenAIRE

Hendriks, Frank C.; Mohammadian, Sajjad; Ristanović, Zoran; Kalirai, Sam; Meirer, Florian; Vogt, Eelco T. C.; Bruijnincx, Pieter C. A.; Gerritsen, Hans C.; Weckhuysen, Bert M.

2017-01-01

Abstract Establishing structure–activity relationships in complex, hierarchically structured nanomaterials, such as fluid catalytic cracking (FCC) catalysts, requires characterization with complementary, correlated analysis techniques. An integrated setup has been developed to perform transmission electron microscopy (TEM) and single‐molecule fluorescence (SMF) microscopy on such nanostructured samples. Correlated structure–reactivity information was obtained for 100 nm thin, microtomed secti...

Networking strategies of the microscopy community for improved utilization of advanced instruments: (1) The Australian Microscopy and Microanalysis Research Facility (AMMRF)

International Nuclear Information System (INIS)

Ringer, S.P.; Apperley, M.H.

2014-01-01

This paper describes the strategy underpinning the formation and operation of the Australian Microscopy and Microanalysis Research Facility (AMMRF). AMMRF is a formal collaboration that links eight Australian Universities together to create a user-focused national capability in microscopy and microanalysis. The AMMRF flagship capabilities include: Cameca IMS-1280 and NanoSIMS-50 ion microprobes (University of Western Australia); High-throughput, high-resolution cryoTEM (University of Queensland); Atom Probe Microscopy (University of Sydney); High-resolution Focussed Ion-Beam and SEM (Universities of Adelaide and NSW); High-resolution SEM microanalysis facility (University of New South Wales); and PHI TRIFT V nanoToF ToF-SIMS (University of South Australia). Secondly, a network of peer support and expert training has been established amongst facility professional support staff. The governance and funding of the organisation are described and the advantages and achievements of a nationally coordinated facility for microscopy and microanalysis are set out. Selected data are presented that benchmark the performance of the facility, describe the economic impact and demonstrate the impact on the quality of research outcomes as a result of operating national collaborative research infrastructure for microscopy and microanalysis

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...

TEM characterization of Al-C-Cu-Al2O3 composites produced by mechanical milling

International Nuclear Information System (INIS)

Santos-Beltran, A.; Gallegos-Orozco, V.; Estrada-Guel, I.; Bejar-Gomez, L.; Espinosa-Magana, F.; Miki-Yoshida, M.; Martinez-Sanchez, R.

2007-01-01

Novel Al-based composites (Al-C-Cu-Al 2 O 3 ) obtained by mechanical milling (MM), were characterized by transmission electron microscopy (TEM) and electron energy loss spectroscopy (EELS). Analyses of composites were carried out in both, the as-milled and the as-sintered conditions. C nanoparticles were found in the as-milled condition and Al 2 O 3 nanofibers were found in as-sintered products, as determined by EELS. C and Cu react with Al to crystallize in Al 3 C 4 and Al 2 Cu structures, respectively

Effect of interparticle interactions on size determination of zirconia and silica based systems – A comparison of SAXS, DLS, BET, XRD and TEM

Science.gov (United States)

Pabisch, Silvia; Feichtenschlager, Bernhard; Kickelbick, Guido; Peterlik, Herwig

2012-01-01

The aim of this work is a systematic comparison of size characterisation methods for two completely different model systems of oxide nanoparticles, i.e. amorphous spherical silica and anisotropic facet-shaped crystalline zirconia. Size and/or size distribution were determined in a wide range from 5 to 70 nm using small-angle X-ray scattering (SAXS), dynamic light scattering (DLS), nitrogen sorption (BET), X-ray diffraction (XRD) and transmission electron microscopy (TEM). A nearly perfect coincidence was observed only for SAXS and TEM for both types of particles. For zirconia nanoparticles considerable differences between different measurement methods were observed. PMID:22347721

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.

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.

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.

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

OSCE vs. TEM: Different approaches to assess clinical skills of nursing students

Directory of Open Access Journals (Sweden)

Prasuna Jelly

2017-01-01

Full Text Available Introduction: Nurses are trained with specific clinical skills, and objective structured clinical examination (OSCE could be a better approach to assess clinical skills of nursing students. Materials and Methods: A comparative study was conducted by observational checklist regarding antenatal care and opinionnaire on the usefulness of OSCE and tradition evaluation method (TEM was used to assess the clinical skills and to get opinion. Results: The mean score of OSCE was more than TEM and the difference was statistically significant (P < 0.001. The opinion of students regarding the usefulness of OSCE was higher than TEM. Conclusions: The study concluded that implementing OSCE will overweigh the advantages of the TEM.

Transmission Electron Microscopy and Diffractometry of Materials

CERN Document Server

Fultz, Brent

2013-01-01

This book explains concepts of transmission electron microscopy (TEM) and x-ray diffractometry (XRD) that are important for the characterization of materials. The fourth edition adds important new techniques of TEM such as electron tomography, nanobeam diffraction, and geometric phase analysis. A new chapter on neutron scattering completes the trio of x-ray, electron and neutron diffraction. All chapters were updated and revised for clarity. The book explains the fundamentals of how waves and wavefunctions interact with atoms in solids, and the similarities and differences of using x-rays, electrons, or neutrons for diffraction measurements. Diffraction effects of crystalline order, defects, and disorder in materials are explained in detail. Both practical and theoretical issues are covered. The book can be used in an introductory-level or advanced-level course, since sections are identified by difficulty. Each chapter includes a set of problems to illustrate principles, and the extensive Appendix includes la...

TEM analysis of fine sulphides dissolution and precipitation in steel

International Nuclear Information System (INIS)

Garbarz, B.; Marcisz, J.; Wojtas, J.

2003-01-01

Results of transmission electron microscopy (TEM) investigation of morphology, size distribution and chemistry of nano-inclusions formed in 4 mm thick laboratory steel ingots in as-cast condition and after heat treatment are reported. The investigated steel contained 0.11-0.14 C, 0.6 Mn, 0.25 Si, 0.22 Cu, 0.025-0.037 S (wt.%), and 80-115 ppm O and solidified at an average cooling rate of 250 K s -1 . In the as-cast specimens most nano-inclusions had a diameter in the range 10-100 nm with an average size of 30 nm. They were identified by microanalysis in thin foils as sulphides: MnS, (Mn,Cu)S, CuS and Cu 2 S. After a solution treatment of the thin ingots the re-precipitation of nano-sulphides was investigated

Analytical electron microscopy of neutron-irradiated reactor alloys

International Nuclear Information System (INIS)

Thomas, L.E.

1982-01-01

Exposure to the high neutron fluxes and temperatures from 400 to 650 0 C in the core region of a fast breeder reactor profoundly alters the microstructure and properties of structural steels and superalloys. The development of irradiation-induced voids, dislocations and precipitates, as well as segregation of alloying elements on a microscopic scale has been related to macroscopic swelling, creep, hardening and embrittlement which occur during prolonged exposures in reactor. Microanalytical studies using TEM/STEM methods, primarily energy dispersive x-ray (EDX) microanalysis, have greatly aided understanding of alloy behavior under irradiation. The main uses of analytical electron microscopy in studying irradiated alloys have been the identification of irradiation-induced precipitates and determination of the changes in local composition due to irradiation-induced solute segregation

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.)

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.)

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.

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.

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

Integrated Transmission Electron and Single-Molecule Fluorescence Microscopy Correlates Reactivity with Ultrastructure in a Single Catalyst Particle

OpenAIRE

Hendriks, Frank C.; Mohammadian, Sajjad; Ristanovic, Zoran; Kalirai, Samanbir; Meirer, Florian; Vogt, Eelco T. C.; Bruijnincx, Pieter C. A.; Gerritsen, Hans; Weckhuysen, Bert M.

2018-01-01

Establishing structure–activity relationships in complex, hierarchically structured nanomaterials, such as fluid catalytic cracking (FCC) catalysts, requires characterization with complementary, correlated analysis techniques. An integrated setup has been developed to perform transmission electron microscopy (TEM) and single-molecule fluorescence (SMF) microscopy on such nanostructured samples. Correlated structure–reactivity information was obtained for 100 nm thin, microtomed sections of a ...

Mechanical Conversion for High-Throughput TEM Sample Preparation

International Nuclear Information System (INIS)

Kendrick, Anthony B; Moore, Thomas M; Zaykova-Feldman, Lyudmila

2006-01-01

This paper presents a novel method of direct mechanical conversion from lift-out sample to TEM sample holder. The lift-out sample is prepared in the FIB using the in-situ liftout Total Release TM method. The mechanical conversion is conducted using a mechanical press and one of a variety of TEM coupons, including coupons for both top-side and back-side thinning. The press joins a probe tip point with attached TEM sample to the sample coupon and separates the complete assembly as a 3mm diameter TEM grid, compatible with commercially available TEM sample holder rods. This mechanical conversion process lends itself well to the high through-put requirements of in-line process control and to materials characterization labs where instrument utilization and sample security are critically important

Chemical Reactions of Molecules Promoted and Simultaneously Imaged by the Electron Beam in Transmission Electron Microscopy.

Science.gov (United States)

Skowron, Stephen T; Chamberlain, Thomas W; Biskupek, Johannes; Kaiser, Ute; Besley, Elena; Khlobystov, Andrei N

2017-08-15

The main objective of this Account is to assess the challenges of transmission electron microscopy (TEM) of molecules, based on over 15 years of our work in this field, and to outline the opportunities in studying chemical reactions under the electron beam (e-beam). During TEM imaging of an individual molecule adsorbed on an atomically thin substrate, such as graphene or a carbon nanotube, the e-beam transfers kinetic energy to atoms of the molecule, displacing them from equilibrium positions. Impact of the e-beam triggers bond dissociation and various chemical reactions which can be imaged concurrently with their activation by the e-beam and can be presented as stop-frame movies. This experimental approach, which we term ChemTEM, harnesses energy transferred from the e-beam to the molecule via direct interactions with the atomic nuclei, enabling accurate predictions of bond dissociation events and control of the type and rate of chemical reactions. Elemental composition and structure of the reactant molecules as well as the operating conditions of TEM (particularly the energy of the e-beam) determine the product formed in ChemTEM processes, while the e-beam dose rate controls the reaction rate. Because the e-beam of TEM acts simultaneously as a source of energy for the reaction and as an imaging tool monitoring the same reaction, ChemTEM reveals atomic-level chemical information, such as pathways of reactions imaged for individual molecules, step-by-step and in real time; structures of illusive reaction intermediates; and direct comparison of catalytic activity of different transition metals filmed with atomic resolution. Chemical transformations in ChemTEM often lead to previously unforeseen products, demonstrating the potential of this method to become not only an analytical tool for studying reactions, but also a powerful instrument for discovery of materials that can be synthesized on preparative scale.

Transmission electron microscopy study for investigating high-temperature reliability of Ti10W90-based and Ta-based diffusion barriers up to 600 C

International Nuclear Information System (INIS)

Budhiman, Nando; Schuermann, Ulrich; Kienle, Lorenz; Jensen, Bjoern; Chemnitz, Steffen; Wagner, Bernhard

2016-01-01

Abstractauthoren Transmission electron microscopy (TEM) analysis, including energy dispersive X-ray (EDX) (elemental mapping, line, and point measurements) and energy filtered TEM (EFTEM) methods, is applied to investigate the high temperature reliability, especially material diffusion, of two types of diffusion barriers: titanium-tungsten-based (Ti 10 W 90 -based) and tantalum-based (Ta-based), with nickel (Ni) layer on top. Both barriers were deposited as a form of stacked layers on sili-con (Si) wafers using the physical vapor deposition (PVD) technique. TEM analysis is performed on both barriers before and after annealing (at 600 C for 24 h inside a vacuum chamber). No diffusion of material into the Si substrate as observed. Additionally, only diffusion between the Ni and adjoining Ti 10 W 90 layers, and between Ni and adjoining Ta layers in the Ti 10 W 90 -based and Ta-based barriers, respectively, are observed due to annealing. (copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

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.

In-situ observation of recrystallization in an AlMgScZr alloy using confocal laser scanning microscopy

International Nuclear Information System (INIS)

Taendl, J.; Nambu, S.; Orthacker, A.; Kothleitner, G.; Inoue, J.; Koseki, T.; Poletti, C.

2015-01-01

In this work we present a novel in-situ approach to study the recrystallization behavior of age hardening alloys. We use confocal laser scanning microscopy (CLSM) at 400 °C to investigate the static recrystallization of an AlMg4Sc0.4Zr0.12 alloy in-situ. The results are combined with electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) analyses. It was found that CLSM is a powerful tool to visualize both the local initiation and temporal sequence of recrystallization. After fast nucleation and initial growth, the grain growth rate decreases and the grain boundary migration stops after some minutes due to Zener pinning from Al 3 (Sc,Zr) precipitates produced during the heat treatment. EBSD and TEM analyses confirm both the boundary movements and the particle-boundary interactions. - Highlights: • First time that CLSM is used to study recrystallization in-situ. • The start and end of recrystallization can be directly observed. • The procedure is easy to apply and requires only simple data interpretation. • In-situ observations on the surface correlate to modifications inside the bulk. • In-situ observations correlate to EBSD and EFTEM analyses.

In-situ observation of recrystallization in an AlMgScZr alloy using confocal laser scanning microscopy

Energy Technology Data Exchange (ETDEWEB)

Taendl, J., E-mail: johannes.taendl@tugraz.atl [Institute of Materials Science and Welding, Graz University of Technology, Graz (Austria); Nambu, S. [Department of Materials Engineering, The University of Tokyo, Tokyo 113-8656 (Japan); Orthacker, A.; Kothleitner, G. [Institute of Electron Microscopy and Nanoanalysis, Graz University of Technology, Graz (Austria); Graz Center for Electron Microscopy, Graz (Austria); Inoue, J.; Koseki, T. [Department of Materials Engineering, The University of Tokyo, Tokyo 113-8656 (Japan); Poletti, C. [Institute of Materials Science and Welding, Graz University of Technology, Graz (Austria)

2015-10-15

In this work we present a novel in-situ approach to study the recrystallization behavior of age hardening alloys. We use confocal laser scanning microscopy (CLSM) at 400 °C to investigate the static recrystallization of an AlMg4Sc0.4Zr0.12 alloy in-situ. The results are combined with electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) analyses. It was found that CLSM is a powerful tool to visualize both the local initiation and temporal sequence of recrystallization. After fast nucleation and initial growth, the grain growth rate decreases and the grain boundary migration stops after some minutes due to Zener pinning from Al{sub 3}(Sc,Zr) precipitates produced during the heat treatment. EBSD and TEM analyses confirm both the boundary movements and the particle-boundary interactions. - Highlights: • First time that CLSM is used to study recrystallization in-situ. • The start and end of recrystallization can be directly observed. • The procedure is easy to apply and requires only simple data interpretation. • In-situ observations on the surface correlate to modifications inside the bulk. • In-situ observations correlate to EBSD and EFTEM analyses.

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)

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.

Polarized Light Microscopy

Science.gov (United States)

Frandsen, Athela F.

2016-01-01

Polarized light microscopy (PLM) is a technique which employs the use of polarizing filters to obtain substantial optical property information about the material which is being observed. This information can be combined with other microscopy techniques to confirm or elucidate the identity of an unknown material, determine whether a particular contaminant is present (as with asbestos analysis), or to provide important information that can be used to refine a manufacturing or chemical process. PLM was the major microscopy technique in use for identification of materials for nearly a century since its introduction in 1834 by William Fox Talbot, as other techniques such as SEM (Scanning Electron Microscopy), FTIR (Fourier Transform Infrared spectroscopy), XPD (X-ray Powder Diffraction), and TEM (Transmission Electron Microscopy) had not yet been developed. Today, it is still the only technique approved by the Environmental Protection Agency (EPA) for asbestos analysis, and is often the technique first applied for identification of unknown materials. PLM uses different configurations in order to determine different material properties. With each configuration additional clues can be gathered, leading to a conclusion of material identity. With no polarizing filter, the microscope can be used just as a stereo optical microscope, and view qualities such as morphology, size, and number of phases. With a single polarizing filter (single polars), additional properties can be established, such as pleochroism, individual refractive indices, and dispersion staining. With two polarizing filters (crossed polars), even more can be deduced: isotropy vs. anisotropy, extinction angle, birefringence/degree of birefringence, sign of elongation, and anomalous polarization colors, among others. With the use of PLM many of these properties can be determined in a matter of seconds, even for those who are not highly trained. McCrone, a leader in the field of polarized light microscopy, often

TEM-145 and TEM-146 β-lactamases produced by Escherichia coli ...

African Journals Online (AJOL)

GREGO

2007-03-05

Mar 5, 2007 ... Key words: Escherichia coli, plasmid-mediated, TEM β-lactamase. ... Enterobacteriaceae, the most prevalent mechanism of resistance to ... the production of a relatively inhibitor-resistant OXA-type β-lactamase .... and 8.6 as transcripts of the E. coli chromosomal AmpC .... Mode of action and mechanisms of.

TEM Microstructure and Chemical Composition of Transition Zone Between Steel Tube and An Inconel 625 Weld Overlay Coating Produced by CMT Method

Directory of Open Access Journals (Sweden)

Rozmus-Górnikowska M.

2017-06-01

Full Text Available The aim of this work was to investigate the microstructure and chemical composition of the transition zone between 16Mo3 steel and Inconel 625 weld overlay coating produced by the Cold Metal Transfer (CMT method. Investigations were primarily carried out through transmission electron microscopy (TEM on thin foils prepared by FIB (Focus Ion Beam.

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.

A convenient method for X-ray analysis in TEM that measures mass thickness and composition

Science.gov (United States)

Statham, P.; Sagar, J.; Holland, J.; Pinard, P.; Lozano-Perez, S.

2018-01-01

We consider a new approach for quantitative analysis in transmission electron microscopy (TEM) that offers the same convenience as single-standard quantitative analysis in scanning electron microscopy (SEM). Instead of a bulk standard, a thin film with known mass thickness is used as a reference. The procedure involves recording an X-ray spectrum from the reference film for each session of acquisitions on real specimens. There is no need to measure the beam current; the current only needs to be stable for the duration of the session. A new reference standard with a large (1 mm x 1 mm) area of uniform thickness of 100 nm silicon nitride is used to reveal regions of X-ray detector occlusion that would give misleading results for any X-ray method that measures thickness. Unlike previous methods, the new X-ray method does not require an accurate beam current monitor but delivers equivalent accuracy in mass thickness measurement. Quantitative compositional results are also automatically corrected for specimen self-absorption. The new method is tested using a wedge specimen of Inconel 600 that is used to calibrate the high angle angular dark field (HAADF) signal to provide a thickness reference and results are compared with electron energy-loss spectrometry (EELS) measurements. For the new X-ray method, element composition results are consistent with the expected composition for the alloy and the mass thickness measurement is shown to provide an accurate alternative to EELS for thickness determination in TEM without the uncertainty associated with mean free path estimates.

A short note on how to convert a conventional analytical TEM into an analytical Low Voltage TEM

International Nuclear Information System (INIS)

Stöger-Pollach, M.

2014-01-01

The present work is a short note on the performance of a conventional transmission electron microscope (TEM) being operated at very low beam energies (below 20 keV). We discuss the high tension stability and resolving power of this uncorrected TEM. We find out that the theoretical lens performance can nearly be achieved in practice. We also demonstrate that electron energy loss spectra can be recorded at these low beam energies with standard equipment. The signal-to-noise ratio is sufficiently good for further data treatment like multiple scattering deconvolution and Kramers–Kronig analysis. - Highlights: • TEM operation at very low beam energies (below 20 keV). • Testing of hardware performance at low beam energies. • EELS spectra recorded with 10 keV electrons

Electron microscopy of the amphibian model systems Xenopus laevis and Ambystoma mexicanum.

Science.gov (United States)

Kurth, Thomas; Berger, Jürgen; Wilsch-Bräuninger, Michaela; Kretschmar, Susanne; Cerny, Robert; Schwarz, Heinz; Löfberg, Jan; Piendl, Thomas; Epperlein, Hans H

2010-01-01

In this chapter we provide a set of different protocols for the ultrastructural analysis of amphibian (Xenopus, axolotl) tissues, mostly of embryonic origin. For Xenopus these methods include: (1) embedding gastrulae and tailbud embryos into Spurr's resin for TEM, (2) post-embedding labeling of methacrylate (K4M) and cryosections through adult and embryonic epithelia for correlative LM and TEM, and (3) pre-embedding labeling of embryonic tissues with silver-enhanced nanogold. For the axolotl (Ambystoma mexicanum) we present the following methods: (1) SEM of migrating neural crest (NC) cells; (2) SEM and TEM of extracellular matrix (ECM) material; (3) Cryo-SEM of extracellular matrix (ECM) material after cryoimmobilization; and (4) TEM analysis of hyaluronan using high-pressure freezing and HABP labeling. These methods provide exemplary approaches for a variety of questions in the field of amphibian development and regeneration, and focus on cell biological issues that can only be answered with fine structural imaging methods, such as electron microscopy. Copyright © 2010 Elsevier Inc. All rights reserved.

HUMAN CAPSULE EPITHELIAL-CELL DEGENERATION A LM, SEM AND TEM INVESTIGATION

NARCIS (Netherlands)

JONGEBLOED, WL; KALICHARAN, D; WORST, JGF

1993-01-01

The degeneration of the capsule epithelium of cataractous lenses has been studied with LM, SEM on TEM with emphases on TEM. The observed degeneration of the epithelial cells can be described as follows: The cell nucleus becomes picnotic and desintegrates as result of change of the chromatin.

Anisotropic Shape Changes of Silica Nanoparticles Induced in Liquid with Scanning Transmission Electron Microscopy

NARCIS (Netherlands)

Zecevic, J.; Hermannsdorfer, Justus; Schuh, Tobias; de Jong, Krijn P.; de Jonge, Niels

2017-01-01

Liquid-phase transmission electron microscopy (TEM) is used for in-situ imaging of nanoscale processes taking place in liquid, such as the evolution of nanoparticles during synthesis or structural changes of nanomaterials in liquid environment. Here, it is shown that the focused electron beam of

Experimental evaluation of the ‘transport-of-intensity’ equation for magnetic phase reconstruction in Lorentz transmission electron microscopy

Energy Technology Data Exchange (ETDEWEB)

Kohn, Amit, E-mail: akohn@post.tau.ac.il [Department of Materials Science and Engineering, Faculty of Engineering, Tel Aviv University, 69978 Tel Aviv (Israel); Habibi, Avihay; Mayo, Martin [Department of Materials Engineering, Ben-Gurion University of the Negev, 84105 Beer Sheva (Israel)

2016-01-15

The ‘transport-of-intensity’ equation (TIE) is a general phase reconstruction methodology that can be applied to Lorentz transmission electron microscopy (TEM) through the use of Fresnel-contrast (defocused) images. We present an experimental study to test the application of the TIE for quantitative magnetic mapping in Lorentz TEM without aberration correction by examining sub-micrometer sized Ni{sub 80}Fe{sub 20} (Permalloy) elements. For a JEOL JEM 2100F adapted for Lorentz microscopy, we find that quantitative magnetic phase reconstructions are possible for defoci distances ranging between approximately 200 μm and 800 μm. The lower limit originates from competing sources of image intensity variations in Fresnel-contrast images, namely structural defects and diffraction contrast. The upper defocus limit is due to a numerical error in the estimation of the intensity derivative based on three images. For magnetic domains, we show quantitative reconstructions of the product of the magnetic induction vector and thickness in element sizes down to approximately 100 nm in lateral size and 5 nm thick resulting in a minimal detection of 5 T nm. Three types of magnetic structures are tested in terms of phase reconstruction: vortex cores, domain walls, and element edges. We quantify vortex core structures at a diameter of 12 nm while the structures of domain walls and element edges are characterized qualitatively. Finally, we show by image simulations that the conclusions of this experimental study are relevant to other Lorentz TEM in which spherical aberration and defocus are dominant aberrations. - Highlights: • Testing TIE for quantitative magnetic phase reconstruction in Lorentz TEM. • Quantitative magnetic phase reconstructions for defoci distances in 200–800 μm range. • Minimal detection of the product of the magnetic induction and thickness is 5 T nm. • Quantitative phase reconstruction for vortex core structures at 12 nm diameter. • Observations

Chromatic Aberration Correction for Atomic Resolution TEM Imaging from 20 to 80 kV.

Science.gov (United States)

Linck, Martin; Hartel, Peter; Uhlemann, Stephan; Kahl, Frank; Müller, Heiko; Zach, Joachim; Haider, Max; Niestadt, Marcel; Bischoff, Maarten; Biskupek, Johannes; Lee, Zhongbo; Lehnert, Tibor; Börrnert, Felix; Rose, Harald; Kaiser, Ute

2016-08-12

Atomic resolution in transmission electron microscopy of thin and light-atom materials requires a rigorous reduction of the beam energy to reduce knockon damage. However, at the same time, the chromatic aberration deteriorates the resolution of the TEM image dramatically. Within the framework of the SALVE project, we introduce a newly developed C_{c}/C_{s} corrector that is capable of correcting both the chromatic and the spherical aberration in the range of accelerating voltages from 20 to 80 kV. The corrector allows correcting axial aberrations up to fifth order as well as the dominating off-axial aberrations. Over the entire voltage range, optimum phase-contrast imaging conditions for weak signals from light atoms can be adjusted for an optical aperture of at least 55 mrad. The information transfer within this aperture is no longer limited by chromatic aberrations. We demonstrate the performance of the microscope using the examples of 30 kV phase-contrast TEM images of graphene and molybdenum disulfide, showing unprecedented contrast and resolution that matches image calculations.

ERDA, RBS, TEM and SEM characterization of microstructural evolution in helium-implanted Hastelloy N alloy

Energy Technology Data Exchange (ETDEWEB)

Gao, Jie [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); School of Physical Sciences, University of Chinese Academy of Sciences, Beijing 100049 (China); Bao, Liangman [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Huang, Hefei, E-mail: huanghefei@sinap.ac.cn [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Li, Yan, E-mail: liyan@sinap.ac.cn [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Lei, Qiantao [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Institute of Modern Physics, Fudan University, Shanghai 200433 (China); Deng, Qi [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); Liu, Zhe; Yang, Guo [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800 (China); School of Physical Sciences, University of Chinese Academy of Sciences, Beijing 100049 (China); Shi, Liqun [Institute of Modern Physics, Fudan University, Shanghai 200433 (China)

2017-05-15

Hastelloy N alloy was implanted with 30 keV, 5 × 10{sup 16} ions/cm{sup 2} helium ions at room temperature, and subsequent annealed at 600 °C for 1 h and further annealed at 850 °C for 5 h in vacuum. Using elastic recoil detection analysis (ERDA) and transmission electron microscopy (TEM), the depth profiles of helium concentration and helium bubbles in helium-implanted Hastelloy N alloy were investigated, respectively. The diffusion of helium and molybdenum elements to surface occurred during the vacuum annealing at 850 °C (5 h). It was also observed that bubbles in molybdenum-enriched region were much larger in size than those in deeper region. In addition, it is worth noting that plenty of nano-holes can be observed on the surface of helium-implanted sample after high temperature annealing by scanning electron microscope (SEM). This observation provides the evidence for the occurrence of helium release, which can be also inferred from the results of ERDA and TEM analysis.

Correlating TEM images of damage in irradiated materials to molecular dynamics simulations

International Nuclear Information System (INIS)

Schaeublin, R.; Caturla, M.-J.; Wall, M.; Felter, T.; Fluss, M.; Wirth, B.D.; Diaz de la Rubia, T.; Victoria, M.

2002-01-01

TEM image simulations are used to couple the results from molecular dynamics (MD) simulations to experimental TEM images. In particular we apply this methodology to the study of defects produced during irradiation. MD simulations have shown that irradiation of FCC metals results in a population of vacancies and interstitials forming clusters. The limitation of these simulations is the short time scales available, on the order of 100 s of picoseconds. Extrapolation of the results from these short times to the time scales of the laboratory has been difficult. We address this problem by two methods: we perform TEM image simulations of MD simulations of cascades with an improved technique, to relate defects produced at short time scales with those observed experimentally at much longer time scales. On the other hand we perform in situ TEM experiments of Au irradiated at liquid-nitrogen temperatures, and study the evolution of the produced damage as the temperature is increased to room temperature. We find that some of the defects observed in the MD simulations at short time scales using the TEM image simulation technique have features that resemble those observed in laboratory TEM images of irradiated samples. In situ TEM shows that stacking fault tetrahedra are present at the lowest temperatures and are stable during annealing up to room temperature, while other defect clusters migrate one dimensionally above -100 deg. C. Results are presented here

Novel sample preparation for operando TEM of catalysts

International Nuclear Information System (INIS)

Miller, Benjamin K.; Barker, Trevor M.; Crozier, Peter A.

2015-01-01

A new TEM sample preparation method is developed to facilitate operando TEM of gas phase catalysis. A porous Pyrex-fiber pellet TEM sample was produced, allowing a comparatively large amount of catalyst to be loaded into a standard Gatan furnace-type tantalum heating holder. The increased amount of catalyst present inside the environmental TEM allows quantitative determination of the gas phase products of a catalytic reaction performed in-situ at elevated temperatures. The product gas concentration was monitored using both electron energy loss spectroscopy (EELS) and residual gas analysis (RGA). Imaging of catalyst particles dispersed over the pellet at atomic resolution is challenging, due to charging of the insulating glass fibers. To overcome this limitation, a metal grid is placed into the holder in addition to the pellet, allowing catalyst particles dispersed over the grid to be imaged, while particles in the pellet, which are assumed to experience identical conditions, contribute to the overall catalytic conversion inside the environmental TEM cell. The gas within the cell is determined to be well-mixed, making this assumption reasonable. - Highlights: • High in-situ conversion of CO to CO 2 achieved by a novel TEM sample preparation method. • A 3 mm fiber pellet increases the TEM sample surface area by 50×. • Operando atomic resolution is maintained by also including a 3 mm grid in the sample. • Evidence for a well-mixed gas composition inside the ETEM cell is given

Transmission electron microscopy and photoluminescence characterization of InGaAs strained quantum wires on GaAs vicinal (110) substrates

CERN Document Server

Shim, B R; Ota, T; Kobayashi, K; Maehashi, K; Nakashima, H; Lee, S Y

1999-01-01

We have used transmission electron microscopy (TEM) and photoluminescence (PL) to study InGaAs/AlGaAs strained quantum wires (QWRs) grown by molecular beam epitaxy (MBE) on GaAs vicinal (110) substrates. The cross-sectional TEM image reveals that InGaAs QWRs structures are naturally formed on AlGaAs giant steps. In the plan-view TEM images, the fringe pattern in the giant-step region is observed for In sub x Ga sub 1 sub - sub x As layers with x<= 0.4 We measured the separation of the fringe in the plan-view TEM images and compared the result with the calculated fringe separation. From this result, we conclude that the fringes observed in the plan-view TEM images are moire fringes. PL spectra of the InGaAs QWRs samples reveal 80-meV shifts to lower energy with respect to the spectrum of a quantum well (QWL) grown on a (001) substrate under the same conditions. We also measured the polarization anisotropy of the PL spectra from the QWRs. The PL peak shifts systematically toward higher energy with decreasing...

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.

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

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

SEM and TEM characterization of microstructure of stainless steel composites reinforced with TiB2

International Nuclear Information System (INIS)

Sulima, Iwona; Boczkal, Sonia; Jaworska, Lucyna

2016-01-01

Steel-8TiB 2 composites were produced by two new sintering techniques, i.e. Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT) sintering. This study discusses the impact of these sintering methods on the microstructure of steel composites reinforced with TiB 2 particles. Scanning electron microscopy (SEM), wavelength dispersive spectroscopy (WDS), X-ray diffraction, electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) were used to analyze the microstructure evolution in steel matrix composites. The results of microscopic examinations revealed a close relationship between the composite microstructure and the methods and conditions of sintering. Substantial differences were observed in the grain size of materials sintered by HP-HT and SPS. It has been demonstrated that the composites sintered by HP-HT tend to form a chromium-iron-nickel phase in the steel matrix. In contrast, the microstructure of the composites sintered by SPS is characterized by the presence of complex borides and chromium-iron phase. - Highlights: •The steel-8TiB 2 composites were fabricated by Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT). •Sintering techniques has an important effect on changes in the microstructure of steel-8TiB 2 composites. •New phases of different size and morphology were identified.

Analysis of microstructure in mouse femur and decalcification effect on microstructure by electron microscopy

Directory of Open Access Journals (Sweden)

Taehoon Jeon

2010-10-01

Full Text Available Microstructure and decalcification effect by ethylenediaminetetraacetic acid (EDTA on microstructure were studied for the compact bone of mouse femur by optical and electron microscopy. Especially the (002 reflection plane on the selected area electron diffraction (SAED of hydroxyapatite (HA was analyzed in detail. Two types of HA crystals were observed by transmission electron microscopy (TEM. One was needle-like crystals known as general HA crystals, and the other was flake-like crystals. Major constituents of two types of crystals were calcium, phosphorus, and oxygen. The Ca/P ratios of two types of crystals were close to the ideal value of HA within experimental error. Intensity data obtained from each crystals were also very similar. These results indicated that two types of crystals were actually same HA crystals. It was noticed that the (002 reflection plane on SAED displayed ring, spot, or arc patterns in accordance with orientations of HA crystals. Decalcification by EDTA process obsecured outline of osteons and havarsian canals, and changed morphology of the bone section. As the results of decalcification it was observed by TEM-EDS (Energy Dispersive Spectroscopy that all peaks of calcium and phosphorus disappeared, and intensity of oxygen peak was substantially reduced. Moreover, collagen appeared to be disaggreated.

HR-TEM and FT-Raman dataset of the caffeine interacted Phe–Phe peptide nanotube for possible sensing applications

OpenAIRE

Narayanan, A. Lakshmi; Dhamodaran, M.; Solomon, J. Samu; Karthikeyan, B.; Govindhan, R.

2017-01-01

Sensing ability of caffeine interaction with Phe-Phe annotates (PNTs), is presented (Govindhan et al., 2017; Karthikeyan et al., 2014; Tavagnacco et al., 2013; Kennedy et al., 2011; Wang et al., 2017) [1–5] in this data set. Investigation of synthesized caffeine carrying peptide nanotubes are carried out by FT-Raman spectral analysis and high resolution transmission electron microscopy (HR-TEM). Particle size of the caffeine loaded PNTs is < 40 nm. The FT-Raman spectrum signals are enhanced i...

TEM investigation of irradiated U-7 weight percent Mo dispersion fuel

International Nuclear Information System (INIS)

Van den Berghe, S.

2009-01-01

In the FUTURE experiment, fuel plates containing U-7 weight percent Mo atomized powder were irradiated in the BR2 reactor. At a burn-up of approximately 33 percent 235 U (6.5 percent FIMA or 1.41 10 21 fissions/cm 3 meat), the fuel plates showed an important deformation and the irradiation was stopped. The plates were submitted to detailed PIE at the Laboratory for High and Medium level Activity. The results of these examinations were reported in the scientific report of last year and published in open literature. Since then, the microstructural aspects of the FUTURE fuel were studied in more detail using transmission electron microscopy (TEM), in an attempt to understand the nature of the interaction phase and the fission gas behavior in the atomized U(Mo) fuel. The FUTURE experiment is regarded as the definitive proof that the classical atomized U(Mo) dispersion fuel is not stable under irradiation, at least in the conditions required for normal operation of plate-type fuel. The main cause for the instability was identified to be the irradiation behavior of the U(Mo)-Al interaction phase which is formed between the U(Mo) particles and the pure aluminum matrix during irradiation. It is assumed to become amorphous under irradiation and as such cannot retain the fission gas in stable bubbles. As a consequence, gas filled voids are generated between the interaction layer and the matrix, resulting in fuel plate pillowing and failure. The objective of the TEM investigation was the confirmation of this assumption of the amorphisation of the interaction phase. A deeper understanding of the actual nature of this layer and the fission gas behaviour in these fuels in general can allow a more oriented search for a solution to the fuel failures

In situ TEM visualization of superior nanomechanical flexibility of shear-exfoliated phosphorene.

Science.gov (United States)

Xu, Feng; Ma, Hongyu; Lei, Shuangying; Sun, Jun; Chen, Jing; Ge, Binghui; Zhu, Yimei; Sun, Litao

2016-07-14

Recently discovered atomically thin black phosphorus (called phosphorene) holds great promise for applications in flexible nanoelectronic devices. Experimentally identifying and characterizing nanomechanical properties of phosphorene are challenging, but also potentially rewarding. This work combines for the first time in situ transmission electron microscopy (TEM) imaging and an in situ micro-manipulation system to directly visualize the nanomechanical behaviour of individual phosphorene nanoflakes. We demonstrate that the phosphorene nanoflakes can be easily bent, scrolled, and stretched, showing remarkable mechanical flexibility rather than fracturing. An out-of-plane plate-like bending mechanism and in-plane tensile strain of up to 34% were observed. Moreover, a facile liquid-phase shear exfoliation route has been developed to produce such mono-layer and few-layer phosphorene nanoflakes in organic solvents using only a household kitchen blender. The effects of surface tensions of the applied solvents on the ratio of average length and thickness (L/T) of the nanoflakes were studied systematically. The results reported here will pave the way for potential industrial-scale applications of flexible phosphorene nanoelectronic devices.

Comparison between measured and predicted turbulence frequency spectra in ITG and TEM regimes

Science.gov (United States)

Citrin, J.; Arnichand, H.; Bernardo, J.; Bourdelle, C.; Garbet, X.; Jenko, F.; Hacquin, S.; Pueschel, M. J.; Sabot, R.

2017-06-01

The observation of distinct peaks in tokamak core reflectometry measurements—named quasi-coherent-modes (QCMs)—are identified as a signature of trapped-electron-mode (TEM) turbulence (Arnichand et al 2016 Plasma Phys. Control. Fusion 58 014037). This phenomenon is investigated with detailed linear and nonlinear gyrokinetic simulations using the Gene code. A Tore-Supra density scan is studied, which traverses through a linear (LOC) to saturated (SOC) ohmic confinement transition. The LOC and SOC phases are both simulated separately. In the LOC phase, where QCMs are observed, TEMs are robustly predicted unstable in linear studies. In the later SOC phase, where QCMs are no longer observed, ion-temperature-gradient (ITG) modes are identified. In nonlinear simulations, in the ITG (SOC) phase, a broadband spectrum is seen. In the TEM (LOC) phase, a clear emergence of a peak at the TEM frequencies is seen. This is due to reduced nonlinear frequency broadening of the underlying linear modes in the TEM regime compared with the ITG regime. A synthetic diagnostic of the nonlinearly simulated frequency spectra reproduces the features observed in the reflectometry measurements. These results support the identification of core QCMs as an experimental marker for TEM turbulence.

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

(CryoTransmission Electron Microscopy of Phospholipid Model Membranes Interacting with Amphiphilic and Polyphilic Molecules

Directory of Open Access Journals (Sweden)

Annette Meister

2017-10-01

Full Text Available Lipid membranes can incorporate amphiphilic or polyphilic molecules leading to specific functionalities and to adaptable properties of the lipid bilayer host. The insertion of guest molecules into membranes frequently induces changes in the shape of the lipid matrix that can be visualized by transmission electron microscopy (TEM techniques. Here, we review the use of stained and vitrified specimens in (cryoTEM to characterize the morphology of amphiphilic and polyphilic molecules upon insertion into phospholipid model membranes. Special emphasis is placed on the impact of novel synthetic amphiphilic and polyphilic bolalipids and polymers on membrane integrity and shape stability.

Characterization of TEM1/endosialin in human and murine brain tumors

International Nuclear Information System (INIS)

Carson-Walter, Eleanor B; Walter, Kevin A; Winans, Bethany N; Whiteman, Melissa C; Liu, Yang; Jarvela, Sally; Haapasalo, Hannu; Tyler, Betty M; Huso, David L; Johnson, Mahlon D

2009-01-01

TEM1/endosialin is an emerging microvascular marker of tumor angiogenesis. We characterized the expression pattern of TEM1/endosialin in astrocytic and metastatic brain tumors and investigated its role as a therapeutic target in human endothelial cells and mouse xenograft models. In situ hybridization (ISH), immunohistochemistry (IH) and immunofluorescence (IF) were used to localize TEM1/endosialin expression in grade II-IV astrocytomas and metastatic brain tumors on tissue microarrays. Changes in TEM1/endosialin expression in response to pro-angiogenic conditions were assessed in human endothelial cells grown in vitro. Intracranial U87MG glioblastoma (GBM) xenografts were analyzed in nude TEM1/endosialin knockout (KO) and wildtype (WT) mice. TEM1/endosialin was upregulated in primary and metastatic human brain tumors, where it localized primarily to the tumor vasculature and a subset of tumor stromal cells. Analysis of 275 arrayed grade II-IV astrocytomas demonstrated TEM1/endosialin expression in 79% of tumors. Robust TEM1/endosialin expression occurred in 31% of glioblastomas (grade IV astroctyomas). TEM1/endosialin expression was inversely correlated with patient age. TEM1/endosialin showed limited co-localization with CD31, αSMA and fibronectin in clinical specimens. In vitro, TEM1/endosialin was upregulated in human endothelial cells cultured in matrigel. Vascular Tem1/endosialin was induced in intracranial U87MG GBM xenografts grown in mice. Tem1/endosialin KO vs WT mice demonstrated equivalent survival and tumor growth when implanted with intracranial GBM xenografts, although Tem1/endosialin KO tumors were significantly more vascular than the WT counterparts. TEM1/endosialin was induced in the vasculature of high-grade brain tumors where its expression was inversely correlated with patient age. Although lack of TEM1/endosialin did not suppress growth of intracranial GBM xenografts, it did increase tumor vascularity. The cellular localization of TEM1

In-situ TEM observation of nano-void formation in UO2 under irradiation

Science.gov (United States)

Sabathier, C.; Martin, G.; Michel, A.; Carlot, G.; Maillard, S.; Bachelet, C.; Fortuna, F.; Kaitasov, O.; Oliviero, E.; Garcia, P.

2014-05-01

Transmission electron microscopy (TEM) observations of UO2 polycrystals irradiated in situ with 4 MeV Au ions were performed at room temperature (RT) to better understand the mechanisms of cavity and ultimately fission products nucleation in UO2. Experiments were carried out at the JANNuS Orsay facility that enables in situ ion irradiations inside the microscope to be carried out. The majority of 4 MeV gold ions were transmitted through the thin foil, and the induced radiation defects were investigated by TEM. Observations showed that nano-void formation occurs at ambient temperature in UO2 thin foils irradiated with energetic heavy ions under an essentially nuclear energy loss regime. The diameter and density of nano-objects were measured as a function of the gold irradiation dose at RT. A previous paper has also revealed a similar nano-object population after a Xe implantation performed at 390 keV at 870 K. The nano-object density was modelled using simple concepts derived from Classical Molecular Dynamics simulations. The results are in good agreement, which suggests a mechanism of heterogeneous nucleation induced by energetic cascade overlaps. This indicates that nano-void formation mechanism is controlled by radiation damage. Such nanovoids are likely to act as sinks for mobile fission products during reactor operation.

Characterization of TEM Moiré Patterns Originating from Two Monolayer Graphenes Grown on the Front and Back Sides of a Copper Substrate by CVD Method

Science.gov (United States)

Yamazaki, Kenji; Maehara, Yosuke; Gohara, Kazutoshi

2018-06-01

The number of layers affects the electronic properties of graphene owing to its unique band structure, called the Dirac corn. Raman spectroscopy is a key diagnostic tool for identifying the number of graphene layers and for determining their physical properties. Here, we observed moiré structures in transmission electron microscopy (TEM) observations; these are signature patterns in multilayer, although Raman spectra showed the typical intensity of the 2D/G peak in the monolayer. We also performed a multi-slice TEM image simulation to compare the 3D atomic structures of the two graphene membranes with experimental TEM images. We found that the experimental moiré image was constructed with a 9-12 Å interlayer distance between graphene membranes. This structure was constructed by transferring CVD-grown graphene films that formed on both sides of the Cu substrate at once.

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.

Studies on Chromium-free Conversion coatings on Aluminum | Oki ...

African Journals Online (AJOL)

The development of a chromium-free conversion coating on aluminum has been studied using transmission electron microscopy (TEM), Auger Electron (AES) and Secondary ion mass spectroscopy (SIMS) techniques. Within the limits of the resolution of the TEM, the coating is uniformly clear and featureless. It is composed ...

Advances in Transmission Electron Microscopy : In Situ Straining and In Situ Compression Experiments on Metallic Glasses

NARCIS (Netherlands)

De Hosson, Jeff Th. M.

In the field of transmission electron microscopy (TEM), fundamental and practical reasons still remain that hamper a straightforward correlation between microscopic structural information and deformation mechanisms in materials. In this article, it is argued that one should focus in particular on in

Development of a versatile TEM specimen holder for the characterization of photocatalytic materials

DEFF Research Database (Denmark)

Cavalca, Filippo; Langhammer, C.; Hansen, Thomas Willum

2011-01-01

conventional TEM analysis on photocatalysts with several in situ TEM techniques including environmental TEM (ETEM), in situ photo activation and localized surface plasmon resonance (LSPR) spectroscopy [3-4]. These experiments are facilitated by the construction of a specimen holder capable of illuminating....../on nanomaterials and thin films. We present results from combined ETEM-LSPR studies of thermally-induced catalytic phenomena and on metal nanoparticle sintering, an important process in catalysis, which we study in situ in both real and model systems by means of indirect nanoplasmonic sensing and ETEM....

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.

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.

TEM examination of microstructural evolution during processing of 14CrYWTi nanostructured ferritic alloys

International Nuclear Information System (INIS)

Kishimoto, H.; Alinger, M.J.; Odette, G.R.; Yamamoto, T.

2004-01-01

A transmission electron microscopy (TEM) study was carried out on the co-evolution of the coarser-scale microstructural features in mechanically alloyed (MA) powders and hot isostatic press (HIP) consolidated Fe-14Cr-3W-0 and 0.4Ti-0.25Y 2 O 3 nanostructured ferritic alloys (NFAs). The pancake shaped nanoscale grains in the as-MA powders are textured and elongated parallel to the particle surface. Powder annealing results in re-crystallization at 850 deg. C and grain growth at 1150 deg. C. The grains also recrystallize and may grow in the alloys HIPed at 850 deg. C, but appear to retain a polygonized sub-grain structure. The grains are larger and more distinct in the alloys HIPed at 1000 and 1150 deg. C. However, annealing resulted in bi-modal grain size distribution. Finer grains retained a significant dislocation density and populations of small precipitates with crystal structures distinct form the matrix. The grains and precipitates were much larger in alloys without Ti

Transmission electron microscopy characterization of the interfacial structure of a galvanized dual-phase steel

Energy Technology Data Exchange (ETDEWEB)

Aslam, I., E-mail: ia31@msstate.edu [Center for Advanced Vehicular Systems, Mississippi State University, MS 39759 (United States); Department of Mechanical Engineering, Mississippi State University, MS 39762 (United States); Li, B. [Center for Advanced Vehicular Systems, Mississippi State University, MS 39759 (United States); Department of Chemical and Materials Engineering, University of Nevada, Reno, NV 89557 (United States); Martens, R.L.; Goodwin, J.R. [Central Analytical Facility, the University of Alabama, Tuscaloosa, AL 35487 (United States); Rhee, H.J. [Center for Advanced Vehicular Systems, Mississippi State University, MS 39759 (United States); Department of Mechanical Engineering, Mississippi State University, MS 39762 (United States); Goodwin, F. [International Zinc Association, Durham, NC 27713 (United States)

2016-10-15

Site-specific studies were carried out to characterize the interface of a galvanized dual-phase (DP) steel. Focused ion beam (FIB) was used to prepare specimens in the interface region (~ 100 nm thick) between the coating and the substrate. Transmission electron microscopy (TEM), scanning TEM (STEM), and high resolution TEM (HRTEM) were performed to resolve the phases and the structures at the interface between the zinc (Zn) coating and the steel substrate. The STEM and TEM results showed that a continuous manganese oxide (MnO) film with a thickness of ~ 20 nm was present on the surface of the substrate while no silicon (Si) oxides were resolved. Internal oxide particles were observed as well in the sub-surface region. Despite the presence of the continuous oxide film, a well-developed inhibition layer was observed right on top of the oxide film. The inhibition layer has a thickness of ~ 100 nm. Possible mechanisms for the growth of the inhibition layer were discussed. - Highlights: •Site-specific examinations were performed on the Zn/steel interface. •Continuous external MnO oxides (20 nm) were observed at the interface. •No Si oxides were observed at the interface. •Internal oxide particles were distributed in the subsurface. •A continuous inhibition layer grew on top of the external oxides.

Establishment of in situ TEM-implanter/accelerator interface facility at Wuhan University

International Nuclear Information System (INIS)

Guo, L.P.; Liu, C.S.; Li, M.; Song, B.; Ye, M.S.; Fu, D.J.; Fan, X.J.

2008-01-01

In order to perform in situ investigations on the evolution of microstructures during ion irradiation for the evaluation of irradiation-resistance performance of advanced materials, we have established a transmission electron microscope (TEM)-implanter/accelerator interface facility at Wuhan University, the first of its kind in China. A Hitachi H800 TEM was linked to a 200 kV ion implanter and a 2x1.7 MV tandem accelerator through the interface system designed on the basis of ion beam transportation calculations. Effective steps were taken to isolate the TEM from mechanical vibration transmitted from the ion beam lines, and no significant degradation of microscope resolution was observed when the TEM operated under high zoom modes during the ion implantation. In the test experiments, ion beams of N + , He + , Ar + , and H + 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 80 nA. The amorphisation process of Si crystal irradiated by N + ion beams was successfully observed in the preliminary experiments, demonstrating that this interface facility is capable of in situ study of ion irradiated samples

The Electrochemical Behavior of SnSb as an Anode for Li-ion Batteries Studied by Electrochemical Impedance Spectroscopy and Electron Microscopy

International Nuclear Information System (INIS)

Tesfaye, Alexander T.; Yücel, Yasemin D.; Barr, Maïssa K.S.; Santinacci, Lionel; Vacandio, Florence; Dumur, Frédéric; Maria, Sébastien; Monconduit, Laure; Djenizian, Thierry

2017-01-01

Highlights: •Electrochemical behavior of SnSb is investigated by EIS, SEM and TEM. •Formation of SEI and cracks occurs during cycling experiments. •The capacity fading as a result of the electrode modifications is discussed. -- Abstract: Evolution of the electrical and morphological properties of micron-sized SnSb has been investigated to understand the electrochemical behavior observed during cycling experiments. Electron microscopy techniques (scanning electron microscopy and transmission electron microscopy) and electrochemical impedance spectroscopy have been combined to evidence the electrode modifications and particularly the formation of a solid electrolyte interphase (SEI) layer. Evolution of the SEI resistance and the charge transfer resistance with the cell voltage can be explained by the electrolyte degradation and expansion/contraction of the electrode. Furthermore, we show that the SEI formation is not limited at the first discharge/charge of the battery. The continuous growth of the SEI layer up to 50 cycles associated to the electrode pulverization caused by the large volume variations are responsible for the capacity fading.

Growth of Pd-Filled Carbon Nanotubes on the Tip of Scanning Probe Microscopy

Directory of Open Access Journals (Sweden)

Tomokazu Sakamoto

2009-01-01

Full Text Available We have synthesized Pd-filled carbon nanotubes (CNTs oriented perpendicular to Si substrates using a microwave plasma-enhanced chemical vapor deposition (MPECVD for the application of scanning probe microscopy (SPM tip. Prior to the CVD growth, Al thin film (10 nm was coated on the substrate as a buffer layer followed by depositing a 5∼40 nm-thick Pd film as a catalyst. The diameter and areal density of CNTs grown depend largely on the initial Pd thickness. Scanning electron microscopy (SEM and transmission electron microscopy (TEM images clearly show that Pd is successfully encapsulated into the CNTs, probably leading to higher conductivity. Using optimum growth conditions, Pd-filled CNTs are successfully grown on the apex of the conventional SPM cantilever.

TEM characterization of irradiated microstructure of Fe-9%Cr ODS and ferritic-martensitic alloys

Science.gov (United States)

Swenson, M. J.; Wharry, J. P.

2018-04-01

The objective of this study is to evaluate the effects of irradiation dose and dose rate on defect cluster (i.e. dislocation loops and voids) evolution in a model Fe-9%Cr oxide dispersion strengthened steel and commercial ferritic-martensitic steels HCM12A and HT9. Complimentary irradiations using Fe2+ ions, protons, or neutrons to doses ranging from 1 to 100 displacements per atom (dpa) at 500 °C are conducted on each alloy. The irradiated microstructures are characterized using transmission electron microscopy (TEM). Dislocation loops exhibit limited growth after 1 dpa upon Fe2+ and proton irradiation, while any voids observed are small and sparse. The average size and number density of loops are statistically invariant between Fe2+, proton, and neutron irradiated specimens at otherwise fixed irradiation conditions of ∼3 dpa, 500 °C. Therefore, we conclude that higher dose rate charged particle irradiations can reproduce the neutron irradiated loop microstructure with temperature shift governed by the invariance theory; this temperature shift is ∼0 °C for the high sink strength alloys studied herein.

Novel sample preparation for operando TEM of catalysts.

Science.gov (United States)

Miller, Benjamin K; Barker, Trevor M; Crozier, Peter A

2015-09-01

A new TEM sample preparation method is developed to facilitate operando TEM of gas phase catalysis. A porous Pyrex-fiber pellet TEM sample was produced, allowing a comparatively large amount of catalyst to be loaded into a standard Gatan furnace-type tantalum heating holder. The increased amount of catalyst present inside the environmental TEM allows quantitative determination of the gas phase products of a catalytic reaction performed in-situ at elevated temperatures. The product gas concentration was monitored using both electron energy loss spectroscopy (EELS) and residual gas analysis (RGA). Imaging of catalyst particles dispersed over the pellet at atomic resolution is challenging, due to charging of the insulating glass fibers. To overcome this limitation, a metal grid is placed into the holder in addition to the pellet, allowing catalyst particles dispersed over the grid to be imaged, while particles in the pellet, which are assumed to experience identical conditions, contribute to the overall catalytic conversion inside the environmental TEM cell. The gas within the cell is determined to be well-mixed, making this assumption reasonable. Copyright © 2015 Elsevier B.V. All rights reserved.

"One-sample concept" micro-combinatory for high throughput TEM of binary films.

Science.gov (United States)

Sáfrán, György

2018-04-01

Phases of thin films may remarkably differ from that of bulk. Unlike to the comprehensive data files of Binary Phase Diagrams [1] available for bulk, complete phase maps for thin binary layers do not exist. This is due to both the diverse metastable, non-equilibrium or instable phases feasible in thin films and the required volume of characterization work with analytical techniques like TEM, SAED and EDS. The aim of the present work was to develop a method that remarkably facilitates the TEM study of the diverse binary phases of thin films, or the creation of phase maps. A micro-combinatorial method was worked out that enables both preparation and study of a gradient two-component film within a single TEM specimen. For a demonstration of the technique thin Mn x Al 1- x binary samples with evolving concentration from x = 0 to x = 1 have been prepared so that the transition from pure Mn to pure Al covers a 1.5 mm long track within the 3 mm diameter TEM grid. The proposed method enables the preparation and study of thin combinatorial samples including all feasible phases as a function of composition or other deposition parameters. Contrary to known "combinatorial chemistry", in which a series of different samples are deposited in one run, and investigated, one at a time, the present micro-combinatorial method produces a single specimen condensing a complete library of a binary system that can be studied, efficiently, within a single TEM session. That provides extremely high throughput for TEM characterization of composition-dependent phases, exploration of new materials, or the construction of phase diagrams of binary films. Copyright © 2018 Elsevier B.V. All rights reserved.

A-10/TF34 Turbine Engine Monitoring System (TEMS)

Science.gov (United States)

Christopher, R. G.

1981-01-01

The hardware and software development of the A-10/TF34 turbine engine monitoring system (TEMS) is described. The operation and interfaces of the A-10/TF34 TEMS hardware are discussed with particular emphasis on function, capabilities, and limitations. The TEMS data types are defined and the various data acquisition modes are explained. Potential data products are also discussed.

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.

Instruments for radiation measurement in biosciences. Series 3. radioluminography. 11. Application of imaging plate in transmission electron microscopy

International Nuclear Information System (INIS)

Oikawa, Tetsuo

1999-01-01

Properties and application of the imaging plate (IP) in transmission electron microscopy (TEM) are reviewed. TEM has the resolution level of around 0.2 nm, which enables direct observation of molecules and atoms. In TEM, there are such recording systems as photographic film, TV camera, slow-scan CCD camera and IP. IP, to the electron beam, has the higher sensitivity than the film and has the broad dynamic range. Linearity between the input beam intensity and output signal is good, which makes it possible to record the image even with the small electron dose. Signal/noise ratio and detective quantum efficiency are important factors for precise image analysis. Fading phenomenon is a defect of IP, which weakens the signal output as time passing. For instance of application, IP is used for imaging of AgBr crystal fragile to strong electron beam required for the film. IP is necessary for quantitative analysis of TEM images and for the recently developed energy-filter TEM. (K.H.)

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

Plasticity mechanisms in ultrafine grained freestanding aluminum thin films revealed by in-situ transmission electron microscopy nanomechanical testing

International Nuclear Information System (INIS)

Idrissi, Hosni; Kobler, Aaron; Amin-Ahmadi, Behnam; Schryvers, Dominique; Coulombier, Michael; Pardoen, Thomas; Galceran, Montserrat; Godet, Stéphane; Raskin, Jean-Pierre; Kübel, Christian

2014-01-01

In-situ bright field transmission electron microscopy (TEM) nanomechanical tensile testing and in-situ automated crystallographic orientation mapping in TEM were combined to unravel the elementary mechanisms controlling the plasticity of ultrafine grained Aluminum freestanding thin films. The characterizations demonstrate that deformation proceeds with a transition from grain rotation to intragranular dislocation glide and starvation plasticity mechanism at about 1% deformation. The grain rotation is not affected by the character of the grain boundaries. No grain growth or twinning is detected

Plasticity mechanisms in ultrafine grained freestanding aluminum thin films revealed by in-situ transmission electron microscopy nanomechanical testing

Energy Technology Data Exchange (ETDEWEB)

Idrissi, Hosni, E-mail: hosni.idrissi@ua.ac.be [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Institute of Mechanics, Materials and Civil Engineering, Université catholique de Louvain, Place Sainte Barbe 2, B-1348 Louvain-La-Neuve (Belgium); Kobler, Aaron [Institute of Nanotechnology (INT) and Karlsruhe Nano Micro Facility (KNMF), Karlsruhe Institute of Technology - KIT, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany); Joint Research Laboratory Nanomaterials (KIT and TUD) at Technische Universität Darmstadt (TUD), Petersenstr. 32, 64287 Darmstadt (Germany); Amin-Ahmadi, Behnam; Schryvers, Dominique [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Coulombier, Michael; Pardoen, Thomas [Institute of Mechanics, Materials and Civil Engineering, Université catholique de Louvain, Place Sainte Barbe 2, B-1348 Louvain-La-Neuve (Belgium); Galceran, Montserrat; Godet, Stéphane [Matters and Materials Department, Université Libre de Bruxelles, 50 Av. FD Roosevelt CP194/03, 1050 Brussels (Belgium); Raskin, Jean-Pierre [Information and Communications Technologies, Electronics and Applied Mathematics (ICTEAM), Microwave Laboratory, Université catholique de Louvain, B-1348 Louvain-la-Neuve (Belgium); Kübel, Christian [Institute of Nanotechnology (INT) and Karlsruhe Nano Micro Facility (KNMF), Karlsruhe Institute of Technology - KIT, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen (Germany)

2014-03-10

In-situ bright field transmission electron microscopy (TEM) nanomechanical tensile testing and in-situ automated crystallographic orientation mapping in TEM were combined to unravel the elementary mechanisms controlling the plasticity of ultrafine grained Aluminum freestanding thin films. The characterizations demonstrate that deformation proceeds with a transition from grain rotation to intragranular dislocation glide and starvation plasticity mechanism at about 1% deformation. The grain rotation is not affected by the character of the grain boundaries. No grain growth or twinning is detected.

VES/TEM 1D joint inversion by using Controlled Random Search (CRS) algorithm

Science.gov (United States)

Bortolozo, Cassiano Antonio; Porsani, Jorge Luís; Santos, Fernando Acácio Monteiro dos; Almeida, Emerson Rodrigo

2015-01-01

Electrical (DC) and Transient Electromagnetic (TEM) soundings are used in a great number of environmental, hydrological, and mining exploration studies. Usually, data interpretation is accomplished by individual 1D models resulting often in ambiguous models. This fact can be explained by the way as the two different methodologies sample the medium beneath surface. Vertical Electrical Sounding (VES) is good in marking resistive structures, while Transient Electromagnetic sounding (TEM) is very sensitive to conductive structures. Another difference is VES is better to detect shallow structures, while TEM soundings can reach deeper layers. A Matlab program for 1D joint inversion of VES and TEM soundings was developed aiming at exploring the best of both methods. The program uses CRS - Controlled Random Search - algorithm for both single and 1D joint inversions. Usually inversion programs use Marquadt type algorithms but for electrical and electromagnetic methods, these algorithms may find a local minimum or not converge. Initially, the algorithm was tested with synthetic data, and then it was used to invert experimental data from two places in Paraná sedimentary basin (Bebedouro and Pirassununga cities), both located in São Paulo State, Brazil. Geoelectric model obtained from VES and TEM data 1D joint inversion is similar to the real geological condition, and ambiguities were minimized. Results with synthetic and real data show that 1D VES/TEM joint inversion better recovers simulated models and shows a great potential in geological studies, especially in hydrogeological studies.

TEM-turbulence in stellarators and its optimization

Science.gov (United States)

Proll, Josefine H. E.; Helander, Per; Lazerson, Samuel; Mynick, Harry; Xanthopoulos, Pavlos

2014-10-01

Quasi-isodynamic stellarators, which are especially optimized for neoclassical transport, have been shown to be resilient towards trapped-electrons modes (TEMs) in large regions of parameter space. In these configurations, all particles have average ``good curvature.'' It was shown analytically that, thanks to this property, particles that bounce faster than the mode in question draw energy from it near marginal stability, so that the ordinary density-gradient-driven TEM has to be stable in the electrostatic and collisionless limit.This has been confirmed in linear flux-tube simulations that were performed with the GENE code. Several magnetic field configurations were compared and it was found that the growth rates of the TEMs drop with increasing degree of quasi-isodynamicity. These findings can be used to optimize stellarators with respect to TEM turbulence by reducing the fraction of trapped particles with bounce averaged ``bad curvature.'' An appropriate proxy function has therefore been designed to be implemented in STELLOPT, a stellarator optimization tool that can now be used to further explore the configuration space of neoclassically optimized stellarators with the aim to extract designs with improved turbulent transport. This work was facilitated by the Max-Planck/Princeton Center for Plasma Physics.

Transformations of gold nanoparticles investigated using variable temperature high-resolution transmission electron microscopy

Energy Technology Data Exchange (ETDEWEB)

Young, N.P. [Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH (United Kingdom); Huis, M.A. van; Zandbergen, H.W. [Kavli Institute of Nanoscience, Delft University of Technolgy, Lorentzweg 1, NL-2628CJ, Delft, The Netherlands. (Netherlands); Xu, H. [Department of Geology and Geophysics, and Materials Science Program, University of Wisconsin-Madison, Madison, WI (United States); Kirkland, A.I., E-mail: angus.kirkland@materials.ox.ac.uk [Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH (United Kingdom)

2010-04-15

Recently designed advanced in-situ specimen holders for transmission electron microscopy (TEM) have been used in studies of gold nanoparticles. We report results of variable temperature TEM experiments in which structural transformations have been correlated with specimen temperature, allowing general trends to be identified. Transformation to a decahedral morphology for particles in the size range 5-12 nm was observed for the majority of particles regardless of their initial structure. Following in-situ annealing, decahedra were found to be stable at room temperature, confirming this as the equilibrium morphology, in agreement with recently calculated phase diagrams. Other transitions at low temperature in addition to surface roughening have also been observed and correlated with the same nanoscale phase diagram. Investigations of gold particles at high temperature have revealed evidence for co-existing solid and liquid phases. Overall, these results are important in a more precise understanding of the structure and action of catalytic gold nanoparticles and in the experimental verification of theoretical calculations.

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

Electrical and optical studies in polyaniline nanofibre–SnO 2 ...

Indian Academy of Sciences (India)

Polyaniline nanofibre–tin oxide (PAni-SnO2) nanocomposites are synthesized and mixed with polyvinyl alcohol (PVA) as stabilizer to cast free-standing films. Composite films are characterized by X-ray diffraction studies (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), ...

Microstructure of NiTi orthodontic wires observations using transmission electron microscopy

OpenAIRE

Ferčec, J.; Jenko, D.; Buchmeister, B.; Rojko, F.; Budič, B.; Kosec, B.; Rudolf, R.

2014-01-01

This work presents the results of the microstructure observation of six different types of NiTi orthodontic wires by using Transmission Electron Microscopy (TEM). Within these analyses the chemical compositions of each wire were observed in different places by applying the EDS detector. Namely, the chemical composition in the orthodontic wires is very important because it shows the dependence between the phase temperatures and mechanical properties. Microstructure observations showed that ort...

Laboratory design for high-performance electron microscopy

Energy Technology Data Exchange (ETDEWEB)

O' Keefe, Michael A.; Turner, John H.; Hetherington, Crispin J.D.; Cullis, A.G.; Carragher, Bridget; Jenkins, Ron; Milgrim, Julie; Milligan,Ronald A.; Potter, Clinton S.; Allard, Lawrence F.; Blom, Douglas A.; Degenhardt, Lynn; Sides, William H.

2004-04-23

Proliferation of electron microscopes with field emission guns, imaging filters and hardware spherical aberration correctors (giving higher spatial and energy resolution) has resulted in the need to construct special laboratories. As resolutions improve, transmission electron microscopes (TEMs) and scanning transmission electron microscopes (STEMs) become more sensitive to ambient conditions. State-of-the-art electron microscopes require state-of-the-art environments, and this means careful design and implementation of microscope sites, from the microscope room to the building that surrounds it. Laboratories have been constructed to house high-sensitive instruments with resolutions ranging down to sub-Angstrom levels; we present the various design philosophies used for some of these laboratories and our experiences with them. Four facilities are described: the National Center for Electron Microscopy OAM Laboratory at LBNL; the FEGTEM Facility at the University of Sheffield; the Center for Integrative Molecular Biosciences at TSRI; and the Advanced Microscopy Laboratory at ORNL.

Indications and techniques of transanal endoscopic microsurgery (TEMS).

Science.gov (United States)

Qi, Yanjie; Stoddard, David; Monson, John R T

2011-08-01

Transanal endoscopic microsurgery (TEMS) has recently reemerged as a valuable technique for the management of rectal neoplasms - both benign and malignant. Since the original description of this technique in the early 1980s, TEMS has emerged as the approach of choice for most benign rectal tumors because of the excellent views provided and superior dissection techniques possible when compared to traditional transanal excision. Many published reports demonstrate that the lowest rates of recurrence are associated with TEMS probably because of full-thickness excision with negative margins. Increasingly, TEMS is being applied to primary rectal cancer when used alone as a full-thickness excision alone or in combination with additional therapies, depending on tumor stage. There is now a significant evidence base to suggest that this approach should be considered as part of a multidisciplinary approach to rectal cancer. This paper describes indications and techniques for this technology.

Structural characterizaiton and gas reactions of small metal particles by high-resolution, in-situ TEM and TED

Science.gov (United States)

1984-01-01

The existing in-situ transmission electron microscopy (TEM) facility was improved by adding a separately pumped mini-specimen chamber. The chamber contains wire-evaporation sources for three metals and a specimen heater for moderate substrate temperatures. A sample introduction device was constructed, installed, and tested, facilitating rapid introduction of a specimen into the mini-chamber while maintaining the background pressure in that chamber in the 10(-9) millibar range. Small particles and clusters of Pd, grown by deposition from the vapor phase in an in-situ TEM facility on amorphous and crystalline support films of alumina and on ultra-thin carbon films, were analyzed by conventional high-resolution TEM and image analysis in terms of detectability, number density, and size distribution. The smallest particles that could be detected and counted contained no more than 6 atoms; size determinations could be made for particles 1 nm in diameter. The influence of various oxygen plasma treatments, annealing treatments, and of increasing the substrate temperature during deposition was investigated. The TEM technique was employed to demonstrate that under otherwise identica l conditions the lattice parameter of Pd particles in the 1 to 2 nm size range and supported in random orientation on ex-situ prepared mica films is expanded by some 3% when compared to 5 nm size particles. It is believed that this expansion is neither a small-particle diffraction effect nor due to pseudomorphism, but that it is due to a annealing-induced transformation of the small as-deposited particles with predominantly composite crystal structures into larger particles with true f.c.c. structure and thus inherently smaller lattice parameter.

Towards a more realistic picture of in situ biocide actions: Combining physiological and microscopy techniques

Energy Technology Data Exchange (ETDEWEB)

Speranza, M., E-mail: speranzamariela@gmail.com [Museo Nacional de Ciencias Naturales, MNCN-CSIC, Serrano 115 bis, 28006 Madrid (Spain); Wierzchos, J.; De Los Rios, A.; Perez-Ortega, S. [Museo Nacional de Ciencias Naturales, MNCN-CSIC, Serrano 115 bis, 28006 Madrid (Spain); Souza-Egipsy, V. [Instituto de Ciencias Agrarias, ICA-CSIC, Serrano 115 bis, 28006 Madrid (Spain); Ascaso, C., E-mail: ascaso@mncn.csic.es [Museo Nacional de Ciencias Naturales, MNCN-CSIC, Serrano 115 bis, 28006 Madrid (Spain)

2012-11-15

In this study, we combined chlorophyll a fluorescence (ChlaF) measurements, using pulse-amplitude-modulate (PAM) equipment, with scanning electron microscopy in backscattered electron mode (SEM-BSE) and transmission electron microscopy (TEM) images to evaluate the actions of Koretrel at lower concentrations on Verrucaria nigrescens colonising a dolostone. ChlaF measurements are good indicators of the damaging effects of biocides. However, these indicators only provide an incomplete view of the mechanism of biocides used to control biodeterioration agents. The death of the V. nigrescens photobiont at two biocide concentrations was revealed by PAM, SEM-BSE and TEM. Once Koretrel was applied, the Fv/Fm ratios markedly fell in the first few hours after the 1.5% treatment, and ratios for the 3% dilution remained close to zero throughout the study. The algal zone shows the plasmolysed appearance of the photobiont cells, and important aspects related to the action of the biocide on free and lichenised fungi were also detected using SEM-BSE. Many of the mycobiont cells had only their cell walls preserved; although, some fungal hyphae in lichen thalli and some microorganisms in endolithic clusters maintained lipid storage in their cytoplasm. These results indicated that the combination of physiological and microscopy techniques improves the assessment of biocide action in situ and this will help to optimize protocols in order to reduce the emission of these compounds to the environment. -- Highlights: Black-Right-Pointing-Pointer We combined ChlaF measurements with EM images to analyses the biocides action on stone biodeterioration agents. Black-Right-Pointing-Pointer At lower biocide concentrations damage to photobiont and mycobiont cells integrity, ultrastructure and vitality were observed. Black-Right-Pointing-Pointer The limited action of biocides on fungi and algae were detected using SEM-BSE. Black-Right-Pointing-Pointer The combination of physiological and microscopy

Direct nanofabrication and transmission electron microscopy on a suite of easy-to-prepare ultrathin film substrates

International Nuclear Information System (INIS)

Allred, Daniel B.; Zin, Melvin T.; Ma, Hong; Sarikaya, Mehmet; Baneyx, Francois; Jen, Alex K.-Y.; Schwartz, Daniel T.

2007-01-01

A high-yield, easy to master method for preparing electron transparent metal, oxide, and carbon ultrathin film substrates suitable for direct nano/micro-fabrication and transmission electron microscopy (TEM) is presented. To demonstrate the versatility of these substrates for fabrication processes, we use e-beam lithography, self-assembled colloidal and protein templates, and microcontact printing to create patterned masks for subsequent electrodeposition of two dimensional and three dimensional structures. The electrodeposited structures range in scale from a few nanometers to a few micrometers in characteristic dimensions. Because fabrication occurs directly on ultrathin films, TEM analysis of the resulting materials and buried interfaces is straightforward without any destructive sample preparation. We show that all the normal TEM analytical methods (imaging, diffraction, electron and X-ray spectroscopies) are compatible with the fabricated structures and the thin film substrates. These electron transparent substrates have largely rendered the need for TEM sample preparation on fabricated structures obsolete in our lab

Morphological Study on Room-Temperature-Cured PMMA-Grafted Natural Rubber-Toughened Epoxy/Layered Silicate Nanocomposite

Directory of Open Access Journals (Sweden)

N. Y. Yuhana

2012-01-01

Full Text Available A morphological study was conducted on ternary systems containing epoxy, PMMA-grafted natural rubber, and organic chemically modified montmorillonite (Cloisite 30B. Optical microscopy, transmission electron microscopy (TEM, scanning electron microscopy (SEM, energy dispersive X-ray (EDX, and wide-angle X-ray diffraction (WAXD analysis were used. The following four materials were prepared at room temperature: cured unmodified epoxy, cured toughened epoxy, cured unmodified epoxy/Cloisite 30B nanocomposites, and cured toughened epoxy/Cloisite 30B nanocomposites. Mixing process was performed by mechanical stirring. Poly(etheramine was used as the curing agent. The detailed TEM images revealed co-continuous and dispersed spherical rubber in the epoxy-rubber blend, suggesting a new proposed mechanism of phase separation. High-magnification TEM analysis showed good interactions between rubber and Cloisite 30B in the ternary system. Also, it was found that rubber particles could enhance the separation of silicates layers. Both XRD and TEM analyses confirmed that the intercalation of Cloisite 30B was achieved. No distinct exfoliated silicates were observed by TEM. Aggregates of layered silicates (tactoids were observed by SEM and EDX, in addition to TEM at low magnification. EDX analysis confirmed the presence of organic and inorganic elements in the binary and ternary epoxy systems containing Cloisite 30B.

Preparation of carbon-free TEM microgrids by metal sputtering

International Nuclear Information System (INIS)

Janbroers, S.; Kruijff, T.R. de; Xu, Q.; Kooyman, P.J.; Zandbergen, H.W.

2009-01-01

A new method for preparing carbon-free, temperature-stable Transmission Electron Microscope (TEM) grids is presented. An 80% Au/20% Pd metal film is deposited onto a 'holey' microgrid carbon supported on standard mixed-mesh Au TEM grids. Subsequently, the carbon film is selectively removed using plasma cleaning. In this way, an all-metal TEM film is made containing the 'same' microgrid as the original carbon film. Although electron transparency of the foil is reduced significantly, the open areas for TEM inspection of material over these areas are maintained. The metal foil can be prepared with various thicknesses and ensures good electrical conductivity. The new Au/Pd grids are stable to at least 775 K under vacuum conditions.

Preparation of carbon-free TEM microgrids by metal sputtering.

Science.gov (United States)

Janbroers, S; de Kruijff, T R; Xu, Q; Kooyman, P J; Zandbergen, H W

2009-08-01

A new method for preparing carbon-free, temperature-stable Transmission Electron Microscope (TEM) grids is presented. An 80% Au/20% Pd metal film is deposited onto a 'holey' microgrid carbon supported on standard mixed-mesh Au TEM grids. Subsequently, the carbon film is selectively removed using plasma cleaning. In this way, an all-metal TEM film is made containing the 'same' microgrid as the original carbon film. Although electron transparency of the foil is reduced significantly, the open areas for TEM inspection of material over these areas are maintained. The metal foil can be prepared with various thicknesses and ensures good electrical conductivity. The new Au/Pd grids are stable to at least 775K under vacuum conditions.

Current status and future directions for in situ transmission electron microscopy

Energy Technology Data Exchange (ETDEWEB)

Taheri, Mitra L. [Department of Materials Science and Engineering, Drexel University (United States); Stach, Eric A. [Center for Functional Nanomaterials, National Laboratory, Brookhaven (United States); Arslan, Ilke [Pacific Northwest National Laboratory, Physical and Computational Sciences Directorate, 902 Battelle Blvd, Richland, WA (United States); Crozier, P.A. [School for Engineering of Matter, Transport and Energy, Arizona State University, Tempe, AZ 85281 (United States); Kabius, Bernd C. [The Pennsylvania State University, University Park, PA 16802 (United States); LaGrange, Thomas [Lawrence Livermore National Laboratory, Physical and Life Science Directorate, Condensed Matter and Materials Division, 7000 East Avenue, P.O. 808 L-356 (United States); Minor, Andrew M. [Department of Materials Science & Engineering, University of California, Berkeley and National Center for Electron Microscopy, Molecular Foundry, Lawrence Berkeley National Laboratory, One Cyclotron Road, MS 72, Berkeley, CA (United States); Takeda, Seiji [Institute of Scientific and Industrial Research (ISIR), Osaka University, 8-1 Mihogaoka, Ibaraki, Osaka 567-0047 (Japan); Tanase, Mihaela [Center for Nanoscale Science and Technology, National Institute of Standards and Technology, Gaithersburg, MD 20899-6203 (United States); Wagner, Jakob B. [Center for Electron Nanoscopy, Technical University of Denmark, Kgs, Lyngby (Denmark); Sharma, Renu, E-mail: renu.sharma@nist.gov [Center for Nanoscale Science and Technology, National Institute of Standards and Technology, Gaithersburg, MD 20899-6203 (United States)

2016-11-15

This review article discusses the current and future possibilities for the application of in situ transmission electron microscopy to reveal synthesis pathways and functional mechanisms in complex and nanoscale materials. The findings of a group of scientists, representing academia, government labs and private sector entities (predominantly commercial vendors) during a workshop, held at the Center for Nanoscale Science and Technology- National Institute of Science and Technology (CNST-NIST), are discussed. We provide a comprehensive review of the scientific needs and future instrument and technique developments required to meet them. - Highlights: • Evaluation of currently available technology for performing in situ experiments using transmission electron microscope. • Limitations of currently available instrumentation with respect to base TEM, specialty TEM holders, and data acquisition systems. • Guidelines and wish list for the areas of future development.

Atomic-resolution transmission electron microscopy of electron beam–sensitive crystalline materials

Science.gov (United States)

Zhang, Daliang; Zhu, Yihan; Liu, Lingmei; Ying, Xiangrong; Hsiung, Chia-En; Sougrat, Rachid; Li, Kun; Han, Yu

2018-02-01

High-resolution imaging of electron beam–sensitive materials is one of the most difficult applications of transmission electron microscopy (TEM). The challenges are manifold, including the acquisition of images with extremely low beam doses, the time-constrained search for crystal zone axes, the precise image alignment, and the accurate determination of the defocus value. We develop a suite of methods to fulfill these requirements and acquire atomic-resolution TEM images of several metal organic frameworks that are generally recognized as highly sensitive to electron beams. The high image resolution allows us to identify individual metal atomic columns, various types of surface termination, and benzene rings in the organic linkers. We also apply our methods to other electron beam–sensitive materials, including the organic-inorganic hybrid perovskite CH3NH3PbBr3.

Current status and future directions for in situ transmission electron microscopy

International Nuclear Information System (INIS)

Taheri, Mitra L.; Stach, Eric A.; Arslan, Ilke; Crozier, P.A.; Kabius, Bernd C.; LaGrange, Thomas; Minor, Andrew M.; Takeda, Seiji; Tanase, Mihaela; Wagner, Jakob B.; Sharma, Renu

2016-01-01

This review article discusses the current and future possibilities for the application of in situ transmission electron microscopy to reveal synthesis pathways and functional mechanisms in complex and nanoscale materials. The findings of a group of scientists, representing academia, government labs and private sector entities (predominantly commercial vendors) during a workshop, held at the Center for Nanoscale Science and Technology- National Institute of Science and Technology (CNST-NIST), are discussed. We provide a comprehensive review of the scientific needs and future instrument and technique developments required to meet them. - Highlights: • Evaluation of currently available technology for performing in situ experiments using transmission electron microscope. • Limitations of currently available instrumentation with respect to base TEM, specialty TEM holders, and data acquisition systems. • Guidelines and wish list for the areas of future development.

Atomic-resolution transmission electron microscopy of electron beam–sensitive crystalline materials

KAUST Repository

Zhang, Daliang

2018-01-18

High-resolution imaging of electron beam-sensitive materials is one of the most difficult applications of transmission electron microscopy (TEM). The challenges are manifold, including the acquisition of images with extremely low beam doses, the time-constrained search for crystal zone axes, the precise image alignment, and the accurate determination of the defocus value. We develop a suite of methods to fulfill these requirements and acquire atomic-resolution TEM images of several metal organic frameworks that are generally recognized as highly sensitive to electron beams. The high image resolution allows us to identify individual metal atomic columns, various types of surface termination, and benzene rings in the organic linkers. We also apply our methods to other electron beam–sensitive materials, including the organic-inorganic hybrid perovskite CH3NH3PbBr3.

Microstructural and micromechanical characterisation of TiAl alloys using atomic force microscopy and nanoindentation

International Nuclear Information System (INIS)

Gebhard, S.; Pyczak, F.; Goeken, M.

2009-01-01

Different microstructures were generated in the Ti-45Al-4.6Nb-0.2B-0.2C and Ti-45Al-1Cr alloys (at.%) by heat treatment. The microstructures were investigated using nanoindentation and atomic force microscopy which was compared with transmission electron microscopy. Topographic contrast is usually used for phase identification in the atomic force microscope. However, it was found that the topographic order of the phases changes with different microstructures and specimen preparations. Nanoindentation measurements provided local hardness values not obtainable by other methods and enabled clear distinction of the phases. The hardness values can give information on surrounding microstructure and solid solution hardening. The mean lamellar spacing of the colonies was measured using both atomic force microscopy and transmission electron microscopy. Atomic force microscopy was found to be suitable to determine the spacing between α 2 /γ-interfaces offering the advantages of easier sample preparation and fewer specimens compared to evaluation by TEM analysis.

16S rRNA gene metabarcoding and TEM reveals different ecological strategies within the genus Neogloboquadrina (planktonic foraminifer.

Directory of Open Access Journals (Sweden)

Clare Bird

Full Text Available Uncovering the complexities of trophic and metabolic interactions among microorganisms is essential for the understanding of marine biogeochemical cycling and modelling climate-driven ecosystem shifts. High-throughput DNA sequencing methods provide valuable tools for examining these complex interactions, although this remains challenging, as many microorganisms are difficult to isolate, identify and culture. We use two species of planktonic foraminifera from the climatically susceptible, palaeoceanographically important genus Neogloboquadrina, as ideal test microorganisms for the application of 16S rRNA gene metabarcoding. Neogloboquadrina dutertrei and Neogloboquadrina incompta were collected from the California Current and subjected to either 16S rRNA gene metabarcoding, fluorescence microscopy, or transmission electron microscopy (TEM to investigate their species-specific trophic interactions and potential symbiotic associations. 53-99% of 16S rRNA gene sequences recovered from two specimens of N. dutertrei were assigned to a single operational taxonomic unit (OTU from a chloroplast of the phylum Stramenopile. TEM observations confirmed the presence of numerous intact coccoid algae within the host cell, consistent with algal symbionts. Based on sequence data and observed ultrastructure, we taxonomically assign the putative algal symbionts to Pelagophyceae and not Chrysophyceae, as previously reported in this species. In addition, our data shows that N. dutertrei feeds on protists within particulate organic matter (POM, but not on bacteria as a major food source. In total contrast, of OTUs recovered from three N. incompta specimens, 83-95% were assigned to bacterial classes Alteromonadales and Vibrionales of the order Gammaproteobacteria. TEM demonstrates that these bacteria are a food source, not putative symbionts. Contrary to the current view that non-spinose foraminifera are predominantly herbivorous, neither N. dutertrei nor N. incompta

Focus-variation image reconstruction in field-emission TEM

NARCIS (Netherlands)

Coene, W.M.J.; Janssen, A.J.E.M.; Op de Beeck, M.; Van Dyck, D.; Van Zwet, E.J.; Zandbergen, H.W.; Bailey, G.W.; Rieder, C.L.

1993-01-01

The use of a field emission gun (FEG) in high resolution TEM (HRTEM) improves the information limit much below the point resolution. In the area between point and information resolution of the FEG-TEM, image interpretation is complicated by the lens aberrations and focus effects. Different

ToTem: a tool for variant calling pipeline optimization.

Science.gov (United States)

Tom, Nikola; Tom, Ondrej; Malcikova, Jitka; Pavlova, Sarka; Kubesova, Blanka; Rausch, Tobias; Kolarik, Miroslav; Benes, Vladimir; Bystry, Vojtech; Pospisilova, Sarka

2018-06-26

High-throughput bioinformatics analyses of next generation sequencing (NGS) data often require challenging pipeline optimization. The key problem is choosing appropriate tools and selecting the best parameters for optimal precision and recall. Here we introduce ToTem, a tool for automated pipeline optimization. ToTem is a stand-alone web application with a comprehensive graphical user interface (GUI). ToTem is written in Java and PHP with an underlying connection to a MySQL database. Its primary role is to automatically generate, execute and benchmark different variant calling pipeline settings. Our tool allows an analysis to be started from any level of the process and with the possibility of plugging almost any tool or code. To prevent an over-fitting of pipeline parameters, ToTem ensures the reproducibility of these by using cross validation techniques that penalize the final precision, recall and F-measure. The results are interpreted as interactive graphs and tables allowing an optimal pipeline to be selected, based on the user's priorities. Using ToTem, we were able to optimize somatic variant calling from ultra-deep targeted gene sequencing (TGS) data and germline variant detection in whole genome sequencing (WGS) data. ToTem is a tool for automated pipeline optimization which is freely available as a web application at  https://totem.software .

Determination of the Projected Atomic Potential by Deconvolution of the Auto-Correlation Function of TEM Electron Nano-Diffraction Patterns

Directory of Open Access Journals (Sweden)

Liberato De Caro

2016-11-01

Full Text Available We present a novel method to determine the projected atomic potential of a specimen directly from transmission electron microscopy coherent electron nano-diffraction patterns, overcoming common limitations encountered so far due to the dynamical nature of electron-matter interaction. The projected potential is obtained by deconvolution of the inverse Fourier transform of experimental diffraction patterns rescaled in intensity by using theoretical values of the kinematical atomic scattering factors. This novelty enables the compensation of dynamical effects typical of transmission electron microscopy (TEM experiments on standard specimens with thicknesses up to a few tens of nm. The projected atomic potentials so obtained are averaged on sample regions illuminated by nano-sized electron probes and are in good quantitative agreement with theoretical expectations. Contrary to lens-based microscopy, here the spatial resolution in the retrieved projected atomic potential profiles is related to the finer lattice spacing measured in the electron diffraction pattern. The method has been successfully applied to experimental nano-diffraction data of crystalline centrosymmetric and non-centrosymmetric specimens achieving a resolution of 65 pm.

Size Determination of Au Aerosol Nanoparticles by Off-Line TEM/STEM Observations

Science.gov (United States)

Karlsson, Lisa S.; Deppert, Knut; Malm, Jan-Olle

2006-12-01

Determination of particle size distributions of Au aerosol nanoparticles has been performed by a TEM/STEM investigation. The particles are generated by an evaporation/condensation method and are size-selected by differential mobility analyzers (DMA) based on their electrical mobility. Off-line TEM measurements resulted in equivalent projected area diameters assuming that the particles are spherical in shape. In this paper critical factors such as magnification calibration, sampling, image analysis, beam exposure and, particle shape are treated. The study shows that the measures of central tendency; mean, median and mode, are equal as expected from a narrow size distribution. Moreover, the correlation between TEM/STEM and DMA are good, in practice 1:1. Also, STEM has the advantage over TEM due to enhanced contrast and is proposed as an alternative route for determination of particle size distributions of nanoparticles with lower contrast.

Size Determination of Au Aerosol Nanoparticles by Off-Line TEM/STEM Observations

International Nuclear Information System (INIS)

Karlsson, Lisa S.; Deppert, Knut; Malm, Jan-Olle

2006-01-01

Determination of particle size distributions of Au aerosol nanoparticles has been performed by a TEM/STEM investigation. The particles are generated by an evaporation/condensation method and are size-selected by differential mobility analyzers (DMA) based on their electrical mobility. Off-line TEM measurements resulted in equivalent projected area diameters assuming that the particles are spherical in shape. In this paper critical factors such as magnification calibration, sampling, image analysis, beam exposure and, particle shape are treated. The study shows that the measures of central tendency; mean, median and mode, are equal as expected from a narrow size distribution. Moreover, the correlation between TEM/STEM and DMA are good, in practice 1:1. Also, STEM has the advantage over TEM due to enhanced contrast and is proposed as an alternative route for determination of particle size distributions of nanoparticles with lower contrast

Transmission electron microscopy of polyhydroxybutyrate-co-valerate (PHBV)/nanocrystalline cellulose (NCC) bio-nanocomposite prepared using cryo-ultramicrotomy

Science.gov (United States)

Ismarul, N. I.; Engku, A. H. E. U.; Siti, N. K.; Tay, K. Y.

2017-12-01

Environmental issues on disposal and end-of-life for product made from synthetic petroleum-derived polymers have gained increasing attention from materials scientist to search for new materials with similar physical and mechanical properties but environmental friendly in a way that they are renewable and biodegradable as well. This work is to study the effect of nanocrystalline cellulose in improving the thermal stability of polyhydroxybutyrate-co-valerate biopolymer for high temperature processing of packaging material. 10 % w/w PHBV-NCC bio-nanocomposite feedstock pellet prepared using RONDOL minilab compounder was used as the sample for the preparation of Transmission Electron Microscopy (TEM) sample. RMC Cryo-Ultramicrotomy equipment was used to prepare the ultra-thin slice of the bio-nanocomposite pellet under liquid nitrogen at - 60 °C. Diamond knife was used to slice off about 80-100 nm ultra-thin bio-nanocomposite films and was transferred into the lacey carbon film coated grid using cooled sugar solution. A few drops of phosphotungstic acid was used as negative stain to improve the contrast during the TEM analysis. HITACHI TEM systems was used to obtain the TEM micrograph of PHBV-NCC bio-nanocomposite using 80kV accelerating voltage. A well dispersed NCC in PHBV matrix, ranging from 5 to 25 nm in width was observed.

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

Preparation of carbon-free TEM microgrids by metal sputtering

Energy Technology Data Exchange (ETDEWEB)

Janbroers, S., E-mail: stephan.janbroers@albemarle.com [Albemarle Catalysts B.V., Nieuwendammerkade 1-3, 1030 BE, Amsterdam (Netherlands); Kavli Institute of Nanoscience, Delft University of Technology, Lorentzweg 1, 2628 CJ Delft (Netherlands); Kruijff, T.R. de; Xu, Q. [Kavli Institute of Nanoscience, Delft University of Technology, Lorentzweg 1, 2628 CJ Delft (Netherlands); Kooyman, P.J. [DelftChemTech, Delft University of Technology, Julianalaan 136, 2628 BL, Delft (Netherlands); Kavli Institute of Nanoscience, Delft University of Technology, Lorentzweg 1, 2628 CJ Delft (Netherlands); Zandbergen, H.W. [Kavli Institute of Nanoscience, Delft University of Technology, Lorentzweg 1, 2628 CJ Delft (Netherlands)

2009-08-15

A new method for preparing carbon-free, temperature-stable Transmission Electron Microscope (TEM) grids is presented. An 80% Au/20% Pd metal film is deposited onto a 'holey' microgrid carbon supported on standard mixed-mesh Au TEM grids. Subsequently, the carbon film is selectively removed using plasma cleaning. In this way, an all-metal TEM film is made containing the 'same' microgrid as the original carbon film. Although electron transparency of the foil is reduced significantly, the open areas for TEM inspection of material over these areas are maintained. The metal foil can be prepared with various thicknesses and ensures good electrical conductivity. The new Au/Pd grids are stable to at least 775 K under vacuum conditions.

Regulation of ETG turbulence by TEM driven zonal flows

Science.gov (United States)

Asahi, Yuuichi; Ishizawa, Akihiro; Watanabe, Tomohiko; Tsutsui, Hiroaki; Tsuji-Iio, Shunji

2013-10-01

Anomalous heat transport driven by electron temperature gradient (ETG) turbulence is investigated by means of gyrokinetic simulations. It is found that the ETG turbulence can be suppressed by zonal flows driven by trapped electron modes (TEMs). The TEMs appear in a statistically steady state of ETG turbulence and generate zonal flows, while its growth rate is much smaller than those of ETGs. The TEM-driven zonal flows with lower radial wave numbers are more strongly generated than those driven by ETG modes, because of the higher zonal flow response to a density source term. An ExB shearing rate of the TEM-driven zonal flows is strong enough to suppress the long-wavelength ETG modes which make the main contribution to the turbulent transport.

Performance of a field emission gun TEM/STEM

International Nuclear Information System (INIS)

Carpenter, R.W.; Bentley, J.

1979-01-01

First experimental results on a Phillips EM 400 TEM/STEM fitted with a field-emission electron gun and objective twin lens are given here. Operation of the FEG is reliable up to maximum design voltage (120 kV). Highest resolution achieved in TEM was 1.9 A fringe. A wide variety of diffraction modes were demonstrated, ranging from CBDP from a small area (approx. 10 A dia) in STEM mode to SAD with angular resolution of 8 μrad in TEM mode. The EDS sensitivity is very high. STEM imaging performance to the highest magnifications examined (200 kx) is good. Work is in progress to evaluate the limits of STEM performance

Retrofit implementation of Zernike phase plate imaging for cryo-TEM.

Science.gov (United States)

Marko, Michael; Leith, Ardean; Hsieh, Chyongere; Danev, Radostin

2011-05-01

In-focus phase-plate imaging is particularly beneficial for cryo-TEM because it offers a substantial overall increase in image contrast, without an electron dose penalty, and it simplifies image interpretation. We show how phase-plate cryo-TEM can be implemented with an appropriate existing TEM, and provide a basic practical introduction to use of thin-film (carbon) phase plates. We point out potential pitfalls of phase-plate operation, and discuss solutions. We provide information on evaluating a particular TEM for its suitability. Copyright © 2011 Elsevier Inc. All rights reserved.

Characterization of CuCl quantum dots grown in NaCl single crystals via optical measurements, X-ray diffraction, and transmission electron microscopy

Science.gov (United States)

Miyajima, Kensuke; Akatsu, Tatsuro; Itoh, Ken

2018-05-01

We evaluated the crystal size, shape, and alignment of the lattice planes of CuCl quantum dots (QDs) embedded in NaCl single crystals by optical measurements, X-ray diffraction (XRD) patterns, and transmission electron microscopy (TEM). We obtained, for the first time, an XRD pattern and TEM images for CuCl QDs in NaCl crystals. The XRD pattern showed that the lattice planes of the CuCl QDs were parallel to those of the NaCl crystals. In addition, the size of the QDs was estimated from the diffraction width. It was apparent from the TEM images that almost all CuCl QDs were polygonal, although some cubic QDs were present. The mean size and size distribution of the QDs were also obtained. The dot size obtained from optical measurements, XRD, and TEM image were almost consistent. Our new findings can help to reveal the growth mechanism of semiconductor QDs embedded in a crystallite matrix. In addition, this work will play an important role in progressing the study of optical phenomena originating from assembled semiconductor QDs.

Investigation of (Fe,Co)NbB-Based Nanocrystalline Soft Magnetic Alloys by Lorentz Microscopy and Off-Axis Electron Holography.

Science.gov (United States)

Zheng, Changlin; Kirmse, Holm; Long, Jianguo; Laughlin, David E; McHenry, Michael E; Neumann, Wolfgang

2015-04-01

The relationship between microstructure and magnetic properties of a (Fe,Co)NbB-based nanocrystalline soft magnetic alloy was investigated by analytical transmission electron microscopy (TEM). The microstructures of (Fe0.5Co0.5)80Nb4B13Ge2Cu1 nanocrystalline alloys annealed at different temperatures were characterized by TEM and electron diffraction. The magnetic structures were analyzed by Lorentz microscopy and off-axis electron holography, including quantitative measurement of domain wall width, induction, and in situ magnetic domain imaging. The results indicate that the magnetic domain structure and particularly the dynamical magnetization behavior of the alloys strongly depend on the microstructure of the nanocrystalline alloys. Smaller grain size and random orientation of the fine particles decrease the magneto-crystalline anisotropy and suggests better soft magnetic properties which may be explained by the anisotropy model of Herzer.

The role of electron irradiation history in liquid cell transmission electron microscopy

Energy Technology Data Exchange (ETDEWEB)

Moser, Trevor H.; Mehta, Hardeep S.; Park, Chiwoo; Kelly, Ryan T.; Shokuhfar, Tolou; Evans, James E.

2018-04-20

In situ liquid cell transmission electron microscopy (LC-TEM) allows dynamic nanoscale characterization of systems in a hydrated state. Although powerful, this technique remains impaired by issues of repeatability that limit experimental fidelity and hinder the identification and control of some variables underlying observed dynamics. We detail new LC- TEM devices that improve experimental reproducibility by expanding available imaging area and providing a platform for investigating electron flux history on the sample. Irradiation history is an important factor influencing LC-TEM results that has, to this point, been largely qualitatively and not quantitatively described. We use these devices to highlight the role of cumulative electron flux history on samples from both nanoparticle growth and biological imaging experiments and demonstrate capture of time zero, low-dose images on beam-sensitive samples. In particular, the ability to capture pristine images of biological samples, where the acquired image is the first time that the cell experiences significant electron flux, allowed us to determine that nanoparticle movement compared to the cell membrane was a function of cell damage and therefore an artifact rather than visualizing cell dynamics in action. These results highlight just a subset of the new science that is accessible with LC-TEM through the new multiwindow devices with patterned focusing aides.

Virus Particle Detection by Convolutional Neural Network in Transmission Electron Microscopy Images.

Science.gov (United States)

Ito, Eisuke; Sato, Takaaki; Sano, Daisuke; Utagawa, Etsuko; Kato, Tsuyoshi

2018-06-01

A new computational method for the detection of virus particles in transmission electron microscopy (TEM) images is presented. Our approach is to use a convolutional neural network that transforms a TEM image to a probabilistic map that indicates where virus particles exist in the image. Our proposed approach automatically and simultaneously learns both discriminative features and classifier for virus particle detection by machine learning, in contrast to existing methods that are based on handcrafted features that yield many false positives and require several postprocessing steps. The detection performance of the proposed method was assessed against a dataset of TEM images containing feline calicivirus particles and compared with several existing detection methods, and the state-of-the-art performance of the developed method for detecting virus was demonstrated. Since our method is based on supervised learning that requires both the input images and their corresponding annotations, it is basically used for detection of already-known viruses. However, the method is highly flexible, and the convolutional networks can adapt themselves to any virus particles by learning automatically from an annotated dataset.

In situ TEM-tandem/implanter interface facility in Wuhan University for investigation of radiation effects

International Nuclear Information System (INIS)

Guo Liping; Li Ming; Liu Chuansheng; Song Bo; Ye Mingsheng; Fan Xiangjun; Fu Dejun

2007-01-01

Transmission electron microscope (TEM) interfaced to one or more ion implanters and/or accelerators, i.e. in situ TEM, provides effective tools to observe microstructural changes of studied samples during the ion irradiation. Evolution of both radiation damages and irradiation-induced nano-sized microstructures can be investigated with this technique, much more convenient than conventional ex situ techniques. In situ TEM technique has been widely applied in various fields, especially in the study of radiation damages of structural materials of fission and fusion nuclear reactors, and in evaluation and qualification of radioactive waste forms. Nowadays there are more than a dozen such facilities located in Japan, France, and the United States. Recently, we have constructed the first TEM-Tandem/Implanter interface facility of China in Wuhan University. A modified Hitachi H800 TEM was interfaced to a 200 kV ion implanter and a 2 x 1.7 MV tandem accelerator. Effective steps were taken to isolate the TEM from mechanical vibration from the ion beam line, and no obvious wobbling of the TEM image was observed during the ion implantation. The amorphization process of Si crystal irradiated by 115 keV N + ion beam was observed in the primary experiments, demonstrating that this interface facility is capable of in situ study of radiation effects. An online low energy gaseous ion source which may provide 1-20 keV H + and He + is under construction. (authors)

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.

Serial section scanning electron microscopy (S3EM) on silicon wafers for ultra-structural volume imaging of cells and tissues.

Science.gov (United States)

Horstmann, Heinz; Körber, Christoph; Sätzler, Kurt; Aydin, Daniel; Kuner, Thomas

2012-01-01

High resolution, three-dimensional (3D) representations of cellular ultrastructure are essential for structure function studies in all areas of cell biology. While limited subcellular volumes have been routinely examined using serial section transmission electron microscopy (ssTEM), complete ultrastructural reconstructions of large volumes, entire cells or even tissue are difficult to achieve using ssTEM. Here, we introduce a novel approach combining serial sectioning of tissue with scanning electron microscopy (SEM) using a conductive silicon wafer as a support. Ribbons containing hundreds of 35 nm thick sections can be generated and imaged on the wafer at a lateral pixel resolution of 3.7 nm by recording the backscattered electrons with the in-lens detector of the SEM. The resulting electron micrographs are qualitatively comparable to those obtained by conventional TEM. S(3)EM images of the same region of interest in consecutive sections can be used for 3D reconstructions of large structures. We demonstrate the potential of this approach by reconstructing a 31.7 µm(3) volume of a calyx of Held presynaptic terminal. The approach introduced here, Serial Section SEM (S(3)EM), for the first time provides the possibility to obtain 3D ultrastructure of large volumes with high resolution and to selectively and repetitively home in on structures of interest. S(3)EM accelerates process duration, is amenable to full automation and can be implemented with standard instrumentation.

Serial section scanning electron microscopy (S3EM on silicon wafers for ultra-structural volume imaging of cells and tissues.

Directory of Open Access Journals (Sweden)

Heinz Horstmann

Full Text Available High resolution, three-dimensional (3D representations of cellular ultrastructure are essential for structure function studies in all areas of cell biology. While limited subcellular volumes have been routinely examined using serial section transmission electron microscopy (ssTEM, complete ultrastructural reconstructions of large volumes, entire cells or even tissue are difficult to achieve using ssTEM. Here, we introduce a novel approach combining serial sectioning of tissue with scanning electron microscopy (SEM using a conductive silicon wafer as a support. Ribbons containing hundreds of 35 nm thick sections can be generated and imaged on the wafer at a lateral pixel resolution of 3.7 nm by recording the backscattered electrons with the in-lens detector of the SEM. The resulting electron micrographs are qualitatively comparable to those obtained by conventional TEM. S(3EM images of the same region of interest in consecutive sections can be used for 3D reconstructions of large structures. We demonstrate the potential of this approach by reconstructing a 31.7 µm(3 volume of a calyx of Held presynaptic terminal. The approach introduced here, Serial Section SEM (S(3EM, for the first time provides the possibility to obtain 3D ultrastructure of large volumes with high resolution and to selectively and repetitively home in on structures of interest. S(3EM accelerates process duration, is amenable to full automation and can be implemented with standard instrumentation.

Liquid-solid phase transition of Ge-Sb-Te alloy observed by in-situ transmission electron microscopy

Energy Technology Data Exchange (ETDEWEB)

Berlin, Katja, E-mail: katja.berlin@pdi-berlin.de; Trampert, Achim

2017-07-15

Melting and crystallization dynamics of the multi-component Ge-Sb-Te alloy have been investigated by in-situ transmission electron microscopy (TEM). Starting point of the phase transition study is an ordered hexagonal Ge{sub 1}Sb{sub 2}Te{sub 4} thin film on Si(111) where the crystal structure and the chemical composition are verified by scanning TEM and electron energy-loss spectroscopy, respectively. The in-situ observation of the liquid phase at 600°C including the liquid-solid and liquid-vacuum interfaces and their movements was made possible due to an encapsulation of the TEM sample. The solid-liquid interface during melting displays a broad and diffuse transition zone characterized by a vacancy induced disordered state. Although the velocities of interface movements are measured to be in the nanometer per second scale, both, for crystallization and solidification, the underlying dynamic processes are considerably different. Melting reveals linear dependence on time, whereas crystallization exhibits a non-linear time-dependency featuring a superimposed start-stop motion. Our results may provide valuable insight into the atomic mechanisms at interfaces during the liquid-solid phase transition of Ge-Sb-Te alloys. - Highlights: • In-situ TEM observation of liquid Ge-Sb-Te phase transition due to encapsulation. • During melting: Observation of non-ordered interface transition due to premelting. • During solidification: Observation of non-linear time-dependent crystallization.

Liquid-solid phase transition of Ge-Sb-Te alloy observed by in-situ transmission electron microscopy

International Nuclear Information System (INIS)

Berlin, Katja; Trampert, Achim

2017-01-01

Melting and crystallization dynamics of the multi-component Ge-Sb-Te alloy have been investigated by in-situ transmission electron microscopy (TEM). Starting point of the phase transition study is an ordered hexagonal Ge 1 Sb 2 Te 4 thin film on Si(111) where the crystal structure and the chemical composition are verified by scanning TEM and electron energy-loss spectroscopy, respectively. The in-situ observation of the liquid phase at 600°C including the liquid-solid and liquid-vacuum interfaces and their movements was made possible due to an encapsulation of the TEM sample. The solid-liquid interface during melting displays a broad and diffuse transition zone characterized by a vacancy induced disordered state. Although the velocities of interface movements are measured to be in the nanometer per second scale, both, for crystallization and solidification, the underlying dynamic processes are considerably different. Melting reveals linear dependence on time, whereas crystallization exhibits a non-linear time-dependency featuring a superimposed start-stop motion. Our results may provide valuable insight into the atomic mechanisms at interfaces during the liquid-solid phase transition of Ge-Sb-Te alloys. - Highlights: • In-situ TEM observation of liquid Ge-Sb-Te phase transition due to encapsulation. • During melting: Observation of non-ordered interface transition due to premelting. • During solidification: Observation of non-linear time-dependent crystallization.

In situ transmission electron microscopy studies of microstructure evolution in Ba(Zr{sub 0.2}Ti{sub 0.8})O{sub 3}-x(Ba{sub 0.7}Ca{sub 0.3})TiO{sub 3} piezoceramic

Energy Technology Data Exchange (ETDEWEB)

Zakhozheva, Marina

2016-10-21

The purpose of this work is to understand the microstructural features which contribute to the strong electromechanical properties of the lead-free Ba (Zr{sub 0.2}Ti{sub 0.8})O{sub 3}-x(Ba{sub 0.7}Ca{sub 0.3})TiO{sub 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.

Ultrastructural Characterization of the Glomerulopathy in Alport Mice by Helium Ion Scanning Microscopy (HIM).

Science.gov (United States)

Tsuji, Kenji; Suleiman, Hani; Miner, Jeffrey H; Daley, James M; Capen, Diane E; Păunescu, Teodor G; Lu, Hua A Jenny

2017-09-15

The glomerulus exercises its filtration barrier function by establishing a complex filtration apparatus consisting of podocyte foot processes, glomerular basement membrane and endothelial cells. Disruption of any component of the glomerular filtration barrier leads to glomerular dysfunction, frequently manifested as proteinuria. Ultrastructural studies of the glomerulus by transmission electron microscopy (TEM) and conventional scanning electron microscopy (SEM) have been routinely used to identify and classify various glomerular diseases. Here we report the application of newly developed helium ion scanning microscopy (HIM) to examine the glomerulopathy in a Col4a3 mutant/Alport syndrome mouse model. Our study revealed unprecedented details of glomerular abnormalities in Col4a3 mutants including distorted podocyte cell bodies and disorganized primary processes. Strikingly, we observed abundant filamentous microprojections arising from podocyte cell bodies and processes, and presence of unique bridging processes that connect the primary processes and foot processes in Alport mice. Furthermore, we detected an altered glomerular endothelium with disrupted sub-endothelial integrity. More importantly, we were able to clearly visualize the complex, three-dimensional podocyte and endothelial interface by HIM. Our study demonstrates that HIM provides nanometer resolution to uncover and rediscover critical ultrastructural characteristics of the glomerulopathy in Col4a3 mutant mice.

Specific, sensitive, high-resolution detection of protein molecules in eukaryotic cells using metal-tagging transmission electron microscopy

Science.gov (United States)

Risco, Cristina; Sanmartín-Conesa, Eva; Tzeng, Wen-Pin; Frey, Teryl K.; Seybold, Volker; de Groot, Raoul J.

2012-01-01

Summary More than any other methodology, transmission electron microscopy (TEM) has contributed to our understanding of the architecture and organization of cells. With current detection limits approaching atomic resolution, it will ultimately become possible to ultrastructurally image intracellular macromolecular assemblies in situ. Presently, however, methods to unambiguously identify proteins within the crowded environment of the cell’s interior are lagging behind. We describe a novel approach, metal-tagging TEM (METTEM) that allows detection of intracellular proteins in mammalian cells with high specificity, exceptional sensitivity and at molecular scale resolution. In live cells treated with gold salts, proteins bearing a small metal-binding tag will form 1-nm gold nanoclusters, readily detectable in electron micrographs. The applicability and strength of METTEM is demonstrated by a study of Rubella virus replicase and capsid proteins, which revealed virus-induced cell structures not seen before. PMID:22579245

Unravelling surface and interfacial structures of a metal-organic framework by transmission electron microscopy.

Science.gov (United States)

Zhu, Yihan; Ciston, Jim; Zheng, Bin; Miao, Xiaohe; Czarnik, Cory; Pan, Yichang; Sougrat, Rachid; Lai, Zhiping; Hsiung, Chia-En; Yao, Kexin; Pinnau, Ingo; Pan, Ming; Han, Yu

2017-05-01

Metal-organic frameworks (MOFs) are crystalline porous materials with designable topology, porosity and functionality, having promising applications in gas storage and separation, ion conduction and catalysis. It is challenging to observe MOFs with transmission electron microscopy (TEM) due to the extreme instability of MOFs upon electron beam irradiation. Here, we use a direct-detection electron-counting camera to acquire TEM images of the MOF ZIF-8 with an ultralow dose of 4.1 electrons per square ångström to retain the structural integrity. The obtained image involves structural information transferred up to 2.1 Å, allowing the resolution of individual atomic columns of Zn and organic linkers in the framework. Furthermore, TEM reveals important local structural features of ZIF-8 crystals that cannot be identified by diffraction techniques, including armchair-type surface terminations and coherent interfaces between assembled crystals. These observations allow us to understand how ZIF-8 crystals self-assemble and the subsequent influence of interfacial cavities on mass transport of guest molecules.

Switching operation and degradation of resistive random access memory composed of tungsten oxide and copper investigated using in-situ TEM.

Science.gov (United States)

Arita, Masashi; Takahashi, Akihito; Ohno, Yuuki; Nakane, Akitoshi; Tsurumaki-Fukuchi, Atsushi; Takahashi, Yasuo

2015-11-27

In-situ transmission electron microscopy (in-situ TEM) was performed to investigate the switching operation of a resistive random access memory (ReRAM) made of copper, tungsten oxide and titanium nitride (Cu/WOx/TiN). In the first Set (Forming) operation to initialize the device, precipitation appeared inside the WOx layer. It was presumed that a Cu conducting filament was formed, lowering the resistance (on-state). The Reset operation induced a higher resistance (the off-state). No change in the microstructure was identified in the TEM images. Only when an additional Reset current was applied after switching to the off-state could erasure of the filament be seen (over-Reset). Therefore, it was concluded that structural change relating to the resistance switch was localized in a very small area around the filament. With repeated switching operations and increasing operational current, the WOx/electrode interfaces became indistinct. At the same time, the resistance of the off-state gradually decreased. This is thought to be caused by Cu condensation at the interfaces because of leakage current through the area other than through the filament. This will lead to device degradation through mechanisms such as endurance failure. This is the first accelerated aging test of ReRAM achieved using in-situ TEM.

HR-TEM and FT-Raman dataset of the caffeine interacted Phe-Phe peptide nanotube for possible sensing applications.

Science.gov (United States)

Narayanan, A Lakshmi; Dhamodaran, M; Solomon, J Samu; Karthikeyan, B; Govindhan, R

2018-02-01

Sensing ability of caffeine interaction with Phe-Phe annotates (PNTs), is presented (Govindhan et al., 2017; Karthikeyan et al., 2014; Tavagnacco et al., 2013; Kennedy et al., 2011; Wang et al., 2017) [1-5] in this data set. Investigation of synthesized caffeine carrying peptide nanotubes are carried out by FT-Raman spectral analysis and high resolution transmission electron microscopy (HR-TEM). Particle size of the caffeine loaded PNTs is < 40 nm. The FT-Raman spectrum signals are enhanced in the region of 400-1700 cm -1 . These data are ideal tool for the applications like biosensing and drug delivery research (DDS).

Transmission electron microscopy a textbook for materials science

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Williams, David B

1996-01-01

Electron microscopy has revolutionized our understanding the extraordinary intellectual demands required of the mi­ of materials by completing the processing-structure-prop­ croscopist in order to do the job properly: crystallography, erties links down to atomistic levels. It now is even possible diffraction, image contrast, inelastic scattering events, and to tailor the microstructure (and meso structure ) of materials spectroscopy. Remember, these used to be fields in them­ to achieve specific sets of properties; the extraordinary abili­ selves. Today, one has to understand the fundamentals ties of modem transmission electron microscopy-TEM­ of all of these areas before one can hope to tackle signifi­ instruments to provide almost all of the structural, phase, cant problems in materials science. TEM is a technique of and crystallographic data allow us to accomplish this feat. characterizing materials down to the atomic limits. It must Therefore, it is obvious that any curriculum in modem mate­ be use...

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

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)

Qualidade de vida do paciente submetido à Microcirurgia Endoscópica Transanal (TEM Quality of life after Transanal Endoscopic Microsurgery (TEM

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Roberto da Silveira Moraes

2007-03-01

qualidade de vida com a TEM.BACKGROUND: Transanal Endoscopic Microsurgery (TEM is a minimal invasive procedure for the treatment of rectal tumors. Nowadays there has been an increasing medical interest regarding quantitative measurements pertaining quality of life. AIM: To evaluate life quality of patients submitted to TEM at Hospital de Clínicas of the Federal University of Paraná in the Department of Surgery of the Digestive Tract. METHODS: A prospective observational cohort study was done to evaluate the quality of life after TEM. Thirty-four patients answered a questionnaire composed of 14 questions concerning postoperative and labor issues. Questions concerned primarily about: informed consent; pain felt after surgery; patients capacity to walk during the postoperative state; period of return to normal activities; satisfaction regarding the absence of postoperative scars; postoperative incontinence, as well as the recommendation of this surgery to family members or friends. RESULTS: All thirty-four patients claimed to be adequately informed about the procedure. The absence of postoperative pain was observed in 82.5 %, and all demonstrated the capacity to walk in the first postoperative day. In average, returning to normal activities began after the seventh day of surgery. Only five patients (14.70% experimented transitory fecal incontinence, enduring no longer than a week. Three patients (8.82% were later readmitted to the hospital: two with residual tumors and the other for tumor recurrence. Two patients (5.88% complained about temporary modification in his/her sexual life after the surgery, and 97.05% would indicate TEM for his/her family members or friends. The average time period of admission was of three days. CONCLUSION: Patients presented a good evolution, with little postoperative pain, and a low complication index, demonstrating satisfactory and adequate quality of life after TEM.

Transmission electron microscopy of bulk specimens over 10 µm in thickness

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Sadamatsu, Sunao, E-mail: sadamatsu@mech.kagoshima-u.ac.jp [Department of Mechanical Engineering, Kagoshima University, Korimoto, Kagoshima 890-0065 (Japan); Tanaka, Masaki; Higashida, Kenji [Department of Materials Science and Engineering, Kyushu University, Nishi-ku, Fukuoka 819-0395 (Japan); Matsumura, Syo [Department of Applied Quantum Physics and Nuclear Engineering, Kyushu University, Nishi-ku, Fukuoka 819-0395 (Japan); Ultramicroscopy Research Center, Kyushu University, Nishi-ku, Fukuoka 819-0395 (Japan)

2016-03-15

We succeeded the observation of microstructures in bulk-sized specimens of over 10 µm in thickness by employing a technique that combines transmission electron microscopy (TEM) with energy-filtered imaging based on electron energy-loss spectroscopy (EELS). This method is unique in that it incorporates the inelastically scattered electrons into the imaging process. Using this technique, bright and sharp images of dislocations in crystalline silicon specimens as thick as 10 µm were obtained. A calibration curve to determine foil thickness of such a thick specimen was also derived. This method simply extends the observable thickness range in TEM. If combined with tilt series of observation over a significant range of angle, it will disclose three dimensional nanostructures in a µm-order block of a specimen, promoting our understanding of the controlling mechanisms behind various bulky material properties. - Highlights: • We developed a method which enables thick specimens to be observed using EF-TEM. • The effects of energy filter width and position on images were determined. • We suggested a method to determine the thickness of a thick film sample. • We achieved observation of microstructures in specimens with a thickness of 10 µm.

Geoelectrical characterization by joint inversion of VES/TEM in Paraná basin, Brazil

Science.gov (United States)

Bortolozo, C. A.; Couto, M. A.; Almeida, E. R.; Porsani, J. L.; Santos, F. M.

2012-12-01

For many years electrical (DC) and transient electromagnetic (TEM) soundings have been used in a great number of environmental, hydrological and mining exploration studies. The data of both methods are interpreted usually by individual 1D models resulting in many cases in ambiguous models. This can be explained by how the two different methodologies sample the subsurface. The vertical electrical sounding (VES) is good on marking very resistive structures, while the transient electromagnetic sounding (TEM) is very sensitive to map conductive structures. Another characteristic is that VES is more sensitive to shallow structures, while TEM soundings can reach deeper structures. A Matlab program for joint inversion of VES and TEM soundings, by using CRS algorithm was developed aiming explore the best of the both methods. Initially, the algorithm was tested with synthetic data and after it was used to invert experimental data from Paraná sedimentary basin. We present the results of a re-interpretation of 46 VES/TEM soundings data set acquired in Bebedouro region in São Paulo State - Brazil. The previous interpretation was based in geoelectrical models obtained by single inversion of the VES and TEM soundings. In this work we present the results with single inversion of VES and TEM sounding inverted by the Curupira Program and a new interpretation based in the joint inversion of both methodologies. The goal is increase the accuracy in determining the underground structures. As a result a new geoelectrical model of the region is obtained.

Innovative Strategies for Clinical Microscopy Instruction: Virtual Versus Light Microscopy.

Science.gov (United States)

McDaniel, M Jane; Russell, Gregory B; Crandall, Sonia J

2018-06-01

The purpose of the study was to compare virtual microscopy with light microscopy to determine differences in learning outcomes and learner attitudes in teaching clinical microscopy to physician assistant (PA) students. A prospective, randomized, crossover design study was conducted with a convenience sample of 67 first-year PA students randomized to 2 groups. One group used light microscopes to find microscopic structures, whereas the other group used instructor-directed video streaming of microscopic elements. At the midpoint of the study, the groups switched instructional strategies. Learning outcomes were assessed via posttest after each section of the study, with comparison of final practical examination results to previous cohorts. Attitudes about the 2 educational strategies were assessed through a postcourse questionnaire with a Likert scale. Analysis of the first posttest demonstrated that students in the video-streamed group had significantly better learning outcomes than those in the light microscopy group (P = .004; Cohen's d = 0.74). Analysis of the posttest after crossover showed no differences between the 2 groups (P = .48). Between the 2 posttests, students first assigned to the light microscopy group scored a 6.6 mean point increase (±10.4 SD; p = .0011), whereas students first assigned to the virtual microscopy group scored a 1.3 mean point increase (±7.1 SD; p = .29). The light microscopy group improved more than the virtual microscopy group (P = .019). Analysis of practical examination data revealed higher scores for the study group compared with 5 previous cohorts of first-year students (P virtual microscopy to traditional light microscopy. Virtual microscopy is an effective educational strategy, and students prefer this method when learning to interpret images of clinical specimens.

Transmission electron microscopy as a tool to image bioinorganic nanohybrids: the case of phage-gold nanocomposites.

Science.gov (United States)

Cao, Binrui; Xu, Hong; Mao, Chuanbin

2011-07-01

In recent years, bioinorganic nanohybrids composed of biological macromolecules and functional inorganic nanomaterials have revealed many unique properties that show promise for the future. Transmission electron microscopy (TEM) is a popular and relatively simple tool that can offer a direct visualization of the nanomaterials with high resolutions. When TEM is applied to visualize bioinorganic nanohybrids, a treatment of negative staining is necessary due to the presence of biological molecules in the nanohybrids except for those with densely packed inorganic materials. However, the conventional negative-staining procedure for regular biological samples cannot be directly applied to such bioinorganic nanohybrids. To image a specific bioinorganic nanohybrid, negative-staining factors such as negative stain type, working pH, staining time, and drying method, should be identified. Currently, no detailed studies have been done to investigate how to adjust negative-staining factors based on specific bioinorganic nanohybrids. In this study, bacteriophage-gold nanoparticle hybrids were chosen as a model to systematically study the effects of each factor on the negative staining of the nanohybrids. The best staining conditions for gold nanoparticle-phage nanohybrids were obtained and the effects of each factor on the negative staining of general nanohybrids were discussed. This work indicates that with proper staining it is possible to use TEM to visualize directly both biological and inorganic components without introducing any artifact. Copyright © 2011 Wiley-Liss, Inc.

Introducing measure-by-wire, the systematic use of systems and control theory in transmission electron microscopy

International Nuclear Information System (INIS)

Tejada, Arturo; Dekker, Arnold J. den; Van den Broek, Wouter

2011-01-01

Transmission electron microscopes (TEMs) are the tools of choice for academic and industrial research at the nano-scale. Due to their increasing use for routine, repetitive measurement tasks (e.g., quality control in production lines) there is a clear need for a new generation of high-throughput microscopes designed to autonomously extract information from specimens (e.g., particle size distribution, chemical composition, structural information, etc.). To aid in their development, a new engineering perspective on TEM design, based on principles from systems and control theory, is proposed here: measure-by-wire (not to be confused with remote microscopy). Under this perspective, the TEM operator yields the direct control of the microscope's internal processes to a hierarchy of feedback controllers and high-level supervisors. These make use of dynamical models of the main TEM components together with currently available measurement techniques to automate processes such as defocus correction or specimen displacement. Measure-by-wire is discussed in depth, and its methodology is illustrated through a detailed example: the design of a defocus regulator, a type of feedback controller that is akin to existing autofocus procedures. -- Highlights: ► High-throughput TEM operation is increasingly needed for research and industry. ► Autonomous high-throughput TEMs enabled by systems and control theory. ► Measure-by-wire is a new holistic automation oriented engineering view of TEM. ► A detailed example shows how to apply MBW to the automatic control of defocus.

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.

Multi-wall carbon nanotubes investigated by positron annihilation techniques and microscopies for further production handling